th

14 International Forensic
Science Symposium

Interpol – Lyon

19 – 22 October 2004

Review Papers
Edited by Dr. Niamh Nic Daéid
Forensic science Unit, University of Strathclyde, Glasgow, UK

1
Table of contents
Preface 4

Dr. Peter Pfefferli, Chairman of the Organising Committee

Scenes of crime
Technical co-ordinator :- James Robertson, Australian Federal Police, Australia

Fingerprints, tool marks and impressions 6

Firearms 47
Fibres 70
Paint and glass 85
Forensic geology 125

Individual evidence
Technical co-ordinator :- Trevor Howard, Forensic Science Service, United Kingdom

Biological evidence (DNA) 137

Biological evidence (hair) 148
Questioned documents (handwriting) 156
Speech and audio analysis, linguistics 171
Imaging 189

Chemical and material analysis

Technical co-ordinator :- Thomas Janovsky, Drug Enforcement Agency, USA

Drugs 207
Toxicology 260
Fire cause and debris analysis 303
Explosives 330
Environmental crime 359

Media evidence
Technical co-ordinator :- Anthony P DiClemente, FBI, USA

Questioned documents 389

Digital evidence 405

Poster presentations 550

Technical co-ordinator :- Dominique Saint-Dizier, France

2
 14th INTERPOL International Forensic Science Symposium, INTERPOL
Lyon (France), October 19 – 22, 2004

Preface
INTERPOL recognizes the demand to present advances made in scientific methods and to look
into future forensic needs and trends, by bringing together executives and senior scientists from
crime laboratories and forensic services throughout the world, to evaluate on a regularly basis
progresses made within a certain period. In this perspective the INTERPOL triennial
International Forensic Science Symposium (IFSS) is offering a comprehensive overview of
key areas of forensic sciences during the previous three years and therefore allow managers to
focus on the most relevant issues.

The objectives of the IFSS are to provide a forum for forensic managers from member states to
facilitate:

a) the presentation of advances made in scientific methods over the previous three (3) years,
and to provide a look into future forensic needs and advances,
b) the exchange of information which will enhance scientific methods in criminal
investigation and the administration of justice,
c) the discussion of problem areas encountered by member states and the possible provision
of solutions, and
d) the exchange and pooling of ideas for future progress

The symposium Proceedings on this CD concentrate on the Review Papers prepared by the
Coordinating Laboratories, which highlight and summarize advances of the various evidence
types. Furthermore the information about special sessions, panel discussions as well as the poster
presentations (as far as available when producing the CD).

According to the program of the IFSS, the various evidence areas are grouped into four major
areas:

! Scenes of Crime Evidence that includes Tool Marks & Impressions, Firearms, Fibres, Paint &
Glass, and Forensic Geology.
! Individual Identification Evidence, which is categorized as Biological Evidence (mainly
DNA), Questioned Documents – Handwriting, and Forensic Acoustics and Imaging.
! Chemical and Material Analysis Evidence, which means Drugs, Toxicology, Fire Cause and
Fire Debris Analysis, Explosives, and Environmental Crime.
! Media Evidence with Image Analysis, Questioned Documents (other than handwriting), and
Digital Evidence.

Besides these main contributions to review the state of the art, three thematic panels complete
the forensic setting. A first panel on Crime Scene goes through the process of management,
people and products at the scene. A second panel is devoted to Forensic Networks established in
various regions of the world for a better joint & combined forensic approach. A third panel is
looking at forensic issues in Scientific Investigations in Terrorist Acts with various experiences
from chemical terrorism until bombings.

3
Forensic science has also an established place within INTERPOL, in the operational police
support directorate. INTERPOL provides ongoing database support in forensic key areas such as
DNA, fingerprints, counterfeiting of travel documents or credit card fraud. A special session
with status report in these major areas considers therefore the role of INTERPOL and its
continuing relationship with the forensic community.

IFSS is only possible with the support of INTERPOL General Secretary, Ronald Noble.
INTERPOL staff coordinated all aspects of INTERPOL’s involvement from meeting
announcements to registration, and producing this CD with the symposium proceedings.

To make the IFSS 2004 possible it took significant effort by the Organizing Committee, each
Coordinating Laboratory and the review paper authors. With special thanks to a number of
persons in the Organizing Committee for their ongoing commitment:

Mr. James Robertson, Ph.D., Australia

Mr. Trevor Howitt, UK
Mr. Thomas Janovsky, USA
Mr. Antony DiClemente, USA
acting as Technical Coordinators of the four evidence review areas

Mr. Joe Bono, USA

Moderator of the Session on Scientific Investigation in Terrorist Acts

Ms. Dominique Saint-Dizier, France

Organizing the poster exhibition

Ms. Niamh Nic Daéid, Ph.D., UK

Preparing the symposium proceedings based on the reviews of the coordinating laboratories

Mr. Simon Dzidrovski, INTERPOL

Acting as liaison between the host and the Organizing Committee

Together with further supporters, the Organizing Committee team made IFSS-2004 possible.

Peter W. Pfefferli, Ph.D., Switzerland

Chair, 14th International Forensic Science Symposium Organizing Committee

4
SCENE of CRIME

5
 FINGERMARKS, SHOESOLE AND
FOOTPRINT IMPRESSIONS, TIRE
IMPRESSIONS, EAR IMPRESSIONS,
TOOLMARKS, LIPMARKS, BITEMARKS

— A Review: 2001 to 2004 —

Christophe Champod*, PhD – Nicole Egli, Lic. IPSC – Pierre A. Margot, PhD
*Corresponding Author
Ecole de Sciences Criminelles
Institut de Police Scientifique,
Bâtiment de chimie
Université de Lausanne
CH-1015 Lausanne-Dorigny
Switzerland
http ://www.unil.ch/esc

6
ABSTRACT

The purpose of this paper is to review the scientific literature from about September 2001 to
August 2004. The review is focused on published papers in scientific journals or proceedings and
on personal communications (complete reports) transmitted to our laboratory. The review will
not cover information coming from international meetings available only in abstract form.

International working group activities as they pertain to the identification process or to the
standardisation are fully discussed.

Fingermarks constitute an important chapter with further discussion on the identification process
as well as detection techniques on various surfaces and in their effect on other types of analyses
(DNA, LCN).

Image acquisition of marks, image processing, recognition as well as automatic treatments are all
parts of the present discussion of biometric systems and will be discussed.

Other biometric means of identification such as lip marks, bite marks, nails are also considered.

Toolmarks, shoe marks, tire marks remain important traces found in major or volume crimes;
their efficient classification and treatment play an important role in identification and crime
analysis. Current developments will be highlighted.

7
CONTENT

Introduction

The use of marks and impressions for forensic intelligence

Fingermarks

Friction ridge skin individualisation process

Dermatoglyphics
Fingermark detection and visualisation

Composition of fingermarks
Physical and chemical detection techniques
Alternative light sources, photography and digital/chemical imaging
Recovery of prints

Fingermark detection and DNA or biological fluid analysis

Shoe sole impressions

Introduction
Individualization process
Visualization
Other

Foot and face impressions

Ear impressions

Toolmarks

Lip- and Bitemarks

Lipmarks
Bitemarks

Tire impressions

Case reports

Miscellaneous

References

8
INTRODUCTION

In this report, we will adopt the following terminology regarding the words ‘print’ and ‘mark’.
The word print will here be used whenever standard, known material is considered, whereas
mark is used to designate the unknown mark or impressions, the recovered/detected traces or
latents.

This report will cover the scientific literature concerning different trace material from September
2001 to August 2004. Because of the amount of material covered, this report does not intend to
be a critical review but merely a point of focus and organisation of the available material. The
material reviewed primarily originates from peer-reviewed journals and published books
although non-reviewed electronic sources may at some points be used. Proceedings of colloquies
will be used only when available in the form of full papers. We will try to cover here more than
390 references and of course we run the risk of having missed important material. We apologise
in advance to any author(s) or organisation(s) whose contribution(s) should have been
mentioned. We also would like to thank individuals and peer groups that kept us informed of
current developments and initiatives in the areas covered in this report. To lighten the text,
references have been numbered, but not sequentially but in alphabetic order to improve
readability of the reference section.

In several of the impression evidence subjects, reference books have been published, covering
the recovery, comparison and evaluation processes. We propose to introduce them upfront. We
may in the next section come back to specific chapters of contributed books.

In the area of fingerprint evidence, we note multiple contributions: Recent publications have
covered the historical aspects of fingerprinting and brought to the table important sociological
perspectives90, re-affirmed the contribution of Dr. Henry Faulds38 (see also256), and documented
the essential development of the method in India during the 19th Century and its influence in
Britain304 (see also316). Champod and co-authors82 provides in “Fingerprints and Other Ridge
Skin Impressions” an overview from the morphogenesis of friction ridge skin, the identification
process and fingerprint detection (including a chapter on chemistry, light and photography). The
book gives also technical appendices providing recipes for reagents and some recent data on
fingerprint statistics (level 1 and level 2 features). The second edition of “Advances in
Fingerprint Technology”193 is complementary and provides detailed contributed chapters in
specific subjects from specific detection techniques to AFIS technology.

The other forensic impression identification fields also benefit from monographs. In the
shoeprint area, a doctoral thesis with a special focus on the different Swiss operational
experiences and development has been published in French127. For ear impressions, the book by
van der Lugt357 is an important contribution to the field. The odontology/bitemark area benefits
from the publication of a new book by Bowers especially to the attention of field investigators56.
A book dedicated in extenso to tire impression evidence has been published by Nause of the
Royal Canadian Mounted Police243.

Biometrics (including AFIS technology) is becoming a field in its own and we decided to limit
its coverage in this review. We do however want to note the recent publications of two books
devoted to fingerprint matters209,241 and an excellent guide to biometrics51 which goes much
deeper than the customary general overview available. Also we recommend a review on AFIS
technology readily accessible to forensic scientists149.

The book by John Russ is an important addition regarding the general use of digital imaging in
forensic science284.

9
Finally, Inman and Rudin present a paper on a forensic paradigm146 introducing the notion of
divisible matter. It is a key contribution that complements the must-have second edition of
Tuthill on individualization353.

The use of marks and impressions for forensic intelligence

We would like to stress on the importance of recent work regarding the use of marks in a
forensic intelligence context. Building up on the work by Ribaux274, recent research have shown
the potential of using fingermarks, footwear impression, gloves marks and toolmarks to be
integrated into a framework for criminal intelligence23,275.

The relationship between forensic/criminal data and the UK national intelligence model has been
exposed by Leary through the FLINTS computer system192. The efforts in the UK to put in place
a database of shoe marks for intelligence purposes have been reported224.

A full assessment of the constrains and possibilities offered by footwear marks in Swiss
operational units for forensic intelligence has been carried out by Girod127. The work illustrates
the successful operational results along with great perspectives for further development in all
area of impression evidence.

The operational use of shoe mark databases is explained by Napier242. The author also notes that
the distribution of fabrication characteristics of prisoners’ shoes and shoemarks recovered from
crime scenes is skewed with respect to the distribution in the general population.

It is clear to us that the future of forensic science holds not only in its contribution as evidence in
court but increasingly in its capacity to provide investigative leads and intelligence. The meeting
organised by the Forensic Science Society in 2002 translates that move towards forensic
intelligence378.

In the UK, the recent study by Rix highlighted the disparity between forces notably on the
intelligence use of shoemark and showed the need to define an appropriate framework and
harmonisation between units. No doubt that the potential of shoemark as intelligence tool
remains to be fully exploited.

Fingermarks

The importance of the Internet for sharing of information is ever increasing. One source of
weekly updates, especially on fingerprint identification issues is the “weekly detail”, an e-mail
newsletter maintained by Kasey Wertheim, which can either be consulted online
(www.clpex.com), or received through email under subscription. Jon Stimac is proposing a
newsletter entitled “Fingerprint Stuff…” which can be downloaded from the Internet
(www.pnwdiai.org/fpstuff/). Another weekly source of information is put together in the United
Kingdom: Dave Charlton who maintains a virtual group dedicated to fingerprint matters
(http://groups.yahoo.com/group/aridgetoofar/) is sending out to registered users “The Wake Up
Call E Magazine”. Likewise, the Southern California Association of Fingerprint Officers
(SCAFO) is putting their publication “The Print” online (www.scafo.org/The_Print/).

This reviewing period has been rich in events in relation to fingerprints as it coincides for
numerous countries with the celebrations of the 100 years of use dactyloscopy in criminal
investigation. We have been made aware of commemorative meetings held in the United
Kingdom (2002), Australia (2003), Germany (2003) and the United States of America (2004).

10
Various groups of fingerprint practitioners are also active. The FBI sponsored Scientific
Working Group on Friction Ridge Analysis, Study and Technology (SWGFAST) published on
the Internet all their proposed standards (www.swgfast.org). The reports from the work carried
out under the umbrella of Interpol from the fingerprint working parties are also available online
(www.interpol.com). The latest Interpol document on fingerprint identification has just been
released147. The activities of the UK Fingerprint Evidence Standard Project Board have been
reported by Leadbetter191. Finally, the ENFSI fingerprint working group should soon publish
information online (www.enfsi.org/).

Information available over the Internet is abundant, and the interest has peaked for two main
reasons: the questioning of the validity of fingerprint identification by courts especially in the
United States, and the use of this biometric means for the identification of terrorists. The focus
here will be particularly on the fingermark identification (in a law enforcement environment),
and less on the use of fingerprints in biometry, which has become a subject for itself.

Peer reviewed journals stay, however, the qualitatively most important source of information,
and cannot be replaced by the completely open forums.

The fingerprint profession as a whole has been put under pressure by several events the last three
years, some of which have been triggered by the application of the principles of admissibility of
expert evidence set by the decision in US v. Daubert2 applied to fingerprints in US v. Mitchell5.
These events have shown the need for the profession to reaffirm its foundations. Also, cases of
erroneous fingermark identifications have been publicized352, and the Internet has been an
excellent media to share these experiences (for instance http://onin.com/fp/problemidents.html)
including the recent case against Brandon Mayfield in the course of the investigation of the
March 2004 Madrid bombings.

Friction ridge skin individualisation process

The functions of the skin has been recently covered in a book117, subject to an excellent
review207. Its focus is not, however, on friction ridge skin in particular. Wertheim and Maceo372
present a highly informative and interesting review of morphogenesis. It is well completed by the
discussion on whether or not primary ridges are formed by fusing ridge units or from ridge
ledges380 and by the in-depth thesis of Kuecken185. This dissertation presents mathematical
models to predict level 1 features on fingerprints, following a thorough analysis of the friction
ridge skin morphogenesis knowledge, innovative.

Until January 2002, all Daubert hearings led to the full admissibility of fingerprint evidence in
the courtroom. January 2002 coincides with the first decision that limits expert testimony on
fingerprint identification. Indeed in US v Llera Plaza8 the defence “Motion to Preclude the
United States from Introducing Latent Fingerprint Identification Evidence” has been partly
successful. Judge Pollak held that a fingerprint expert could not give an opinion of identification
and required that the expert limits his testimony to outline the correspondences observed
between the mark and the print leaving to the court the assessment of the significance of these
findings. That led the Government experts to ask for reconsideration bringing to the debate
background documents in relation to the move of the UK toward the abandonment of the 16
points standard. Judge Pollack later reversed his opinion, and admitted the evidence. Certainly
that decision led to increased scrutiny and interest of the fingerprint area in the scientific
literature85,86 with unprecedented press coverage320 and reactions from the legal
community111,145,287. We also would like to draw the attention on the excellent paper by Robert
Epstein (the Federal Defender in both the Mitchell and Llera Plaza case109). Another paper by

11
the defence lawyer Lisa Steele provides also (and maybe in a more balanced manner) a detailed
analysis of the issues and ways to assess the foundation of fingerprint evidence323. The latest
court decision in the Mitchell case, accepting fingerprint evidence under Daubert, is probably the
most fair and balanced analysis of the field (US v. Byron Mitchell13).

Thatcher342 discusses the admissibility of scientific evidence and important cases with respect to
these questions. A revised and expanded court question list is presented293. An interesting
discussion about the search for truth in a research setting and in the judicial system, outlining
differences and parallels, has been presented46 which is in our opinion more balanced than the
commentary by Risinger and Saks276,288. However, it is fair to say that academic research is too
rare in identification sciences (apart from DNA) and efforts should be made to avoid forensic
science being qualified as an “oxymoron”172.

The Daubert hearing led also to thorough discussion regarding the statistics underpinning the
fingerprint identification process. A comprehensive and critical review of statistical studies on
fingerprints is provided by Stoney327. That chapter also discusses at length the limitation of the
so-called “50k study” undertaken by the Government in one of the major Daubert hearings (US
v. Mitchell). The latter study is also discussed by Kaye169. A study on fingerprint individuality
considering within and between finger variability has been published255, as has a study on the
similarity of identical twins’ fingerprints which showed that automatic verification systems
perform less well on such prints150.

Champod and Evett77 put forward their views that the overall process should remain
probabilistic. Needless to say that this view received mixed reactions95,213 from the profession,
still adhering strongly to the dogma of positivity.

A discussion of problems with scientific testimony in the judicial system and propositions for
solutions is proposed by Kaufman168. An historical overview of the evolution of fingerprints as a
forensic science, parallels with the emergence of DNA analysis, the challenges to the new
technique suffered up to its acceptance and the new challenges to the older technique are
discussed by Mnookin226,227. The paper by Cole91 regarding the history of fingerprint pattern
recognition is of interest within this context. The relationship between DNA and fingerprints is
examined from a historical/sociological point of view206.

The reasons for increased scrutiny in all areas concerned with identification are given by
Gutowski129. Different rulings concerning document examination3, fingerprints5 and DNA4 are
cited. The scrutiny and the reasons for it lead the author to question whether “Field and
Identification Sciences” are truly scientific, if they can meet standards for legal admission, if
their position can be improved and finally if new reporting methods should be introduced. The
author then discusses these questions in depth and gives recommendations. The scientific status
of fingerprint examination has also been discussed elsewhere112. That introspective analysis is
seen in numerous countries; see for example in Hungary319,337.

Two recent cases of wrongful fingerprint identification add oil on the fire of controversy
following the now famous McKie case that still receives deserved attention in the literature215.
Stephan Cowans has recently been exonerated by DNA analysis, the conviction having been
based on erroneous fingerprint identification229. The second case is that of Brandon Mayfield
who was wrongly associated by means of fingerprint to a latent mark revealed by the Spanish
National Police on a plastic bag containing detonators recovered from the stolen van associated
with the Madrid bombings. Three experts from the FBI and an independent court-appointed
expert all identified Brandon Mayfield as the donor of the mark. Mayfield, an Oregon-based
lawyer came to the attention of the FBI once one of the latent marks sent by the Spanish

12
authorities through Interpol gave a hit against his name on the FBI IAFIS. Brandon Mayfield
was arrested and remain in custody for a few weeks until the Spanish fingerprint experts, who
immediately had raised issues with this identification, finally identified the mark with the finger
of an Algerian suspect. The FBI made official excuses and launched a full and transparent
review of its operating procedures. That case received a large press coverage from which we
selected a representative sample176,228. We do observe a positive move towards a much more
open discussion of errors in the fingerprint field (we do refer to a recent national fingerprint
conference in the UK278 and the IAI 2004 conference regarding the Mayfield case).

Loftus and Cole reflect on the interactions that occurred in this case between different types of
evidence204. Haber and Haber discuss here131 and in an unpublished paper130 the importance of
double-blind procedures in this area, while Risinger and co-workers277 discuss in depth observer
effects and confirmation bias without restricting their discussion to fingerprint identification. The
paper by Cooley is also related94. On the research side, Charlton and co-workers (pers. comm.)
are exploring the impact of “contaminating” information on the fingerprint identification
decision process.

A discussion of the collection of marks that have potentially been left simultaneously, therefore
forming a sequence corresponding to the natural handling of an object, for example, is proposed
by Wisniewski387. Anatomical and morphological features, dynamic elements, the amount of
mark residue and the mechanism of latent formation have to be examined in order to declare that
several marks found close to each other form a complex, which in turn allows identification of
the complex with marks that, individually, would not have yielded identification. Digit
determination and a review of general pattern frequencies and the Henry fingerprint
classification has been described122. Boston53 highlights the importance of experience as a
fingerprint examiner. Saviano emphasizes the importance of analysis of level I detail in order to
avoid false exclusions in particular291.

An article reproducing the number of points required for identification in 31 European countries
has appeared20. Seven countries are listed which have no numerical standard. Byrd and Bertram70
provide an article on form-blindness and testing possibilities for applicants for fields in which
visual perception is of utmost importance. The authors furthermore present a survey of latent
print sections on testing requirements concerning eyesight for applicants and fingerprint
examiners.

The identification process is well described in the updated chapter by Olsen and Lee251. The
ACE-V methodology has been challenged88 and re-affirmed359,369 and the analysis stage
considered in detail135, while Langenburg investigates the analysis stage of ACE-V188, and
Beeton describes clearly and comprehensively a five-step process consisting of examination of
the latent, development of hypotheses to be addressed, experimentation, formation of a tentative
conclusion and testing of the conclusion39. A method of comparison of fingerprints based on an
analysis of metric proportions has been presented138. That paper received a strong critique214.
Busey and Vanderkolk assessed visual expertise in fingerprint examiners in one behavioral and
one electrophysiological experiment. They showed differences between fingerprint experts and
novices69.

The incidence and characteristics of interpapillary lines have been investigated using 502 prints
(palms and fingers) and examining 121 volunteers328.

Chaudhry and Pant84 use lateral palm marks in the course of the identification of the authors of
signatures. They give special attention to the positioning of the palm marks with respect to the
signature examined, and investigate the variability of this position using 25 test subjects. The

13
advantage of the method proposed is that even smudged lateral palm marks can be used, as long
as the perimeter is clear. A discussion of the use and interest of palm impressions from an AFIS
perspective is given by Blain48 and the German operational system has been presented348. The
AFIS experience in Hungary is also reported318. Also we would like to note the excellent book
by Tietze and Witthuhn347 on palmar heuristics and statistics that helps practioners positioning
marks while visually searching palm prints for a match.

Dermatoglyphics

Since the advances of DNA analysis in biology, dermatoglyphic research has been drastically
reduced. However, we came across some publications of interest.

It has been shown that, based on general patterns and ridge count, the differentiation between 17
Spanish populations within geographic valleys is greater than between sexes in a given valley25.
Analysis of qualitative digital and palm data clustered Berber females with Iberian samples, and
Berber males were within the variation range of North African groups139. Sexual dimorphisms
have been investigated in India161 in 500 families from five populations. An investigation of
ridge patterns in children exposed to anticonvulsant drugs showed differences with respect to the
general population, especially in those exposed to polytherapy: phenytoin and phenobarbital50.
An association between waist-to-thigh ratio and ridge-count difference between the right fourth
and fifth fingers has been found in healthy subjects, and this difference was inversely associated
with the age of male patients (used as an indicator of survival), notably among the patients with
type 2 diabetes159. A comparison between the dermatoglyphics of humans and rats on the basis
of palmar, plantar and digital pads and flexion creases is presented by Kimura and coworkers177
in order to determine if rats could be used as a model for the study of factors influencing the
development of these characteristics. Four Indian tribal populations have been investigated
considering ridge count asymmetry186 and finger ridge count correlations187. Models regarding
relationships between handedness, dermatoglyphics and sexual orientation have been
evaluated239 and links between ridge counts and schizophrenia investigated286 and disproved.
Palm print research methods, their application and one result have been presented393.

Fingermark detection and visualisation

Apart from the monographs we introduced earlier 82,193, the following papers were focused on
detection and visualisation techniques. As an overview paper, we note the discussion of different
fingermark enhancement techniques by Wickens375 and the updated chapter by Lee194. A review
on current photoluminescence detection of fingermarks with outlook into upcoming strategies
(background suppression by time-resolved imaging and new reagents) is proposed by Menzel220.
Menzel also wrote a complete chapter on the use of nanoparticles to reveal latent marks221.

Since fingermark detection (or aging) heavily depends on the residue composition, we propose to
start with a small subsection devoted to the chemistry of the latent residue and then to focus on
detection techniques.

Composition of fingermarks

We would like to start with the in-depth chapter on fingermark chemistry by Ramotowski271.
Since that publication, we noticed additional contributions we will try to cover below.
Building up on the work by Mong et al.231, analysis of fingermark residue by GC/MS showed no
inference regarding gender can be made from the quantitative ratios of components relative to
squalene26. The analysis of fingermark residue by infrared microspectroscopy allows to monitor
to some degree the aging of a mark384. The aging process of fingermarks has been further

14
described and illustrated by Baniuk34. The author gives some diagnostic indicators in three stages
to describe the external features of ageing of a latent deposit. She insists on the fact that the
causal relationship between these indicators and age is highly dependant on the external and
other conditions. Hence simulations reproducing the case at hand are required to guide as to the
age of a given mark. We concur with the pessimistic view expressed by Wertheim371, when it
comes to estimate the time since deposit for fingermarks.

In the research area, a micro total analysis system, a microchip-based method for direct
sampling, on-chip pre-concentration and electrophoretic separation followed by fluorescence
detection, for the analysis of fingermark residues has been proposed355. One appendix of this
PhD work includes also an overview of the different types of sweat glands.

Physical and chemical detection techniques

Powder
A review of powder methods is proposed by Sodhi and Kaur311. A cost effective powder
formulation based on Rhodamine B dye is proposed317.

Magnetic and nonmagnetic powders have been compared on ceramic materials30. 20 ceramic
cups were chosen and dusted using bi-chromatic and magnetic bi-chromatic powder. The
magnetic powder causes more background noise. The overall result is, however, better when
using magnetic than when using non-magnetic powders.

Powder suspension methods useful on adhesives were tested on 9 different surfaces116. SSP
(sticky side powder) and soot solutions were used with varying formulations. In a second part a
mixture of soot and dishwashing soap to be applied by brushing was presented. The soot mixture
led to better results than SSP, and tests with several powders (Green- and Redwop, Green-, Red-
or Yellowescent, bi-chromatic, etc.) showed that many other suspensions can be used and their
colour chosen with respect to the support of the mark. In particular, Titanium dioxide gives good
results, and even developed marks on the non adhesive side of tape when in suspension360.
Ninhydrin, Cyanoacrylate and Ardrox stain or black powder, black powder and black magnetic
powder have been tested for fingermark visualisation on bones, and black magnetic powder has
been found to be the most suitable technique388. The use of a dress steamer when dusting does
not give the improved results259.
A survey examining the daily exposure to aluminium, carbon black and iron of crime scene
technicians due to powdering was conducted108 and the accumulated values over a normal
workday stay well below the occupational exposure standards.

The use of several casting materials for lifting fingermarks which are difficult to photograph has
been proposed97, as has been the use of children’s glue for the lifting of powdered marks on
uneven surfaces, best results having been obtained using “Elmer’s school glue, no run gel”171. A
method for the use of dental stone for the casting of fingermarks on dark surfaces in a way that
preserves contrast of the (light) powder with the light dental stone is presented179, and dental
stone is compared to stretchy and regular fingerprint tape and rubber lifters as a method for
lifting fingermarks with a discussion of its advantages and disadvantages180. The Isomark® spray
(a synthetic rubber compound casting material) is also a method of choice here62.

Physical developer (PD)

Two review papers of the PD process are a decisive contribution to the understanding of the
method73,74. That allowed to develop a new and less expensive formulation for physical
developer using reverse osmosis/deionized instead of distilled water67,68. The change for purer

15
water leads to a change of the formulation for this reagent. Lloyd reported excellent results with
PD on a class of counterfeit currency203.

Cyanoacrylate (CA)
Following a comparison between two different vacuum fuming systems and atmospheric fuming,
the authors conclude that atmospheric conditions are better than fuming in a vacuum83. Lewis
and co-workers have studied the chemical processes involved in the development of latent
fingermarks using the CA fuming method using clean and oily marks and Scanning Electron
microscopy for the determination of the morphology of the polymer resulting from CA fuming
on both types of marks200. Geller has commented this study123.
Several commercially available glues have been tested by Czubak98 on fresh marks of one donor
on glass, fresh wood, plastic, metal, rubber and polyethylene foil. The results show no difference
between 7 different kinds of glue, which leads to the conclusion that any glue can be used for CA
development of fingermarks. The rinsing of polythene bags contaminated by cocaine for
subsequent treatment by CA fuming has been described208. Five solvents and a solvent mixture
were tested, and diethyl ether has been retained as a suitable method. It inhibits, however,
subsequent treatment using VMD.

Finally, Masters reports that cyanide gas is formed when cured (polymerised or hardened)
cyanoacrylate is heated above 205° C211.

Vacuum metal deposition (VMD)

A series of three articles investigates the following topics with respect to VMD: the influence of
polymer type, mark donor and age156, factors affecting normal and reverse development of latent
marks154 and the development of fingermarks after the deposition of excess gold153. The
visualisation of fingermarks using VMD on a ferromagnetic-coated surface, on the reverse side
of polyethylene film and on foam styrol packing material330 has proven successful.

DFO and ninhydrin

Sodhi and Kaur313 give a historical account of fingermark reagents reacting with amino acids.
The review paper by Almog remains a prerequisite reading in this area18.

Interference by the humidification used for ESDA processing and subsequent fingermark
development by DFO, ninhydrin, the sequence DFO-ninhydrin and two formulations of 1,2-
Indanedione has been evaluated29. Exposure times in the humidification chamber were of 2, 4, 15
and 60 minutes. For DFO, humidification up to 60 minutes is tolerable. Ninhydrin results in less
marks and their quality starts to decline after humidification of over 2 minutes on one type of
paper. For 1,2-indanedione, an exposure to humidity for up to 4 minutes is favourable to the
mark development. Longer exposure times have a detrimental effect for the mark quality after
treatment. Exposure times of more than two minutes also degrade results obtained by the
sequence DFO-ninhydrin.

Optimisation of 1,2-indanedione in HFE7100 and testing of the obtained solution in comparison

with DFO has been performed121, as has the validation of the reagent162. Concentrations of 0.25,
0.50, 0.75, 1.00 1.50 and 2.00 g/L were used, and maximum fluorescence was observed with the
lowest concentration and 10ml/L of solvent with acetic acid. Only small differences between this
1,2-indanedione formulation and DFO was observed, exception made of a stronger initial
fluorescence of DFO. This difference is compensated for after a week of storage in the dark. A
comparison of 1,2-indanedione at concentrations of 1g/L, 0.1g/L and 0.05g/L and DFO on
fingermarks that had been deposited on paper, grey cardboard, banknotes and a passport 1 day, 3
days and a year before treatment has been carried out279,377. The solutions of both reagents were
prepared using HFE 7100, petroleum benzene and Frigen (CFC-113). HFE7100 is the solvent

16
yielding the best results. This result is confirmed by others282,283,303. The authors conclude that
1,2-indanedione at concentrations of 1g/L and 0.1g/L can be used in many cases more efficient
than DFO and that no background colouring is observed using 1,2-indanedione, as opposed to
DFO. One 1,2-indanedione formulation and two DFO formulations in ozone-friendly solvents
have been tested222, and the results show that HFE7100 is a good (even slightly advantageous)
replacement solvent for DFO. In a field trial comparing two DFO formulations with one 1,2-
indanedione formulation, the DFO formulation developed by the PSDB222 performed
better381,383. The reaction of 1,2 indanediones has been also investigated258. Confirming past
experiences, a ninhydrin formulation using hexane as carrier provides good results292.

5-methylthioninhydrin (5-MTN) as a substitute to ninhydrin is the subject of an article by

Drabarek and Sikora104. Both reagents have been tested on various porous surfaces (white
photocopy paper, newspaper, brown cardboard, white envelopes and yellow stickers). In this
study, the sensitivity and efficiency of the reaction is higher for 5-MTN than for ninhydrin, the
visual differences under white light are not significant. After secondary treatment with zinc salt,
the fluorescence of latents treated with 5-MTN is higher than for ninhydrin, whereas for the
secondary treatment with Cadmium, the reverse is true. The authors propose to use both reagents
in parallel.

Four side-chain-elongated analogues of 5-methoxyninhydrin, soluble in n-hexane, were tested.

Elongation of the side-chain increases solubility, but decreases detection capability of
compounds, 5-ethoxyninhydrin performing equally well as 5-methoxyninhydrin249 and showing
stronger luminescence after zinc complex formation than ninhydrin at room temperature.

A study investigating the applicability of complex formation with metal salts of the DFO amino
acid adduct has been published93. Little, if any, enhancement of luminescence was observed with
Zn, Cd, Ru or Eu treated DFO developed latent fingermarks.

Six ninhydrin analogues containing oxygen, sulfur, and selenium substituents at the C-5 position,
5-(4-nitrophenyl)ninhydrin, and benzo[f]furoninhydrin (giving a strongly luminescent result at
room temperature after zinc complexation) were evaluated as fingermark development reagents
by Kobus and co-workers181. Good fingermark development was obtained using these reagents,
but it was not superior to ninhydrin.

Thermal and Carbonless paper compositions and reactions are presented by Stimac324, who also
tests a formulation of 1,2-Indanedione to be used on thermal paper325. A review of methods
applicable on thermal paper is proposed by Schwarz301, including iodine fuming334, silver
nitrate250, DMAC61, hydrochloric acid64, washing with acetone35,36, dry ninhydrin
application216,250, sublimation of ninhydrin299 and 2-isononyl-ninhydrin (INON or
ThermaNin)301,302,335. The review points out problems with these reagents (costs, sensitivity,
dangers of the reagents, time-intensity), and the best reagent considering all the constraints is
INON. As INON liberates ninhydrin in the presence of water (and a catalytic amount of acid),
the working solution prepared in an apolar solvent is not very durable due to the omnipresence of
water. Schwartz301 presents the preparation of INON. A comparison between ninhydrin and DFO
with or without clearing by Freon and ethyl alcohol, dry ninhydrin and hydrochloric acid showed
that dry ninhydrin is the best single method for the development of marks on thermal paper, and
a sequence is proposed: hydrochloric acid then DFO and dry ninhydrin350. Nitric acid is
mentioned as an alternative to hydrochloric acid332.

The effect of ninhydrin, physical developer and a bleach enhancer on the physical and chemical
examination of documents produced from copiers and printers has been studied189. All treatments
changed the optical properties of inkjet specimens; however, the authors find that it is feasible to

17
examine such documents after ninhydrin treatment, and for documents produced by a
photocopier or laser printer, none of the treatments tested hindered a subsequent physical and
chemical examination189.

Blood
Ortho- and para-phenylenediamine for the enhancement of fingermarks in blood have been
investigated71. Both reagents are effective and less hazardous alternatives to 3,3'-
diaminobenzidine (DAB), particularly on porous surfaces. They result in orange or purple marks,
therefore offering alternative colours to the brown colour of DAB and the light green colour of
ABTS.

The development of bloody fingermarks on skin using amido black is presented190, in the form of
a case report, where cyanoacrylate and powder were used before the application of amido black,
both methods resulting in no visible marks, whereas amido black resulted in two marks.

A report on the results of tests of 15 fluorescent reagents for the development of latent
fingermarks in blood is proposed201. Four methods for blood enhancement (Amido Black,
Hungarian Red, Crowle’s Double Stain and Leucomalachite Green) have been tested on 7
different surfaces114 and Amido Black performed best overall.

Other methods (MMD, lanthanide complexes, Genipin, Rose Bengal, blueing, etc…)
MMD II296 has been evaluated in comparison with MMD I290, and has been found to develop
better marks; however the silver acetate/hydroquinone physical developer, while giving superior
detail, was found to give a weaker development than the silver nitrate/iron(II)/iron(III) physical
developer155. The authors find that a sequence including VMD is more sensitive than MMDII on
nonporous surfaces, whereas on some semiporous surfaces (except on polymer banknotes157),
MMDII is recommended155.

Fingermark detection methods that have direct application to time-resolved imaging techniques
are presented by Bouldin54. Sypro Rose Plus Protein Blot Stain (a lanthanide complex), which
allows the use of time-resolved imaging, is presented by the same author55 as a potentially
universal fingermark reagent.

Almog and coworkers19 present a new fingermark reagent (Genipin), that forms a visible, blue
compound with amino-acids. The reaction product is also luminescent. Additionally, this reagent
is not harmful for laboratory personnel (product currently used as a food additive). The
development process has, however, not yet been optimised.

Another non-toxic fingermark reagent, Rose Bengal, is proposed by Sodhi and Kaur315. The
same group proposed the use of Eosin-blue dye and Phloxine B dye to reveal marks on various
types of surfaces312,314.

A lanthanide shift reagent (tris (6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedionato)

europium (III) or Eu(fod)3) has been investigated for luminescent visualization of latent
fingermarks. The results obtained on paper were inferior to those obtained by DFO. However,
the treatment using Eu(fod)3 permits subsequent treatment by DFO/ninhydrin72. On aluminum
drink cans and galvanized iron the treatment was superior to Superglue/panacryl. Detection of
latent marks on metal surfaces using a scanning Kelvin microprobe is proposed385.

The sublimation of disperse dyes in order to colour plastic tapes (except fingermarks that could
be present) has been tested, with or without prior cyanoacrylate fuming. The conclusions are that
this method provides well-defined fingermarks, and that it should be applied after CA fuming322.

18
Un-du® has been tested with respect to its effect on subsequent treatments using ninhydrin,
Physical developer, gentian violet and Alternate Black Powder and it has been shown not to
inhibit these methods300. It has also been shown that Un-du® is best used before treatment using
ninhydrin. Compressed air for the separation of layers of adhesive tapes by freezing has been
proposed102 and applied successfully.

Excellent results (judged better than with CA on polymer materials) to reveal marks using RTX
on various substrates have been obtained by Centorika and Rone76.

A test of visualisation methods on human skin has been published by Lenertz and
Schönborn197,198. The tested methods were iodine fuming, black Magna-brush® powder and
transfer by Isomark® (a synthetic rubber compound casting material described by Brennan and
co-workers62), white gelatine lifters or transparent mark lifters. 1/8th of the marks were
considered useful for examination. Only greasy marks gave results, powdering being the
preferred method and casting by Isomark® being preferred to lifters when hair is present or the
skin is very uneven.

A new process for development of fingermarks on metal items is proposed by Bersellini and
coworkers42. Electropolymerisation processes of pyrrole and substituted porphyrins are used.
The method is based on the presence of fatty acids that are contained in fingermarks and act as
an insulator. The negatives of the fingermarks are therefore developed. The results presented are
preliminary. Three blueing methods with or without prior CA treatment, CA and basic yellow,
and an etching technique have been tested on brass cartridge cases, with fingermarks deposited
before or after firing and on unfired cartridges120. The results show that the moment of
deposition, the use of the cartridge, and the material on which the fingermarks are deposited with
are more important than the technique used for their development.

Alternative light sources, photography and digital/chemical imaging

Five forensic light sources have been compared taking into account the filter transmission, power
output through the various filters, the uniformity of the beam and the ease of use. The results
indicated that none of the light sources tested is uniformly superior to the others382. To record
marks on substrate reflective surfaces, the precious use of coaxial or episcopic lightning has been
reminded47.

The police forensic Laboratory in Wroclaw (Poland) reports its methodology of digital recording
of fingermarks for the needs of AFIS389. The use of Photoshop® for demonstrative purposes is
presented370. In a broader sense, the use of digital imaging technology has been discussed99.
McMahon217 explains a case where digital treatment of fingermark photographs is scrutinized.

The reduction of the interference of background by adding or subtracting images taken under
different lighting conditions and showing the same background printing or pattern is explained
by Comber92; background subtraction by substitution of the exhibit by an identical object is also
described100. Image treatment by subtraction, fast Fourier transform and contrast adjustment is
discussed using examples by Dalrymple and co-workers101, and some contrast enhancing
techniques are explained by Scarborough and Dziemieszko294. An image restoration technique
based on amplitude and frequency modulation reaction-diffusion is proposed in order to restore
defective or contaminated fingermarks for recognition tasks and not for identification
purposes367. Latent fingerprint enhancement based on AM-FM model has also been developed
by Pattichis and Bovik257.

19
The use of luminescence and visible absorbance chemical imaging technology on treated (DFO,
ninhydrin, CA, luminescent dyes) and non-treated fingermarks has been shown110; unwanted
background can be minimized using this technique.

Recovery of prints

Several methods for obtaining fingerprints from mummified, decomposed or charred fingers are
proposed by Kahana and co-workers158. A method for taking fingerprints from the deceased
using soot powder and gelatine lifters is presented106.

Fingermark detection and DNA or biological fluid analysis

There is still a great interest in the combined use of DNA and fingermarks as shown in numerous
recent cases (see for example346). The use of fingermarks as an indicator of contact is only
possible after visualisation, and thus the way to combine detection processes and DNA analysis
(being from bloody fingermarks or residues left following the bare contact between the friction
skin and a surface) are extensively tested.

A review on analysis of trace quantities of DNA left by contact374 and a commentary329 have
been published. Alessandrini and co-workers17 analysed contact DNA from fingermarks left by
11 persons on glass, wood and metal without any prior detection technique. They showed that
despite the small quantity of DNA detected (0.04 to 0.2ng), a DNA profile can be obtained in a
high percentage of the deposited fingermarks. Extraneous DNA was observed, as were locus
dropout, spurious alleles and stutters. Almost a third of the profiles obtained however were
complete (10 loci) and corresponding to the donor. Another research, focused on paper, not only
investigated nuclear DNA but also mitochondrial DNA32. The authors investigated the influence
of touching time, three methods of fingermark development (ninhydrin, iodine, and soot), delay
between apposition of the fingermark and DNA analysis and the time of day. 80% or more of the
experiments yielded a useful DNA profile, except when a fingermark enhancement method was
used (47%). All samples used for the analysis of mtDNA showed positive results. A study
focused on LCN (low copy number) DNA reports successes obtained on treated (powder, iodine,
ninhydrin, metal deposition or physical developer) fingermarks205.

A laboratory introducing 1,2-indanedione for operational use tested two operational solutions of
this reagent with respect to their effect on subsequent DNA profiling28. The issue here is more
the impact of the chemicals on other DNA present on the substrate that is unconnected to the
fingerprint apposition (e.g. saliva on paper). The test was done on envelopes, with the stamps
being licked by known donors. The envelopes were then treated by one of the reagent solutions
and finally STR typing was conducted. No difference between treated and untreated envelopes
was observed. However, a time effect was observed, for six days after 1,2-indanedione
treatment, no DNA could be extracted anymore. Grubwieser and coworkers128 have also
investigated the DNA profiling of blood and saliva traces after visualization of fingermarks.
Optical, physical, physico-chemical, and chemical methods were used (UV Light, dusting, soot,
manoxol-molybdenum method, iodine-benzoflavone, CA followed by RAM or safranin, silver
nitrate, ninhydrin, DFO, RTX) and special methods for adhesive tapes and blood traces (gentian
violet, SSP, CA/safranin, luminol, amido black, Coomassie Blue, TMB, LCV, LMG and
Hungarian red). Only the last four methods using the airbrush technique were deleterious, but
STR profiles could be obtained using the layer technique. According to Zamir392, small particle
reagent (SPR) does not inhibit DNA analysis from bloodstain. Visualisation using soot or
magnetic powder followed by transfer using tape was tested with regards to its impact on
subsequent DNA analysis298. It has been shown that even from tape-archived fingermarks, DNA
profiles could be obtained. The effect of blood enhancement techniques (amido black, Crowle’s

20
double stain, Hungarian red, leucomalachite green, luminol, ninhydrin and DFO) on subsequent
DNA analysis have been examined specifically on a large variety of surfaces115. No deleterious
effect on DNA analysis has been highlighted, but a loss of biological material was observed. The
importance of the surface on which DNA is deposited is emphasized by a study that tested UV
(on glass) and white light (on plastic bags), white, black and magnetic powder (on glass),
cyanoacrylate and Rhodamine 6G dye or vacuum metal deposition (on plastic bags) and sticky
side powder (on tape). These techniques were shown not to have a deleterious effect on the
subsequent DNA analysis of fingermarks, but on paper and aluminium foil no results were
obtained, with or without treatment272.

A final note will be on presumptive tests for blood: some interference has been observed
between the reaction product of ninhydrin with amino-acids (Ruhemann’s purple) and leuco
crystal violet (LCV)225. If LCV is used, it should come before the ninhydrin process.

We have been also alerted by the recent study by Ramotowski and Regen (US Secret Service,
personal communication). They reported that high doses on radiation required to destroy
biological agents such as anthrax are sufficient to have a detrimental on the success of
fingermark detection techniques. The efficiency of almost all methods are reduced (except PD
and MMD processes).

SHOE SOLE IMPRESSIONS

Introduction

A list of websites showing shoesoles of plenty of models (with special attention given to shoes
sold in Poland) is given in333. General examination of shoe sole marks and chain of custody
issues are also treated. The C.A.S.T. (Chesapeake Area Shoeprint and Tire track) website
(http://members.aol.com/varfee/mastssite/index.html) is an extremely valuable source of
information with links towards the forensic and manufacturers websites. The ENFSI marks
working group is important in this area (www.intermin.fi/intermin/hankkeet/wgm/home.nsf/).
On their web site, all activities of the group are reported along side with an important library of
papers articles and the regular group bulletin (Information Bulletin for Shoeprint/Toolmark
Examiners). The annual report of the activities of the group have just been published165. The
group is organising annual professional meeting. The meeting in Berlin 2001 led to the
publication of a volume of papers166. The German marks group hosted another meeting in Berlin
that led to the publication of a volume21.

Individualization process

Two Daubert decisions concerning the admissibility of shoeprint examiner testimony have been
given7,12: the admissibility of such evidence has been confirmed.

An interesting study pertaining to the discrimination value of wear patterns on 127 right military
boot impressions, acquired after 5 weeks of training, has been published119.

Hara stressed on the need to use high magnification during the examination process to ascertain
the nature of the features available on the outsole136.

On of the subgroup of the ENFSI marks working group under the chair of H. Katterwee of the
BKA took up the challenging task of exploring and guiding as to the choice of an adequate scale
of verbal strength of evidence in the area. That initiative led to a series of letters and papers
arguing the pro and cons of various options49,78,80,148,164,310,336,376. Our laboratory took part to this

21
discussion and expressed our views in favour of a reporting scheme based on the likelihood ratio.
The community at large showed the willingness to keep a standard posterior scale. We think that
the debate will continue.

Visualization

The testing and comparison of a large number of methods for the enhancement of muddy shoe
sole impressions on paper, glass and cotton is reported343.
The particular problem of shoe impressions in snow has been discussed134. The protection of
such marks from the sun in order to avoid melting is mentioned, as is the use of spray paint for
heightening contrast and in preparation for casting, and the use of snow print wax. Finally,
casting using dental stone or sulphur is presented. Shor and co-workers308 propose the use of a
hydraulic press for lifting shoe marks on rough or porous surfaces. Footwear impressions in
blood, once treated by leucocrystal violet, can be further enhanced by spectral enhancement. The
appropriate absorption and emission wavelengths have been determined321.

Other

The recovery and analysis of DNA from shoe insoles is discussed by Bright and Petricevic63.
The prevalence of glass fragments in shoes and on their outside has been investigated281.

Promising results from digital imaging fusion indicates that issues arising from lighting effects
may be overcome in the near future368.

FOOT AND FACE IMPRESSIONS

A comparison between inked and electronically acquired footprints showed that several
geometric indexes diverged between prints taken using both methods354. Kennedy and co-
workers propose and illustrate the comparison of marks with the shape of the foot of a
suspect,174, particularly in cases where the shoe is the source of impressions at the crime scene
but the link between the shoe and its wearer is questioned, or for the use of socked impressions.
A description of the collection of comparison material, a list of barefoot morphology specialists
and an overview of their potential results is given173. An excellent statistical study on foot
morphology considering within and between variability has been published175. A case report
where a toe has been identified196 has been published. We understand that the North Carolina
Court of Appeals 2001 in State v. Berry9 postponed its admission of footmark impression until
completion of above research65.

The influence of different weight-bearing conditions on plantar foot shape has been
investigated351. Impressions left from faces on airbags following accidents are currently
researched in Japan390,391.

EAR IMPRESSIONS

We already mentioned the publication of the book by van der Lugt on the subject357. The practice
in Poland is presented by Kasprzak163. Critical reviews have been recently published79,358. In our
opinion, the field of earmark identification is at its infancy and would benefit from a structured
program of research. Abbas and Rutty14 published a useful guide to web based material on
earprints and concluded also that despite the availability of numerous websites about the uses of
the human ear in forensic science, the true value of the ear in the process of forensic
identification is still in its embryonic stages.

22
Earmark to earprint comparison relies at the moment more on individual experience and
judgement than on a structured body of research undertaken following strict scientific guidelines.
The recognition process is highly subjective and takes advantage of the extraordinary power of
the human eye-brain combination.

The field of earprint identification is currently being researched through an important initiative
under the umbrella of the European community (www.fearid.com). It is a welcome initiative that
led to the publication of a review and exploratory study on the intra- and inter-individual
variability of ear marks has been proposed219.

Two cases involving earmarks have reached the Court of Appeal in the United Kingdom. The
Court of Appeal11 allowed the admission of earprint evidence but received additional
information that emerged more clearly since trial that shed some new light on the strength of the
evidence. Had that evidence been available to the defence at trial, it might have reasonably
affected the decision of the jury to convict and hence the conviction was quashed and a new trial
was ordered22. In Dallagher, the Court ruled that earprint evidence was held admissible, leaving
the duty of highlighting its limits to the adversarial system itself through a proper voir dire or at
trial (that decision was confirmed in another recent Appeal case R. v. Mark J. Kempster10).
Following the Appeal decision in Dallagher, on demand of the prosecution in preparation of this
new trial, subsequent DNA tests were carried out on the lifted ear marks. The analysis showed a
partial non-matching DNA profile, which was immediately interpreted as proving that the
earprint was not Dallagher's. That causal relationship was trumpeted in the press and among
scientific commentators118. This led the prosecution to formally drop the case. Mark Dallagher
was freed in January 2004 after serving 7 years in prison.

In State v. Kunze6 the Court heard some twenty experts in identification evidence and came to
the conclusion that earmark identification was not a field that has gained general acceptance
among peers. The Court ruled that earmark evidence cannot be accepted as scientific evidence
under the Frye test. The re-investigation of this case led to the discovery of close neighbours
(close agreement between earmarks originating from different sources) among the potential
donors in that case96.

The use of the ear in forensic practice is described more generally by Swift331 who stressed upon
the disputed state of earmark identification. The following groups for internal and external
examination are given: congenital and genetic, identification, pathological processes, trauma and
estimation of the post-mortem interval.

Procedures of casting the external ear in a way that causes minimal distortion have been
presented in a medical context184,212 (for auricular prostheses).

An interesting article on ear identification in the particular case of an image from a surveillance
camera has been published143.

TOOLMARKS

Note that this section is restricted to toolmarks and we do not ambition to cover the intertwined
field of firearms identification. So restricted, our review will then be quite limited.

Daubert issues have led the entire firearm and toolmark profession to extensively review and
discuss its foundations. The peer review process of their professional journal has been
reaffirmed103. It also restored the ongoing debate regarding the identification criteria and its
description, the process being either 1) purely qualitative in the examiners perception; 2) both

23
qualitative and quantitative in the examiners perception or; 3) both qualitative and quantitative
through actual recording of runs of consecutively matching striae (CMS). For toolmarks, the case
against Ramirez has been an additional catalyst238. The Supreme Court of Florida rejected
testimonies regarding toolmarks on cartilage because in their opinion they did not satisfy
rigorous Frye1 standards for reliability. Rosenberry published a perfect guide for examiners to
envisage a Daubert hearing280. The paper gives guidance to the relevant literature and an
adequate assessment of proficiency testing results.

A review of firearm and toolmark identification is proposed by Nichols247 adding 22 references

to a previous paper246. The introduction paper by Miller also constitutes a key contribution to the
field, especially for training223. We also recommend the update to the tool mark index listing the
recent references of toolmark papers126.

Nichols also published a full description of CMS theory applied to firearms and toolmarks248
which is well complemented by the papers by Moran235,237 and Tomasetti349 who exposed the
benefits of CMS in the current climate of stronger scrutiny by judiciary. A practical example on
magazine marks has been published by Moran also234.

Individuality of marks left by screwdrivers and its relationship with manufacturing processes has
been given by Lee195. The study of marks left by consecutively manufactured chisels showed that
each chisel produced individual and identifying characteristics107. No carry-over of features
occurred due to the finishing process of the tools. An identification error rate (0.78%) on knife
marks has been assessed through the Knife Identification Project345. Wounds caused by hacking
using machete, cleaver and axe weapons and the characteristics of each weapon type on bone
have been investigated144. Stone published an attempt to apply statistical modelling to the field of
toolmarks326. We applaud the effort but urge the reader to be very critical towards the simplistic
statistical model put forward. That contrasts with the paper by Warniment exploring ways to
assess "negative findings" and their influence on the conclusion about the alternative
proposition365.

Following comments published in INTERface232,364, a recent paper tried to bring the community
to a Bayesian approach81. Some skeptical responses followed233,236,245.

The examination of locks to distinguish between the wear of the original key, the marks left by
copied keys and the marks left by a lockpick is explained using a case example by Ryds285. In the
case described, once the marks on the locks had been determined to come from a copied key
rather than a lockpick, the original key presenting the marks of the copying process has been
found. The author insists that statements about the unauthorized opening of a lock or cylinder
using a copied key should be verified by complementary findings. The restoration of a painted
registration number is described344.

Several toolmark casting materials have been assessed by Sester and co-worker305in function of
ease of application, setting time, cast precision, stability over time, cost and toxicity. None of the
products tested offered advantages in all aspects: each product having its own benefits in
function of the task at hand. A physical model had been proposed to explore penetration of
casting material137. The results highlight the need for precautions to avoid the enclosure of air in
order to ensure accuracy.

Non-contact laser profilometry has been tested as an alternative to visual examination for
extrusion marks in plastic bags43,44. Pigment bands, surface scratches, fisheyes, arrowheads and
extrusion lines were detected. The reported principal advantage of this method above visual
inspection is that the quantitative information on extrusion marks and the comparison algorithm

24
used are more objective than visual inspection. Van Beeste et al.356 have published a detailed
paper outlining the key elements of transparent bags examination. The paper covers the analysis
of the seals, the different types of identifying marks and measurements (some using a capacitive
sensor for measuring surface profile (Octagon® profiler)).

Identification possibilities of marks from working gloves are investigated by Ostrowski253, who
gives examples of the type of impressions that can be left by the different kinds of working
gloves presented, and of fabrication defects that may be visible on impressions. Marks left by
computerised milling processes on dies used for example to prepare Ecstasy tablets have also
been studied showing their differences but also similarities182. Very interesting manufacturing
features on tabloid newspapers have been presented by Craythorne89. Some of these features
(especially the marks left by the tabloid slitter) allowed conclusive association between sheets by
physical fit. To handle the problem of tag switch on cattle, Nic Daeid and her colleagues
elaborated a damage databases of tags that had been subjected to wear and tear, tags that had
been assembled incorrectly and tags that had been separated and then reassembled244. It was
found that the marks found on the abattoir tags differed greatly from the marks found on the
separated tags. However some of the marks found on the separated tags were similar to marks
found on the tags that had been assembled incorrectly.

Progresses on the development of computer based algorithms to handle toolmarks have been
presented both in 2D105,140-142,297 and 3D202. Advances in computer technology will bring new
opportunities to both operationally and within research167. We would like to draw the attention of
the every rich work by Thali and co-workers on 3D-CAD supported photogrammetry techniques
applied to various injuries marks on bodies 338,339,341. The instruction manual by Brueschweiler
and colleagues is also highly relevant here 66.

LIP- AND BITEMARKS

Before focusing on the relevant marks, we noticed some publications on odontological

identification that add to the debate regarding identification criteria. In the context of the
identification of the deceased, an article based on a review of 690 cases from the archives of the
Forensic Odontology Unit of the University of Adelaide has been published15. The results
showed that when more than 12 concordant features were observed, identifications were more
often made than with less than twelve points. However, identifications were made with less than
twelve points, and there were cases where more than twelve points did not lead to identification.
The authors conclude that there is no basis to define a minimum number of concordant points
necessary for odontologic identification. Another article16, again on the ante-mortem/post-
mortem comparison of odontological records, examines the variability of dentition based on
dental treatment notes and/or charts (as opposed to dental radiographs). It was shown that
combinations of missing, filled, and unrestored teeth were very individualistic and an excellent
source for forensic identification. Age estimation from dental features has been described using
five case reports261. The reliability of identification using digitized autoradiographs has been
tested using a web-based survey270. For the increase of readiness of dental personnel in the case
of a mass disaster, exercises staging such a disaster are proposed267,268.

Lipmarks

A review on lip marks has appeared31. As with other impression areas, a void concerning the
interpretation of any concordances is highlighted by the author: the scientific admissibility of
lipmarks in court must be accepted, and this acceptance needs research in several areas. A
general overview of cheiloscopy is also proposed309. The heritability of lipmarks was
examined252: First the general shape of the lips was compared between the members of a family

25
(3 generations), then the patterns observed on the lip, and finally the individual features. The
author concludes that lip shape is predominantly inherited from the mother, as are patterns,
whereas the individual (according to the author) features are inherited from the father most often.
The author considers to have proven the inheritance potential in the case of lip prints.

Bitemarks

A review concerning the scientific basis for human bite mark analysis is proposed by Pretty and
Sweet265. They stress the lack of a fully established scientific basis. Recent observations of close
neighbours264 (close agreement between bite marks originating from different sources) have led
the authors to call for a renewed interest in researching the replication of dental features on
human skin and to raise a cautionary note on claiming individuality in terms of the suspect’s
teeth rather than the pattern they make on the bitten substrate. Distortion in bitemarks is
discussed by Sheasby and MacDonald, who differentiate between distortion due to the bite being
made and distortion introduced when the bitemark is being examined or recorded306. Missing
information concerning bitemark distortion in human skin is deplored by Whittaker373. The case
against Krone retained of course our attention. Krone has been freed in April 2002 after serving
10 years in prison. In the case, the Arizona Supreme Court's en banc (State v. Krone, 182 Ariz.
319, 897 P.2d 621 (en banc, 1995)) decision said that the physical evidence could neither
exclude not include Krone as the perpetrator, and without the bite mark evidence the State had
no case (www.forensic-evidence.com/site/ID/bitemark_ID.html).

An article, addressed to medical examiners as they often are the first to see these wounds,
describing bite injuries, collection of evidence and comparative analysis methods has
appeared266. Reasons for biting behaviour are discussed by Webb and co-workers who conclude
that behavioural data in relation to biting is missing366.

The accuracy of bitemark analysis has been investigated24 in the course of a workshop by
comparing the conclusions reached by certified forensic odontologists. The 32 examiners had an
experience ranging from 2-22 years. They were asked to rate their degree of certainty that a
bitemark was actually shown, and to assess the forensic value of the 4 bitemarks submitted based
on photographs and a dental stone cast for one of the bitemarks. 7 dental models (three of which
did not correspond to any of the marks) were also supplied, and the examiners were asked to rate
the comparisons of the marks and the models. Analysis of the results was carried out using a
ROC analysis, resulting in an accuracy score of 0.86. Accuracy scores were correlated with the
bitemark certainty and forensic value previously assessed, but not with examiner’s experience.
Two studies examining whether ABFO (American Board of Forensic Odontology) certified and
non-certified forensic odontologists differ as to their following the ABFO guidelines in the
collection of victim bitemark evidence218 and suspect evidence263 have been carried out. The
results show that the groups do not differ much, and both follow routinely these guidelines.

A web-based survey of 72 odontologists’ opinions concerning bitemark analyses showed that

while 91% of respondents believe that the human dentition is unique only 78% believe that this
uniqueness could be represented on human skin during the biting process. 70% believed that they
could positively identify an individual from a bitemark, while 22% found a statistical tool more
appropriate for bitemark conclusions260.

Evaluation of the efficiency of digital bite-mark overlays as a technique of comparison is

provided262.

26
Evidence collection concerning bitemarks is reviewed using case examples by Bernitz and van
Niekerk41. A protocol for evidence collection is proposed in order to avoid missing information
which makes impossible adequate analysis in bitemark cases.
Different methods for comparisons in bite mark analysis exist and have been compared183.
Among direct comparisons between suspects’ models and bite marks, traced overlays and
photocopier-generated overlays, the last method resulted in more correct matches than the other
two in this study. The problem of the visibility of ‘white fillings’ and their examination using
quantitative light-induced fluorescence is described and evaluated269.

Borgula and co-workers52 examined the analysis of Streptococci in human bites for forensic
purposes. They showed that on average over 1000 bacteria were recovered 24 hours after the bite
if the site was left undisturbed. Streptococci could also be recovered from bites in various
fabrics. Genomic profiles of the bacteria could be identified exclusively with the teeth of the
individual responsible in this study. A very simple method for the evaluation of bitemark
evidence has been published113.

The possibility of presenting bitemark evidence using Bayes theorem (e.g. the likelihood ratio)
has been examined178, and some of the limitations of such an approach are shown. The authors
conclude that the use of the likelihood ratio cannot helpfully be used for bitemark evidence. It is
true that unfortunately statistics have been very poorly presented in court when associated with
bitemarks210.

Techniques for the photography of bitemarks avoiding perspective and parallax distortion of the
image due to inaccurate positioning of the camera, the object or the reference scale, are
presented57. Methods for the correction of perspective distortion by digital editing techniques are
discussed. Digital methods in dental identification of human remains have been discussed58,160,
as has the use of optical 3D surface scanning for skin and bone injuries338 and 3D CAD
supported photogrammetry341 for bite marks.

In order to identify missing children, tooth prints are now used in addition to photographs,
videos, and fingerprints240.

TIRE IMPRESSIONS

Apart from the book by Nause243 we introduced before, Bessman and Schmeiser report a survey
on tire tread design and tire sizes in Iowa on 1250 vehicles45. Combinations of different tire tread
designs or sizes on a given vehicle are the focus of this survey. It is found that with respect to
tread design, 72% of the vehicles examined have four tires with the same tread design, and 14%
have two pairs of tires with the same tread design. The remaining have either three tires the same
and one different, two the same, the two remaining different from each other, or four different.
With respect to size, 97% of all cars have four tires with the same tread size, 1.6% have two
pairs, 1.4% have three the same and one of a different tread size, and finally one observation
(0.08%) was made of a car with three different tread sizes.

Techniques for casting comparison tires using expandable polyurethane foam, dental stone and
Mikrosil have been proposed and compared386.

The differentiation of tire rubber samples by attenuated total reflectance (ATR) spectroscopy,
diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and pyrolysis-gas
chromatography/mass spectrometry (Py-GC/MS) has been tested289. Only Py-GC/MS showed
good results. The authors conclude that it should be used as a stand-alone technique.

27
CASE REPORTS

Two unusual identifications of fingermarks are reported by Reneau273, both cases involved a
very limited number of minutiae. Latent mark development on paper towels using ninhydrin has
been successful295. Fingermark development on human skin using CA and black magnetic
powder followed by casting is described379. A case where the defence alleged that bleaching after
ninhydrin had occurred, in order for the police to deposit a false fingermark, is presented199. The
authors find that removal of ninhydrin treated marks using bleach is possible, but that the
bleached zone is seen in luminescence mode. Under-inked known prints have been developed
using ninhydrin254. The removal of excess CA from a mark on a knife blade by repeatedly lifting
the mark has been successful133.

Keith170 reports a shoesole impression identification, where the mark was found on a corduroy
cushion. Shor and coworkers report a case where a physical match between insole and shoe was
found307.

The identification of passengers after the crashes of two airplanes dental (and dermatoglyphic)
methods is described by Brannon59,60. A historical case pertaining to forensic dentistry is
presented87. Analysis of bites on dead bettongs in South Australia allowed identifying feral
domestic cats as the likely cause of these deaths152. A case151 where initial examination revealed
a bite mark, which was later determined to be due to a corrugated bottle top, shows the
importance of a careful assessment of injuries. The documentation of a knife wound to the aorta
using Computed Tomography is reported340. The identification of a bear that had killed a young
man has been reported27. The identification of a bite mark in cheese using a silicone rubber cast
is reported40.

Three case reports illustrating the use of anthropometric data based on photographic evidence
have been presented132.

Damage on a paper towel has been investigated and the conclusion was that the damage was due
to cleaning of a pointed and sharp object75. In addition, the authors observe that paper towels
behave quite similarly to fabric to the damaging action of cutting tools.

Walsh reported on a case where pattern matching has been used to associate a paint flake
recovered from a suspect’s address to its source, a fractured weld bead of a gun safe door363. The
pattern on the rear surface of the flake corresponded to the pattern of the cooled metal on the
surface of the weld bead. The evidential significance is discussed in relation to how these
patterns are produced.

An unusual oxidation type and small rounded cavities were observed in a light bulb following
the discovery of a crashed car in a gravel pit37.

The use of Pacemaker stored Event Records for the 40 hours preceding the beating to death of a
victim having a pacemaker has been described230.

MISCELLANEOUS

Image processing and pattern recognition techniques with applications in video image
processing, camera identification, toolmarks, shoemarks, cartridge cases and drugs/pills has been
presented124. The possible ways forensic image databases can function have been discussed125.

28
It has been tested whether the use of an electro shock weapon leaves marks on skin which can be
found in an exterior examination33. On pig skin such marks could not be produced postmortally.
On a living human subject, reddish skin marks which persisted for about 2 hours were observed.

The enhancement of the contrast of blood with respect to background is described in its
theoretical362 and practical361 aspects.

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46
 FIREARMS

— A Review: 2001 to 2004 —

Prepared by:
Gil Hocherman, M.Sc., Superintendent
Arie Zeichner, Ph.D., Commander
Tzipi Kahana, Ph.D., Superintendent

Approved by:
Elazar (Azi) Zadok, Ph.D.,
Brig. General, DIFS Director

ISRAEL POLICE
Investigation Department
Division of Identification & Forensic Science (DIFS)
National Police HQ Jerusalem 91906 Israel
Tel: 972 – 2 – 5309410
Fax: 972 – 2 – 5308688

47
CONTENTS

INTRODUCTION

FIREARMS – BALLISTICS:

Firearms
Firearms Identification
Homemade Firearms
Non-Lethal Weapons

Ammunition
Reference Collection
Interior, Exterior and Terminal Ballistics

Equipment & Techniques

Ballistic Databases
Two Dimensional (2D) Automated Comparison Systems
Three Dimensional (3D) Systems
Crime Scene Reconstruction
Equipment

Professionalism
Education
Law Relating to Firearms
Expert Witness Testimony

FIREARMS – CHEMISTRY:

Compositions, classification and interpretation

Methods and instrumentation
Distribution of GSR particles in the surroundings of a shooting firearm, their
sampling and persistence on different surfaces
Proficiency tests for GSR analysis by SEM/EDX
Detection and analysis of gunpowder (propellant) residues on suspects
Estimation of shooting distance
Chemical analysis for associating firearms and ammunition with gunshot entries
Estimation of time since discharge

FIREARMS –WOUND BALLISTICS

48
INTRODUCTION:

This report covers advances in scientific methods applied to forensic issues (firearms ballistics,
chemistry and wound ballistics) reported since the 13th Interpol Forensic Science Symposium in
October 2001.

A literature review was conducted covering articles published in the principal forensic journals
since 2001.

Following are the data sources and major forensic journals which we used in order to create this
review paper:

o The FORS Forensic Bibliographic Database

o Journal of AFTE (Association of Firearms and Toolmark Examiners)
o Journal of Forensic Sciences
o Forensic Science International
o Wound Ballistics Review
o American Journal of Forensic Medicine & Pathology
o Science and Justice, Forensic Science Society, Harrogate, UK

Most of the abstracts, which appear in this review paper, are discussed in the speaking
presentation. Attached is the Reference List, which contains all of the articles that were
published since the last Interpol Forensic Science Symposium in the principal forensic journals.

We would like to apologize to all the labs and authors whose articles are not mentioned in this
report and in the speaking presentation. Also please, excuse any typographical mistakes.

FIREARMS – BALLISTICS:

The topic of firearms ballistics can be divided into four main issues- firearms, ammunition,
equipment & techniques and professionalism. Each one can be further divided into the following
sub issues:

Firearms

Firearms Identification

The main field of the ballistic expert's work is identifying firearms. The first stage involves
classifying the firearm into firearm types: pistols, rifles, machine guns, etc. The next stage is to
identify the sub-class characteristics of these types, for example identifying a semi-automatic
gun with a CBP (Colt Browning Patent) mechanism such as Colt 1911 pistol. The final stage
involves the absolute identification (individual characteristics) between a specific firearm and
bullets and cartridge cases. The origin of these characteristics stems from the manufacturing
processes and maintenance of the firearms.

The field of identifying firearms is quite conservative. The mechanical mechanisms, which take
part in the firing process, are known and innovations are rare. The expert however must be
familiar with the different firearms, so that when these firearms or their products
(bullets/cartridges) arrive to the lab, he/She will be capable of identifying their source.

A Comparatively large number of papers in this literature scan (approximately 1/3) deal with
identification issues. Many studies are case reports and technical notes regarding unique

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characteristics of firearms and their comparative value. Other studies involve different methods
to calculate the minimum number of identification marks and their values in that process of
positive comparison.

An ballistic expert’s knowledge of technological developments regarding the production and

manufacturing processes (such as lasers, CNC methods and castings parts), as well as advances
in material science (such as composite materials and polymers) is essential. The ability to
identify and understand these new advancements is of critical importance to the firearms expert
(Ref 1-41).

Homemade Firearms

Another field in the expert’s work is examining "out of the ordinary" exhibits. These are the
exhibits in which the process of identification is sometimes difficult, especially at the first stage
of the identification (as previously discussed).

These homemade firearms, known as “zip” guns, consist of all the components of a regular
firearm: a circular barrel, a trigger, a firing pin and mechanisms of loading and maintenance. Use
of a simple metal pipe as a barrel (even without lands and grooves) and an iron-sharpened pin as
a firing pin (a simple nail or screw) are ideas borrowed from existing and proven firearms.

The expert should be able to determine if the weapon he/She is examining, which may not even
look like a weapon, can be legally regarded as a firearm. In order to examine these homemade
firearms, the expert must be familiar with the specific examining procedures. The right
ammunition must be chosen in order to precisely reconstruct the crime scene. A scientific
conclusion should be based on the characteristics of speed, penetration energy, etc.(Ref 42-57).
In the literature review, we can see that the amount of reports has grown in this field. This may
be due to the strong enforcement of security agencies regarding the laws related to ownership,
accessibility and use of firearms. This may be related to increased level of international terrorism
and its grater public awareness.

Non-Lethal Weapons

The use of firearms frequently leads to irreversible consequences (namely, death). In many cases
in which security forces are involved or in the case of self-defense, there is no need to use lethal
weapons in order to neutralize an attacker. For this reason the branch of “non-lethal weapons”
has developed. The use of these weapons is for neutralizing an attacker for a certain period of
time without causing cumulative or permanent harm. These neutralizing methods consist of
chemicals such as gases, which cause burning sensations, tearing of the eyes and asphyxiation.
Another method uses a physiological element, which neutralizes an attacker by effecting
muscular contraction, which leads to momentary fainting. The instruments used to deliver the
high voltage necessary to bring about this effect are known as shockers. Other methods employ
mechanical element, such as a net, which limits physical motion. Still others use adhesive
materials (foams).

A number of articles have been written on this subject focusing on methods of non-lethal
weapons use and health influences on persons targeted by them. Constitutional and social
implications, which derive from using these weapons, have also been reported (Ref 58-63).

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Ammunition

The firearms expert should know his/her way through firearms as well as ammunition. The
expert must be familiar with the complex production procedures, production tools, and their
effect on ammunition in the sense of its components, the toolmarks and the effect on the ballistic
characteristics.

Reference Collection

The ballistic lab must be equipped with an ammunition collection in order to perform its work.
Among the professional demands, the expert must identify and characterize specific ammunition,
for example, infrequently used ammunition, outdated ammunition, new ammunition, variation of
hunting loads (size and number of the pellets), sub-sonic ammunition, etc. This reference
collection is also used for testing ballistic characteristics, such as velocity, penetration and bullet
fragmentation, as well as comparison between manufacturing toolmarks in order to prevent
mistaking them for individual marks left by the shooting process. The reference collection
should be composed of a literature collection, which contains technical details from the different
manufacturers that are organized in a convenient searching method.

Review of the articles in this field, concentrates on new and unique types of ammunition. These
articles contain ballistic characteristics, such as caliber data, bullet weights, ballistic coefficients,
gunpowder composition, shelf life and storage conditions etc, (Ref 64-87, Ref 97-100).

Interior, Exterior and Terminal Ballistics

The field of ballistics is divided into three sub-fields:

Interior Ballistics – The study of the motion of the projectiles within the firearm from the
moment of ignition until it leaves the barrel. It includes analysis of friction, momentum, effects
of the gaseous environment, spiral movement, etc. Exterior Ballistics – This part deals with the
behaviour of the projectile after it leaves the barrel until the moment it hits the target. It includes
movement in the air, velocity, stability, gas effects, gravitational effects, etc.

Terminal Ballistics –The study of the projectile’s impact on the target. It is known as “wound
ballistics” whenever the target is a living tissue (this will be discussed later on.)

The articles in this field are a collection of tests and data related to various types of ammunition.
These diverse research methods detail the equipment needed to measure ballistic characteristics,
experimental conditions used for the testing and the special computer software that control and
analyze terminal ballistics. Specific situations such as the use of incorrect caliber and its effect
on ballistic characteristics, such as velocity, penetration energy, and lethality, as well as the
toolmarks imparted on the ammunition are also mentioned (Ref 88-91). Some articles report on
handmade ammunition and its ballistic characteristics (Ref 92-93).

Equipment & Techniques

Ballistic Databases

The increase of usage of semi-automatic and automatic firearms in crimes on the one hand, and
computerized techniques development on the other has lead to the rapid establishment of ballistic
databases to help the forensic scientist.

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These databases allow the law enforcement agencies to interrelate cartridges and bullets from
various crime scenes as well as suspected firearms. A secondary use of these databases is for the
identification of the changing trends of firearms involved in crime. The advantages of these
systems are their power to deal with the growing number of crime scene exhibits, as opposed to
previous lab procedures which lead to delays, backlogs and prioritization.

Articles dealing with the procedures of use of these databases in different police forces have
been published. The efficiency of these systems is checked continuously and advantages and
disadvantages are monitored (ref 104-105).

Two Dimensional (2D) Automated Comparison Systems

Systems which automatically compare between firearm exhibits are based on two-dimensional
surface screening. The systems are able to deal with a large number of exhibits simultaneously,
but the human factor is critical in determining their performance. The procedure of inputting data
by the specific system operator, strongly affects the quality of the results. Aspects such as
keeping the surface parallel, correct orientations of the different areas of interest (firing pin–
ejector–breech face), degree of lighting, focus and correct determination of the area of interest
are crucial in systems performance. Research shows that a skilled operator can improve system
performance through proper data acquisition and their correct analysis. A number of research
papers describe the use of the two-dimensional system installations, like IBIS®, in different
locations as well as defining criteria for standardization of the input process (through protocols),
analysis and other methods. All these factors are interrelated and improve the output (Ref 106-
113).One important work describes the BRASSTRAX® system of FTI, currently considered the
next generation of two-dimensional systems. This system attempts to provide solutions for the
complex problems that were previously noted. In this system, the acquisition procedure is fully
automated and nullifies the "noise" (operator error) thus improving the results (ref 113).

Three Dimensional (3D) Systems

An automatic bullet comparison system, which is based on three-dimensional technology also

superior to the two-dimensional systems. The automatic system and the data acquisition phase
are more stable and less sensitive to "noise" caused by the operator. These systems are only in
the beginning phases of use in forensics ballistic labs. An example of such a system is the
BULLETTRAX® of FTI (Ref 113-115).

Crime Scene Reconstruction

A number of articles deal with the reconstruction of crime scenes. For example, typical behavior
of the bullet flight and its impact with different targets, such as glass, car parts etc. The
importance of these research articles is the establishment of reference data for future incidents as
well as supplying an explanation about the testing methods; the use of scene reconstruction
methodology can serve the firearms experts a useful demonstrative tool in court (Ref 94-103,
151-157).

Another field in which a three-dimensional system is used is in crime scene reconstruction

(distances and angles). Apart from its capability to create visual simulations, which are usually
used for court presentations, it also helps the investigator to become more confident of different
presumptions and crime scene interpretations. This system is actually a combination of CAD
(computer aided design) and animation software (ref. 116-117).

Equipment

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Control & Management systems – Computer software helps the expert or the lab manager to
control great amounts of exhibits and their output. These types of software are the FIMS®
(Firearms Information Management System) or EUROBIS® (European ballistic information
system on IBIS platform) or GRC® (General Rifling Characteristics) which are specific to the
ballistic field ( Ref. 113).

Bullet Traps – Bullet traps are used to stop a bullet that has been shot without causing physical
damage or leaving additional marks apart from the barrel signature for comparison use (Ref 120-
121).

Ballistic Gelatin- Ballistic gelatin is widely used by forensic scientists, firearm examiners,
wound ballistics experts, ammunition manufacturers, and those who are involved in the
evaluation and procurement of ammunition for law enforcement agencies (Ref 118).

The Oehler M43 Personal Ballistics Laboratory (PBL) System- PBL is capable of: determining
ballistic coefficients for various projectiles, measuring pressure, velocity and other internal
ballistic properties, comparing propellants, and measuring velocity loss when projectiles
penetrate or ricochet off various objects (Ref 119).

High Speed Photography System- A high-speed photography system is used for the analysis of
discharge of firearms (Ref 122).

Serial Numbers Engraved by Laser- Marking serial numbers by laser on critical parts of the
firearm that are used during the process of shooting. Their obliteration would render the firearm
inoperable (Ref 123).

Professionalism

Education

Weapon experts must go through a extensive training process which includes acquiring a deep
theoretical and practical knowledge of the different types of firearms and ammunition. The
expert must learn the different comparison criterions, the equipment and their historical
development, and the manufacturing processes including the development of material sciences.
The literature in this field is extensive, and today, in the Internet era, it is important to select the
relevant data from the huge amount available.
Many works are published these days in the field of expert training and it is possible to see a
trend towards specialization. This is due to the standardization of lab procedures and lab
accreditation. Another contributing factor is the growing maturity of the judicial courts,
prosecution and other law agencies, which understand the superiority of forensic interpretation of
exhibits as compared with other types of evidence (Ref. 124-134).

Law Relating to Firearms

Laws and definitions in different countries, vary in regard to firearms, licenses, holding and even
use of the firearms and ammunition. The law sometimes requires updating, due to natural
changes of society and technology, overall it is a complex and long procedure (Ref. 143-145).

Expert Witness Testimony

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An important part of the expert's work is giving testimony in court explaining his/her findings to
a judge and/or jury (depending upon the country). This testimony must include presentation of
the scientific basis of the method, the procedures, the equipment, the management of work sheets
and raw data, and analyses and final conclusions.

The forensic expert should be able to summarizes the scientific processes and demonstrate them
to the court. Part of the process of acceptance the credibility of the expert is by questioning the
expert’s skill level and professional knowledge. This may include innovation in equipment,
methods in theories used in fieldwork and validity in the scientific community (Ref. 146-150).

FIREARMS-CHEMISTRY

During discharge from a firearm, various materials evolve from the muzzle (accompanying
projectile) and other possible openings in the firearm. These materials include primer and
gunpowder (propellant) residues as well as metal particles from the projectile and from the
cartridge case. Throughout this report, all these materials will be called firearms discharge
residues (FDR) (1,2), while the term gunshot residues (GSR) will refer to primer residues only.
In the relevant literature, sometimes inorganic GSR or inorganic components refer to primer
residues and organic GSR or organic components refer to gunpowder residues.

Primer (GSR)

Compositions, classification and interpretation

The problem of classification of various compositions of GSR particles continued to be of

interest for research, in particular the alleged “unique” compositions to GSR: (a) lead, antimony
and barium, (b) antimony and barium. This problem was discussed in two recent reviews on
GSR: by Romolo and Margot (1) and by Zeichner (2). Further to the studies, reported previously,
showing that particles of composition (b) might be found, although in very small amounts, in
residues from fireworks and among particles collected from automobiles, Torre et al. (3),
reported that some types of brake linings contain lead, antimony and barium and they can
represent a source of particles showing GSR-like elemental profiles. Most of these particles
could be easily discriminated from GSR by means of the high levels of iron or the presence of
“prohibited” elements in the EDX spectrum. However, particles with iron at minor or trace levels
and lacking “prohibited” elements were also found but did not have spherical morphology. In
view of these findings, the morphological criterion becomes more important for identification of
GSR than was suggested (4).
Kirkbride et al. (5) studied the distribution of lead and barium in GSR derived from .22 caliber
rimfire ammunition. The study confirmed the nonhomogeneous nature of GSR. Coumbaros et al.
(6) reported for the first time about glass-containing GSR particles in .22 caliber ammunition
using SEM/EDX and TOF-SIMS for the analysis.

Lebiedzik and Johnson (7) reported that indicators of the type of weapon and ammunition used
in firing can be obtained from the distribution of GSR shapes and compositions. In a series of
studies, Brozek-Mucha et al. (8-10) attempted to evaluate the possibility of differentiation
between various types of ammunition by means of GSR analysis with SEM/EDX.

There is no consensus among the forensic laboratories regarding the number of particles needed
to confirm the presence of GSR. The controversy among the experts on this question is still
unresolved (Personal communication, 8th Firearms Working Group meeting, Brugge, Belgium,
September 2001). There is much more agreement regarding the wording of reports when a lab

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decided that there is a positive result. In such a case the statement: “The sample is consistent
with the suspect having discharged a firearm, having been in the vicinity of a firearm when it
was discharged, or having handled an item with GSR on it” resembles the phrasing of most of
the labs (2). In any case, it is very important to compare the GSR compositions found on a
suspect to the GSR compositions of the spent cartridge cases (if found) at the scene of crime as
well as to the GSR compositions in the suspected firearm (if apprehended). Sometimes the
evidential value of such comparisons may be much higher than the degree of “uniqueness” of the
GSR particles found on the suspect, for instance, if the GSR particles found on a suspect are
consistent with the GSR in the spent cartridge cases of a rare ammunition.

Methods and instrumentation

In casework, SEM/EDX continues to be the method of choice for the GSR detection and
identification in samples from suspects of shooting, due to its higher evidential value as
compared to the bulk methods of analysis (1,2). Continuous improvements in the SEM and the
EDX technologies are also reflected in the GSR analysis by SEM/EDX. Nowadays most of the
manufacturers of the SEM/EDX equipment offer automated search systems for GSR particles,
which make the analysis much easier as compared to manual search, which is very tedious.
Nevertheless, even with the automated search systems the analysis may be quite long, amounting
to several hours per square centimeter of a sample depending on the surface density of particles
having high average atomic number.

Mastruko (11) demonstrated the use of an environmental SEM (ESEM) for the GSR detection
and identification. Ikeda et al. (12) demonstrated the application of SEM/WDX for detection and
identification of GSR particles from hands, hair and clothing. The method has been implemented
in casework. As was already mentioned in the previous paragraph, time-of-flight secondary ion
mass spectrometry (TOF-SIMS) was studied recently for the analysis of GSR (6,13). The method
may be used as a complimentary technique to SEM/EDX, since it has the capability of depth and
trace elements profiling. Trombka et al. (14) constructed a breadboard model of a portable XRF
system using room temperature silicon and cadmium-zinc telluride (CZT) detector. This system
is similar to those being developed for planetary exploration programs and was aimed to be used
in the crime scene for the examination of GSR blood and semen. Preliminary experiments were
conducted, however it appears that additional research is needed before the system may be
implemented in casework.

Recently, the U.S. Department of Energy’s Sandia National Laboaratories, working with Law
Enforcement Technologies Inc. announced the development of the ISID TM-1 (Instant shooter
ID Kit). It appears that it is an updated version of the “Dermal Nitrate” or “Paraffin” test. As in
the case of the “Dermal Nitrate” test it was argued that “The concerns of non-specificity of the
ISID TM-1 kit need to be critically evaluated in light of its potential usefulness in the field and
any legal issues associated with its documented “false positives” ” (15). Steffen and Niewhoner
(16) conducted a study to visualize zinc containing GSR particles (lifted from various surfaces
by Filmolux® transparent adhesive film) using modified dithizone and xylenolorange tests.

Distribution of GSR particles in the surroundings of a shooting firearm, their sampling and
persistence on different surfaces

Kolar et al. (17) conducted experiments to study the distribution of GSR particles in the
surroundings of shooting firearm (pistol CZ 85 caliber 9 mm Luger). The particles were
collected from accumulating targets at the height of 10 cm from the floor. They found that
maximum number of GSR could be found in the right front quadrant at a distance of 2-4 m with

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respect to the shooting firearm position and shooting direction. GSR particles were even found in
distance 10 m from shooting firearm.

Sarkis et al. (18) reported a new method for collection of GSR from the hands of shooters for the
analysis by ICP/MS. The sampling procedure is based on EDTA solution as a complexing agent
on moistened swabs. They found that this solution was superior to nitric acid solution or
deionized water as a collecting technique for GSR.

Schutz et al. (19) conducted a study to evaluate parameters influencing GSR retention on
shooter’s hands. The following results were reported: (a) the amount of GSR on hands or other
skin surfaces varies with the type of firearm and ammunition used. (b) An exponential loss of
GSR occurs with time, independent of factors such as the size, the shape and the chemical
composition. (c) No preferential retention of GSR results according to the size, the shape and the
chemical composition.

Proficiency tests for GSR analysis by SEM/EDX

Niewhoner et al. (20,21) have continued to conduct ENFSI proficiency test programs on
identification of GSR by SEM/EDX. Since the 13th Interpol Forensic Science Symposium, two
proficiency tests were conducted: the GSR2001 (20) and the GSR 2003 (21). In these tests for
the first time “synthetic GSR particles” (pseudo-particles) consisting of the three-element
composition (PbSbBa) were prepared by microelectronics technology on the stubs. All the
participating laboratories received the same samples, namely stubs with the same number of
pseudo-particles, in the same locations on the stub and with the same size distribution. In the
GSR2003 test the pseudo-particles of 2.4, 1.2, 0.8 and 0.5 micron size were prepared on the
stubs. The presence of sub-micron particles was very important for the performance assessment
of the SEM/EDX systems used by the participating laboratories. The results show that 75% of
the laboratories meet the proficiency criteria for detection of GSR particles having size of 1.2
microns or larger. However, the capability of detecting sub-micron particles has to be improved
(21).

Detection and analysis of gunpowder (propellant) residues on suspects

Numerous studies have been published on the analysis of propellant residues in the past,
however only a few of them (2) proposed operational methods (which have also been
implemented in casework) for sampling, detection and identification of these residues on
shooters and/or their clothing. The amounts of propellant residues that may be left on the
shooter’s hands several hours after shooting may be very small (normally in the nanogram
levels). Thus the sensitivity of the analytical technique is a crucial factor in its applicability for
the detection and identification of the gunpowder residues on suspects of shooting and their
clothing.

To the best of our knowledge, only two methods are used operationally for detection and
identification of propellant residues on shooters’ hands: high performance liquid
chromatography with a pendant mercury drop electrode detector (HPLC/PMDE) and GC/TEA
due to their high sensitivities i.e., between tens to hundreds of pg for NG, 2,4 DNT and 2,6 DNT.
The Forensic Science Service in UK employs the same method for sampling and analysis of
traces of explosives, primer GSR and gunpowder residues on suspects and their clothing (2). The
residues are collected from the hands, the face and the neck of a suspect by means of a swabbing
kit.

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Yu et al. (22) reported a novel method for detection and analysis of methyl centralite (MC), one
of the possible components in gunpowder, in swabs collected from shooters. The authors claimed
that they could detect MC on hands (without washing them) up to eight hours after firing, and
after washing them with water up to three times. A method in which the clothing is first sampled
by double-sided adhesive for GSR analysis by SEM/EDX, followed by vacuum collection for
propellant residue examination by GC/TEA, IMS and GC/MS was introduced recently into
casework in the Israel Police (23). Recently Zeichner and Eldar (24) reported a novel method for
extraction and analysis of gunpowder residues on double-side adhesive coated stubs. For the first
time the method enables analysis of propellant residues on a double-side adhesive coated stub
after it was examined for primer residues by (SEM/EDX). Thus, the probative value of the
evidence may be increased.

Micellar electrokinetic capillary electrophoresis (MECE) with a diode array UV detector

continued to be of interest for the analysis of the characteristic components in gunpowder
residues (25,26). In spite of the high discrimination power of the technique, it is not sensitive
enough to be implemented in casework for detection and analysis of propellant residues on
suspects or their clothing.

Detection of firearm imprints on the hands of suspects

Almog et al. (27-30) continued to study the reagent 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine

(PDT) and its analogues for visualizing iron traces on hands. PDT itself reacts with ferrous ion to
give a magenta complex. The formulation named “Ferroprint” which includes PDT and ascorbic
acid (as a reducing agent), has been in operational use in Israel since 1980.

In a study (28) involving 147 volunteers, including males and females, it was found that strong
and medium marks were developed (immediately after contact) on over 70% of the volunteers
without considerable difference between males and females. In this study, three analogues of
PDT were also examined on 15 volunteers. The obtained impressions were compared to the
magenta impressions obtained by PDT. In most cases the marks developed by PDT were more
intense and had somewhat higher resolution than marks obtained using the analogues.

Precaution is necessary when using the developed stain on the hand by PDT to provide evidence.
The firearm or any other object held must have a distinctive or characteristic morphology and the
pattern produced on the skin must reflect this if it is to be used as associative evidence. In the
more commonly encountered situation where there is a reaction, but where the pattern is less
distinct, the results may be useful, but only as an investigative aid. From casework experience of
using Ferroprint in Israel, it appears that most of the benefit of using the test is in confirming
suicides. It may also be useful in determining the murderer in homicide-suicide cases, where the
evidence at the scene of crime is impaired intentionally (27).

Estimation of shooting distance

Zeichner and Glattstein (31) reviewed the developments during the past 10 years on the
subject. The review discusses the examination of clothing targets, cadavers and exhibits that
cannot be processed in the laboratory. Color tests for gunpowder, lead and copper residues in
addition to visual/microscopic examination, remain the primary methods for estimating shooting
distance on clothing targets. Lifting of the gunpowder residues by an adhesive lifter from the
shot targets and applying the color test on the lifter improves the methodology for clothing and
introduces a new methodology for human body examinations and for exhibits that cannot be
processed in the laboratory.

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Carrol (32) and Shem (33) reported on the advantages of using the Marshall’s reagent: N-(1-
naphtyl)-ethylene-diamine dihydrochloride over the modified Griess test (using alpha-naphtol )
for gunpowder visualization in terms of visibility and increased contrast. Additional studies
concerning shooting distance on the human body will be reviewed in the chapter dealing with
“wound ballistics”.

Chemical analysis for associating firearms and ammunition with gunshot entries

There is no method to conclusively associate a firearm or ammunition to a gunshot entry. A class

characteristic linkage may be obtained by measuring the diameter of the gunshot entry and by
comparing chemical compositions of FDR in the bullet hole perimeter and around it, FDR in the
barrel of the weapon, FDR in the spent cartridge case and the composition of the fired projectile.
Also, unfired ammunition, if apprehended with the suspect may be analyzed for the above
purpose. The level of association will depend on the rarity of the examined compositions.
Analysis of all the components of the FDR (primer GSR, propellant residues and metal particles
from a projectile) may serve this purpose (2).

MacCrehan et al. (34-36) continued studies for analysis and comparison of fired and unfired
propellants. They found that compositional analysis of the propellant provides information that
can associate residue samples with unfired gunpowder. It was reported that qualitatively
identifying and quantitatively determining the additives in gunpowder to calculate a numerical
propellant (NG) to stabilizer ratio (P/S) may be a useful index in associating handgun-fired
gunpowder residues with unfired powder. In some cases, residues could be reliably differentiated
based on P/S and additive identity. Using ammunition loaded with known smokeless powders
containing different stabilizers, a sequence of shots was fired from a .357 magnum revolver, and
the muzzle exit residues were collected (35). Compositional analysis of the residues, both in bulk
and as single particles, showed only a trace of the previously fired powder in the first shot and
none in subsequent shots. These results are similar to those reported in the past (2). We are not
aware of any study that attempted to compare gunpowder residues in a firearm (e.g. barrel) to the
residues in the gunshot entry. This information could be very useful in assessing the potential of
linking a firearm with a shot target. Although it may be assumed from the reported results that
the composition of the propellant residues in a firearm should resemble the composition of the
last fired round, it is desirable to confirm it experimentally.

Compositional analysis of lead projectiles continued to be of interest for source discrimination.

These included elemental analysis of the lead alloy (37,38) and the lead isotope compositions
(39-42). It was shown (42) that it is impossible to completely remove lead deposits, the “lead
memory” in the barrel from previous shootings by mechanical or chemical means. Nonetheless,
it was found that lead deposits in the gunshot entries are similar in the lead isotope compositions
to the lead of the fired projectiles that hit the targets, in particular short distances.

Estimation of time since discharge

Andrasko and Stahling (43) continued to use the SPME technique for sampling and GC/TEA as
an analytical system to estimate time since discharge of pistols and revolvers. It was found that
the escape of the TEA 2 volatile compound from pistol and revolver barrels with time is rapid
compared to shotguns and can generally be measured for only a few days after the latest
discharge. Wilson et al. (44) adopted the SPME method for sampling the volatile product,
naphthalene in shotgun shells and analyzing it by GC/MS. They found that the escape of
naphthalene can be measured several weeks after the cartridge has been fired.

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FIREARMS – WOUND BALLISTICS

The topic of wound ballistics or terminal ballistics can be divided into two main issues; shooting
range and wound characteristics.

The determination of the shooting range is of paramount importance in gunshot wound

investigations; as a rule medical examiners estimate the shooting distance based on the
morphological characteristics of the wound and it's immediate tissues, Plattner and others, Bhana
et al, Prahlow et al and Verhoff and Karger' publications are but a few that deal with this aspect
of wound ballistics.

Much research has been conducted in the last years on the area of physico-chemical
determination of shooting range, various techniques such as energy dispersive x-ray fluorescence
spectrometry and nitrite residues are advocated by prestigious police laboratories all over the
world.

The literature in wound morphology, trajectory and the correlation between ammunition and
lethality is extensive. Unusual entrance, trajectories and exit wounds are described in detail, thus
enhancing the awareness of the investigators to atypical post-mortem findings as well as to new
types of ammunitions and their wounding effect (Ref. 1-26).

REFERENCES

Firearms –Ballistics

1. Wright-D-C; Individuality and Reproducibility of Striae on Plastic Wad Components

Fired from a Sawed-Off Shotgun, AFTE; 2003; V35 (2); P161-166
2. Dutton-G, Firearms Identification - Sometimes All Is Not As It Seems AFTE; 2003; V35
(2); P245-249
3. Jueckstock-G-E; Moline-K-W, Accidental/Unusual Discharge of a Jennings J-22 AFTE;
2002; V34 (3); P306
4. Drotz-W, Fibres on Bullets After Firing Through Textiles PROC-EUROPEAN-FIBRES-
GROUP; 2002; V10; June; P110-112
5. Haag-L-C, Once Fired, Twice Fired, More? A Novel Method for Assessing the Number
of Firings of Shotshells with Plastic Bodies , AFTE; 2002; V34 (1); P11-15
6. Argaman-U; Shoshani-E; Klein-A, A Suicide Bomber's Weapon, AFTE; 2001; V33 (4);
P335-336
7. Spinder-T, Suppressed Ruger 10/22, AFTE; 2001; V33 (4); P332
8. Monturo-C , Information on Hi-Point Manufacturing AFTE; 2003; V35 (2); P243-244
9. Shoshani-E; Argaman-U; Koffman-A; Giverts-P, A Shortened M-16 Rifle, AFTE; 2002;
V34 (3); P307-309
10. Anon, The Smallest Guns in the World?, Prohibited-and-Concealed-Weapons-Review;
2002; V7; P11
11. Rivera-G-C, Unusual General Rifling Characteristics in a Lorcin L25, AFTE; 2002; V34
(1); P52
12. Gibson-W-M, Bryco Arms Makes a Model Name Change, AFTE; 2002; V34 (1); P52
13. Bartocci-C-R, New Russian Assault Rifle, The AN94, AFTE; 2001; V33 (3); P275-276
14. Keisler-M; Fazio-J, Hi-Point Firearms Hidden Serial Number, AFTE; 2001; V33 93);
P273-274
15. Caunt-R, Interview with Sid Woodcock of Detonics Manufacturing Corp AFTE; 2001;
V33 (4); P354-358
16. Keisler-M-A, Maschinengewehr 08/15, AFTE; 2001; V33 (3); P256-257

59
17. Neel-M-T; Fullerton-A-T; Correa-J-J-J The Unique Modular System of the Infinity
Firearm, AFTE; 2002; V34 (2); P205-206
18. Nedivi-L; Giverts-P; Shoshani-E; Brauner-P, The Magal - A New Weapon in the Fight
on Urban Terrorism, AFTE; 2003; V35 (1); P72-73
19. Hayes-C-M, Personal Defence Weapons - Answer in Search of a Question? WOUND-
BALLISTICS-REVIEW; 2001; V5 (1); P30-36
20. Zielinski-K-R, Full-Auto Conversion of an Uzi, Model B, AFTE; 2002; V34 (4); P399-
400
21. Bartocci-C-R, Fire Control Part Variations in Colt M16/AR15 and Sporter Type Rifles,
AFTE; 2003; V35 (1); P12-18
22. DeFrance-C-S; Van-Arsdale-M-D Full Auto Conversion of Colt AR-15 and Norinco
MAK-90, AFTE; 2002; V34 (2); P170-171
23. Allen-S; Spinder-T, Full-Auto Intratec or Not, AFTE; 2002; V34 (1); P49
24. Shoshani-E; Nedivi-L; Giverts-P, Ejector's Cut-Out Marks in Shotguns and Their
Comparison Value, AFTE; 2002; V34 (4); P391-393
25. Bartocci-C-R, The Current Production ArmaLite AR-10 Series Rifle, AFTE; 2002; V34
(3); P312-313
26. Thompson-E; Wyant-R Sardius 9mm Semi-Automatic Pistol, AFTE; 2002; V34 (3);
P319
27. Amberger-R, Unusually Rifled Shotgun Barrel, AFTE; 2002; V34 (3); P311
28. Shoshani-E; Argaman-U; Hocherman-G; Koffman-A Metal Chip Marks on Fired
Cartridge Cases, AFTE; 2002; V34 (2); P172-174
29. Wallace-E; Rivet Impression in Bullet Nose, AFTE; 2002; V34 (2); P168-169
30. Register-R-E; Beach-G-T Unusual Breech Face on a Taurus Firearm...? , AFTE; 001;
V33 (4); P334
31. Moline-K; Identification of a Compensated Glock Pistol, AFTE; 2001; V33 (4); P333
32. Monturo-C; Breechface Marks of the Beretta Model 3032 Tomcat, AFTE; 2001; V33 (2);
P142
33. Bartocci-C-R; Characteristics of the 7.62 x 39mm Cartridge, Telling Whether a Fired
Cartridge Case Was Fired in an SKS or AK Type Rifle, AFTE; 2002; V34 (2); P144-147
34. Hocherman-G; Giverts-P; Shosani-E, Identification of Polygonal Barrel Sub-Family
Characteristics, AFTE; 2003; V35 (2); P197-200
35. Clark-J-R; An Interesting Magazine Mark, AFTE; 2003; V35 (1); P71
36. Coody-A-C; Consecutively Manufactured Ruger P-89 Slides, AFTE; 2003; V35 (2);
P157-160
37. Thompson-E; Wyant-R9mm Smith & Wesson Ejectors, AFTE; 2002; V34 (4); P406-407
38. DeFrance-C-S; Van-Arsdale-M-D Validation Study of Electrochemical Rifling, AFTE;
2003; V35 (1); P35-37
39. Cooper-M; Serial Number "Restoration" on a Colt All American Model 2000, AFTE;
2002; V34 (1); P48
40. Shoshani-E; Klain-A; Argaman-U Altering a Serial Number, AFTE; 2001; V33 (2);
P133-134
41. Klees-G-S; The Restoration of Obliterated Laser-Etched Firearm Identifiers by
Conventional and Alternative Decryption Methods, AFTE; 2002; V34 (3); P264-267
42. Hiss-J; Shoshani-E; Zaitsew-K; Giverts-P; Kahana-T, Self Inflicated Gunshot Wound
Caused by a Home-Made Gun - Medico-Legal and Ballistic Examination J-CLIN-
FORENSIC-MED; 2003; V10; P165-168.
43. Uner-H-B; Gokdogan-M-R; Cakan-H, Some Samples of Weapons and Instruments Used
as Weapon in Criminal Offences in Turkey,FORENSIC-SCI-INT; 2003; V132 (2);
March; P113-116.
44. Shakir-A; Koehler-S-A; Wecht-C-H, A Review of Nail Gun Suicides and an Atypical
Case Report, J-FORENSIC-SCI; 2003; V48 (2); March; P409-413

60
45. Desmarais-A; Attar-L , Alarm Pistols Firing 9mm K. (.380 A.C.P), J-ASSOC-
FIREARM-TOOLMARK-EXAM; 2002; V34 (4); P401-402.
46. Argaman-U; Shoshani-E , An Altered Revolver, AFTE; 2002; V34 (4); P394-395.
47. Ventura-F; Blasi-C; Celesti-R,Suicide with the Latest Type of Slaughterer's Gun, AM-J-
FORENSIC-MED-PATHOL; 2002; V23 (4); December; P326-328
48. MacDonald-M, Pen Guns and Zip Guns, PROHIBITED-AND- CONCEALED -
WEAPONS-REVIEW; 2002; V8; P15.
49. Hertel-G-W, The Safegom Revolver, AFTE; 2002; V34 (3); P320-321
50. Argaman-U; Shoshani-E, A Lethal Paint Pistol AFTE; 2002; V34 (3); P304-305
51. Shiers-A, Disguised and Converted Firearms: POLICE-REPORT; 2002; PN 1-4
52. Tyquiengco-J; Toves-E, A Homemade Firearm AFTE; 2001; V33 (3); P259-260
53. Argaman-U; Shoshani-E, Dangerous Walking Stick AFTE; 2001; V33 (3); P248-250
54. Grandy-J, The Construction and Relative Efficiency of a Homemade Sound Suppressor
vs. a Commercial Model AFTE; 2001; V33 (2); P103-111
55. Caunt-R,Dieseling of Airguns Using Commonly Available Fuels AFTE; 2003; V35 (2);
P167-173
56. Monticelli-F; Seidl-S; Betz-P, Air Rifle Injury With an Entrance Through the Nose: A
Case Report and Review of the Literature INT-J-LEG-MED; 2002; V116; P292-294
57. Bock-H; Neu-M; Betz-P; Seidl-S, Unusual Craniocerebral Injury Caused by a Pneumatic
Nail Gun , INT-J-LEG-MED; 2002; V116; P279-281
58. Anders-S; Junge-M; Schulz-F; Puschel-K, Cutaneous Current Marks Due to a Stun Gun
Injury, J-FORENSIC-SCI; 2003; V48 (3); May; P640-642
59. Buttle-J-W,'What's Good For Them Is Good For Us': Outside Influences on the Adoption
of Incapacitate Sprays by the British Police, INT-J-POLICE-SCI-MANAGE; 2003; V5
(2); P98-111
60. Turner-M-S; Jumbelic-M-I, Stun Gun Injuries in the Abuse and Death of a Seven-Month-
Old Infant, J-FORENSIC-SCI; 2003; V48 (1); January; P180-182
61. Haag-M-G; Haag-L-C, Skin Perforation and Skin Simulants, AFTE; 2002; V34 (3);
P268-286
62. Ng-Walali-P-M; Ohtsu-Y; Muraoka-N; Tsunenari-S, Unusual Homicide by Air Gun with
Pellet Embolisation, FORENSIC-SCI-INT; 2001; V124; P17-21
63. Fish-R-M; Geddes-L-A, Effects of Stun Guns and Tasers, LANCET; 2001; V358;
September; P687-688
64. Henderson-E-A; A Tour of Federal Cartridge Company, AFTE; 2002; V34 (3); P316-318
65. Koons-R-D; Grant-D-M; Compositional Variation in Bullet Lead Manufacture; J-
FORENSIC-SCI; 2002; V47 (5); September; P950-958
66. Wallace-E; Toolmark of CCI 'Clean-Fire' Primers, AFTE; 2003; V35 (2); P250
67. Thompson-E; Wyant-R Consecutively Made Cartridge Cases, AFTE; 2002; V34 (4);
P407-408
68. Flater-J-A; Manufacturing Marks on Winchester USA Brand 9mm Luger Primers, AFTE;
2002; V34 (3); P315
69. Wallace-E; Ammunition Update, AFTE; 2003; V35 (2); P242
70. Tulleners-F; Randich-E; Giusto-M ; Vickers Harness Values of Selected 40 S&W
Primers, AFTE; 2003; V35 (2); P204-208
71. Tew-J-D; Incorrect Manufacturer Supplied Test Fire Cartridge Cases, AFTE; 2003; V35
(2); P195-196
72. Lawrence-G-M; Glaser Safety Slug - A Primer for Identification, AFTE; 2003; V35 (1);
P79-80
73. Monturo-C; Plastic 9mm Ammunition, AFTE; 2002; V34 (2); P206-207
74. James-C-R; Idaho Territory Bullets from Speer, AFTE; 2002; V34 (2); P202-204
75. Haag-M; DaVia-K; Foster-J; Ross-C; The Reconstructive Aspects of Bullet Jacket and
Core Weights, AFTE; 2002; V34 (2); P161-164

61
76. Kass-G-G; What's New in Ammunition Report on SHOT Show 2001, AFTE; 2001; V33
(3); P282-283
77. Haag-L-C; Two Unique .22 Calibre Rimfire Bullets from Aguila: Performance and
Properties of Forensic Interest, AFTE; 2001; V33 (3); P276-279
78. Zahradka-A-A; Davis-A-L; Speer 357 SIG Cartridge Improvements, AFTE; 2001; V33
(4); P338-339
79. Wallace-E; Speciality Shotgun Ammunition from FIREQUEST, AFTE; 2001; V33 (2);
P162-164
80. Haag-L-C; The Exterior and Terminal Ballistics of 00 Buckshot, AFTE; 2003; V35 (1);
P25-34
81. Roberts-G-K; Lazzarini-D; Terminal Performance of the 5.7x28mm 31 Grain SS-190
FMJ Bullet Fired by the FN P-90 in 10% Ordnance Gelatin, AFTE; 2002; V34 (3); P302-
303
82. Roberts-G-K; Lazzarini-D; Pomerleau-P; Wounding Effects of Choke 12 Gauge 00
Buckshot Loads Intended for Law Enforcement Duty Using 10% Ordnance Gelatin,
AFTE; 2002; V34 (3); P287-288
83. Haag-L-C; The Exterior and Terminal Ballistics of 00 Buckshot, AFTE; 2002; V34 (2);
P148-157
84. Spinder-T; Allen-S; Speciality Shotgun Ammunition from All Purpose Ammunition,
AFTE; 2002; V34 (1); P53-54
85. Hagen-M; 5.45x39mm JHP Ammunition for the AK-47; WOUND-BALLISTICS-
REVIEW; 2001; V5 (1); P17-19
86. Jones-R; Testing of .357 Magnum Hollow Point Bullets in Water; WOUND-
BALLISTICS-REVIEW; 2001; V5 (1); P23-26
87. Haag-L-C; Zee Bullets - Another Entry into the Lead-Free Market, AFTE; 2001; V33
(2); P149-152
88. Attar-L; Desmarais-A; 9mm Flobert Bullet, AFTE; 2002; V34 (4); P396-398
89. Haag-L-C; Balloting Bullets: Exterior and Wound Ballistics of Balloted Bullets Physical
Characteristics of Balloted Bullets and Associated Cartridge Cases, AFTE; 2002; V34
(4); P375-378
90. Nedivi-L; Shoshani-E; The "Unfired" Cartridge: An Interesting Case Story, AFTE; 2001;
V33 (3); P258-259
91. Smith-G-A; Daniels-G; A Rifled .32 Auto Cartridge Identified to a .380 Auto Pistol,
AFTE; 2002; V34 (1); P50-51
92. Luchini-D; Di-Paolo-M; Morabito-G; Gabbrielli-M ;Case Report of a Homicide by a
Shotgun Loaded with Unusual Ammunition AM-J-FORENSIC-MED-PATHOL; 2003;
V24 (2); June; P198-201
93. Shoshani-E; Argaman-U; Giverts-P; Alteration of .38 Special Ammunition to .38 Smith
& Wesson Ammunition, AFTE; 2002; V34 (2); P183-185
94. Waghmare-N-P; Manna-A; Rao-M-S; Sen-P-K; Statistical Analysis of Impact Parameters
of Soft Nose Bullet Fired on Windowpane; FORENSIC-SCI-INT; 2003; V135 (3);
August; P181-187
95 De-Kinder-J; Lory-S; Van-Laere-W; Demuynck-E; The Deviation of Bullets Passing
Through Window Panes; FORENSIC-SCI-INT; 2002; V125 (1); January; P8-11
96. Theiling-D; Bullet Deflection Due to Angled Intervening Materials, AFTE; 2001; V33
(4); P304-312
97. Peshave-J-R; Singh-H; Determination of Chemical Life of Combustible Cartridge
Cases; J-ENERG-MATER; 2002; V20; P345-356
98. Koons-R-D; Grant-D-M; Compositional Variation in Bullet Lead Manufacture; J-
FORENSIC-SCI; 2002; V47 (5); September; P950-958

62
99. Randich-E; Duerfeldt-W; McLendon-W; Tobin-W; A Metallurgical Review of the
Interpretation of Bullet Lead Compositional Analysis; FORENSIC-SCI-INT; 2002; V127
(3); July; P174-191
100. Thompson-E; Wyant-R; Lead is Lead, AFTE; 2002; V34 (3); P314
101. Cakir-I; Cetin-G; Uner-H-B; Albek-E; Shot Range Estimation Based on Pellet
Distribution in Shots with a Pump-Action Shotgu;n FORENSIC-SCI-INT; 2003; V132;
P211-215
102. Salziger-B; Shooting Distance Determination by Shot Charge Distribution, AFTE; 2002;
V34 (2); P177-182
103. Haag-L-C; Average Pellet-to-Pellet Distance for Estimating Range-of-Fire in Cases
Involving Partial Pellet Patterns, AFTE; 2002; V34 (2); P139-143
104. De-Kinder-J; Ballistic Fingerprinting Databases; SCI-JUST; 2002; V42 (4); P197-203
105. Geradts-Z; Bijhold-J; Content Based Information Retrieval in Forensic Image Databases;
J-FORENSIC-SCI; 2002; V47 (2); P285-292
106. Giverts-P; Springer-E; IBIS and the 5.56 NATO Cartridge Case Fired from an M-16,
AFTE; 2003; V35 (2); P190-194
107. Argaman-U; Shoshani-E; Hocherman-G; Utilisation of the IBIS in Israel, AFTE; 2001;
V33 (3); P269-272
108. Francisco Javier Zanz, Nacional de Policia, Spain; IBIS in the Spanish Police 2000-2004,
International forensic technology symposium, Rome Italy 4-5 May 2004
109. Miguel Oscar Aguilar, Mexico; Integrating IBIS into the PGR laboratory workflow;
International forensic technology symposium, Rome Italy 4-5 May 2004
110. Geradts-Z-J; Bijhold-J; Hermsen-R; Murtagh-F; Image Matching Algorithms for Breech
Face Marks and Firing Pins in a Database of Spent Cartridge Cases of Firearms;
FORENSIC-SCI-INT; 2001; V119 (1); June; P97-106
111. Giverts-P; Argaman-U; Shoshani-E; Aharon-O; An Average Phase Scoring for Bullets, in
the IBIS Correlation Results, AFTE; 2002; V34 (2); P199-202
112. Rector-M; Effects of Ultrasonic Cleaning of Bullets on IBIS Correlation Scores: A
Preliminary Report, AFTE; 2002; V34 (2); P165-168
113. IBIS Users group; International forensic technology symposium, Rome Italy 4-5 May
2004
114. Bachrach-B; Development of a 3D-Based Automated Firearms Evidence Comparison
System; J-FORENSIC-SCI; 2002; V47 (6); November; P1253-1264
115. Banno-A; Possibility of Bullet Identification Using 3D Data; JAPANESE-JOURNAL-
OF-SCIENCE-AND-TECHNOLOGY-FOR-IDENTIFICATION; 2003; V8 (1); P81-97
116. Thali-M-J; Braun-M; Brueschweiler-W; Dirnhofer-R;'Morphological Imprint':
Determination of the Injury-Causing Weapon from the Wound Morphology Using
Forensic 3D/CAD-Supported Photogrammetry; FORENSIC-SCI-INT; 2003; V132;
P177-181
117. Subke-J; Haase-S; Wehner-H-D; Wehner-F; Computer Aided Shot Reconstructions by
Means of Individualised Animated Three-Dimensional Victim Models; FORENSIC-SCI-
INT; 2002; V125 (2-3); February; P245-249
118. Haag-L-C; Custom-Made Moulds for Ballistic Gelatin, AFTE; 2002; V34 (3); P321-322
119. Haag-L-C; The Forensic Uses of the Oehler Model 43 Personal Ballistics Laboratory
System, AFTE; 2002; V34 (1); P16-25
120. Hildebrandt-C-B; Forensic Buddy on Trial, AFTE; 2001; V33 (4); P359-360
121. Garbutt-R; Manual Spa Vacuum for Recovery of Bullets from a Horizontal Test Tank,
AFTE; 2001; V33 (4); P353-354
122. Mager-M; Aharon-O; Aperman-A; High Speed Photography System, AFTE; 2001; V33
(4); P339-341
123. Schutz-F; Serial Numbers Engraved by Laser: A Preliminary Study, AFTE; 2001; V33
(3); P280-281

63
124. Nichols-R-G; Firearm and Toolmark Identification Criteria: A Review of the Literature,
Part II; J-FORENSIC-SCI; 2003; V48 (2); March; P318-327
125. Tomasetti-K-A; Analysis of the Essential Aspects of Striated Tool Mark
Examinations and the Methods for Identification, AFTE; 2002; V34 (3); P289-301
126. Meyers-C; Some Basic Bullet Striae Considerations, AFTE; 2002; V34 (2); P158-160
127. Gaensslen-R-E; How Do I Become A Forensic Scientist? Educational Pathways to
Forensic Science Careers; ANALYTICAL AND BIOANALYTICAL CHEMISTRY;
2003; V376; August; P1151-1155
128. Miller-J ;An Examination of the Application of the Conservative Criteria for
Identification of Striated Toolmarks Using Bullets Fired from Ten Consecutively Rifled
Barrels, AFTE; 2001; V33 (2); P125-132
129. Dutton-G; Firearms Identification, Comparison Microscopes & the Spencer Lens Co. ,
AFTE; 2002; V34 (2); P186-198
130. Champod-C; Baldwin-D; Taroni-F; Buckleton-J-S; Firearm and Tool Marks
Identification: The Bayesian Approach; FSS-REPORT; 2003; NO.RR830; March; P1-19
131. Denio-D-JAn; Index of Firearm Exploded Views Found in the American Rifleman
Magazine, AFTE; 2003; V35 (1); P81-92
132. Moran-B; Reference Collections - The Lifeblood of the Firearm and Tool Mark
Examiner, AFTE; 2001; V33 (3); P219-226
133. Dutton-G; The Rotary Group Study Exchange Programme, AFTE; 2001; V33 (3); P260-
267
134. Lumb-P-D; Rutty-G-N; Forensic Web Watch; J-CLIN-FORENSIC-MED; 2001; V8;
P172-174
135. Shoshani-E; Silverwater-H; Argaman-U; A Design Defect of a Rhoner Pistol, AFTE;
2001; V33 (3); P253-255
136. Karger-B; Joosten-U A Case of "Boomerang" Bullet Ricochet; INT-J-LEG-MED; 2001;
V115; P70-71
137. Giusto-M; Merritt-M; Firearms Safety Bulletin, AFTE; 2002; V34 (4); P408
138. Mikko-D; Magnetic Resonance Imaging (MRI) Involving Firearms, AFTE; 2003; V35
(1); P23-24
139. Ismach-R-B; Reza-A; Ary-R; Sampson-T-R; Bartolomeos-K; Kellermann-A-L
;Unintended Shootings in a Large Metropolitan Area: An Incident-Based Analysis;
ANN-EMERG-MED; 2003; V41 (1); January; P10-17
140 Jacob-J; Charlton-R; Remember Laboratory Safety - Two Barrels in Two Days, AFTE;
2002; V34 (3); P310
141. Silverwater-H; Koffman-A; Zamir-A; Cross-Infection of Infectious Diseases as Applied
to Forensic Firearms Examinations and the Means to Prevent it, AFTE; 2001; V33 (3);
P227-232
142. Horn-A; Amberger-R; Firearm Safety Warning for Bryco Arms Model Jennings Nine,
AFTE; 2001; V33 (2); P145-147
143. Cook-D-S; James-R-S; An Antique Pistol Fatality: Consideration of the Legal and
Pathological Aspects: A Case Report; MED-SCI-LAW; 2002; V42 (4); P351-354
144. Tonner-B; Innovation for Imitations?: A Call for Change in the Law Relating to Imitation
Firearms; CRIM-LAW-REV; 2003; September; P618-62
145. Murdie-A ; Fifty Years of Offensive Weapons; JUSTICE-OF-THE-PEACE; 2003; V167
(17); April; P308-313
146. Grzybowski-R; Miller-J; Moran-B; Murdock-J; Nichols-R; Thompson-R;
Firearm/Toolmark Identification: Passing the Reliability Test Under Federal and State
Evidentiary Standards, AFTE; 2003; V35 (2); P209-241
147. Bunch-S-G; Murphy-D-P; A Comprehensive Validity Study for the Forensic
Examination of Cartridge Cases, AFTE; 2003; V35 (2); P201-203

64
148. Rosenberry-J-L; Firearms/Toolmark Examination and the Daubert Criteria, AFTE; 2003;
V35 (1); P38-48
149. Denio-D-J; The History of the AFTE Journal, the Peer Review Process, and Daubert
Issues, AFTE; 2002; V34 (2); P210-214
150. Moran-B; Photo Documentation of Toolmark Identifications - An Argument in Support,
AFTE; 2003; V35 (2); P174-189
151. Parkinson-G-A; Stringing a Crime Scene to Determine Trajectorie;s J-FORENSIC-
IDENT; 2003; V53 (4); P435-443
152. Thompson-E; Wyant-R; Asphalt Skip Shooting Reconstruction, AFTE; 2003; V35 (1);
P74-75
153. Waghmare-N-P; Badwal-S-S; Manna-A; Phenomena Attending Flight of .315"/8mm
Projectile Fired Through Glass Target, AFTE; 2002; V34 (4); P368-374
154. Parroni-E; Caringi-C; Ciallella-C; Suicide with Two Guns Represents a Special Type
of Combined Suicide ; AM-J-FORENSIC-MED-PATHOL; 2002; V23 (4); December;
P329-333
155. Baker-A-M; Keller-G; Garcia-D; A Novel Hunting Accident. Discharge of a Firearm by
a Hunting Dog; AM-J-FORENSIC-MED-PATHOL; 2001; V22 (3); September; P285-
287
156. Karger-B; Nusse-R; Bajanowski-T; Backspatter on the Firearm and Hand in
Experimental Close-Range Gunshots to the Head; AM-J-FORENSIC-MED-PATHOL;
2002; V23 (3); September; P211-213
157. Thali-M-J; Kneubuehl-B-P; Dirnhofer-R; Zollinger-U; The Dynamic Development of the
Muzzle Imprint by Contact Gunshot: High-Speed Documentation Utilising the "Skin-
Skull-Brain Model"; FORENSIC-SCI-INT; 2002; V127 (3); July; P168-173

Firearms –Chemistry

1. Romolo SR, Margot P. Identification of gunshot residue: a critical review. J Forensic Sci
2001; 119:195-211.
2. Zeichner A. Recent developments in methods of chemical analysis in investigations of
firearm-related events. Anal Bional Chem 2003;376:1178-1191.
3. Torre C, Mattutino G, Vasino V, Robino C. Brake linings: A source of Non-GSR
particles containing lead, barium and antimony. J Forensic Sci 2002;47(3):494-504.
4. ASTM Committee E-30 on Forensic Sciences. ASTM E 1588-95, (Reapproved 2001)
standard guide for gunshot residue analysis by scanning electron microscopy/energy-
dispersive spectroscopy. Annual Book of ASTM Standards July 2002;Vol. 14.02.
5. Coumbaros J, Kirkbride KP, Kobus H, Sarvas I. Distribution of lead and barium in
gunshot residue particles derived from 0.22 caliber rimfire ammunition. J Forensic Sci
2001;46(6):1352-1357.
6. Collins P, Coumbaros J, horsley g, Lynch b, Kirkbride KP, Skinner W, Klass G. Glass-
containing gunshot residue particles: anew type of highly characteristic particle? J
Foensic Sci. 2003;48(3):538-553.
7. Lebiedzik J, Johnson DL Handguns and ammunition indicators extracted from the GSR
analysis.) J Forensic Sci 2002;47(3):483-493.
8. Brozek-Mucha Z, Jankowicz A. Evaluation of the possibility of differentiation between
various types of ammunition by means of GSR examination with SEM/EDX method.
Forensic Sci Int 2001;123(1):39-47.
9. Brozek-Mucha Z, Zadora G. Grouping of ammunition types by means of frequencies of
occurrence of GSR. Forensic Sci Int 2003;135(2):97-104.
10. Brozek-Mucha Z, Zadora G, Dane F. A comparative study of gunshot residue originating
from 9 mm Luger ammunition from various producers. Science & Justice
2003;43(4):229-235.

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11. Mastruko V (2001) 8 th ENFSI-Firearms working group meeting, Brugge, Belgium
12. Kage S, Kudo K, Kaizoji A, Ryumoto J, Ikeda H, Ikeda N. A simple method for
detection of gunshot residue particles from hands, hair, face and clothing using scanning
electron microscopy/wavelength dispersive X-ray (SEM/WDX) J Forensic Sci
2001;46(4):830-834.
13. Coumbaros J, Kirkbride KP, Klass G, Skinner W. Characterisation of 0.22 calibre rimfire
gunshot residues by Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS): A
Preliminary study. Forensic Sci Int 2001; 119 (1):72-81.
14. Trombka JI, Schweittzer J, Selavka C, Dale M, Gahn N, Floyd S, Marie J, Hobson M,
Zeosky J, Martin K, McClannahan T, Solomon P, Gottschang E. Crime scene
investigations using portable, non-destructive space exploration technology. Forensic Sci
Int 2002;129(1):1-9.
15. Martini L, DeMaria A. Evaluation of Law enforcement Technologies Inc. ISID01
“Instant Shooter ID Kit” AFTE Journal 2002;34(4):404-406.
16. Steffen S, Niewhoner L. Improved methods for the collection of gunshot residues (GSR)
and for chemographic testing of lead-free Sintox ammunition. AFTE Journal
2003;35(2):152-156.
17. Fojtasek L, Vacinova J, Kolar P, Kotrly M. Distribution of GSR particles in the
surroundings of shooting pistol. Forensic Sci Int 2003;132(2);99-105.
18. Reis Elt, Souza Sarkis JE, Neto ON, Rodrigues C, Kakazu MH, Viebig S. A new method
for collection and identification of gunshot residues from the hands of shooters. J
Forensic Sci 2003:48(6):1269-1274.
19. Schutz F, Bonfanti MS, Desboeeufs S. Evaluation of parameters influencing GSR’s
retention on shooter’s hands. Zagadnien Nauk Sadawych 2001;47:380-386.
20. Niewhoner L, Wenz HW, Andrasko J, Beijer R, Gunaratnam L. ENFSI proficiency test
program on identification of GSR by SEM/EDX. J Forensic Sci 2003;48(4):786-793.
21. GSR2003, Report on the international proficiency test on identification of GSR by
SEM/EDX.
22. Wu Z, Tong Y, Yu J, Zhang X, Yang C, Pan C, Deng X, Wen Y, Xu Y. The utilization of
MS-MS method in detection of GSRs. J Forensic Sci 2001;46(3):495-501.
23. Zeichner A, Eldar B, Glattstein B, Koffman A, Tamiri T, Muller D. Vacuum collection of
gunpowder residues from clothing worn by shooting suspects, and their analysis by
GC/TEA, IMS and GC/MS. J Forensic Sci 2003;48(5):961-972.
24. Zeichner A, Eldar B. A novel method for extraction and analysis of gunpowder residues
on double-side adhesive coated stubs. Submitted for publication in J Forensic Sci.
25. Northrop DM Gunshot residue analysis by micellar electrokinetic capillary
electrophoresis: assessment for application to casework. Parts I and II. J Forensic Sci
2001 46(3): 549-572.
26. MacCrehan WA, Layman MJ, Secl JD. Hair combing to collect organic gunshot residues
(OGSR). Forensic Sci Int 2003;135:167-173.
27. Leifer A, Wax H, Almog J. Who held the gun?: Decipherement of suicide-homicide
cases using the PDT reagent. J Forensic Ident 2001;51(4): 346-360
28. Leifer A, Avissar Y, Berger S, Wax H, Donchin Y, Almog J Detection of firearm
imprints on the hands of suspects: effectiveness of PDT reaction. J Forensic Sci
2001;46(6):1442-1446.
29. Avissar YY, Sagiv AE, Mandler D, Almog J. Identification of firearms holders by the Fe-
PDT complex. Part I: quantitative determination of iron transfer to the hand and its
dependence on palmar moisture levels. Submitted for publication in J Forensic Sci.
30. Avissar YY, Mandler D, Almog J. Identification of firearms holders by the Fe-PDT
complex. Part II: chemical and time dependent factors. Submitted for publication in
Talanta.

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31. Zeichner A, Glattstein B. Recent developments in the methods of estimating shooting
distance. The Scientific World Journal 2002;2:573-585.
32. Carroll J. An evaluation of various Griess and modified Griess test protocols. AFTE
Journal 2001;33(1):29-36.
33. Shem RJ. A simplified Griess and sodium rhodizonate test. AFTE Journal 2001;33(1):37-
39.
34. Reardon MR, MacCrehan WA. Developing a quantitative extraction technique for
determining the organic additives in smokeless handgun powder. J Forensic Sci
2001;46(4):802-807.
35. Mac Crehan WA, Patierno ER, Duewer DL, Reardon MR Investigating the effect of
changing ammunition on the composition of organic additives in gunshot residue
(OGSR). J Forensic Sci 2001;46(1):57-62.
36. MacCrehan WA, Reardon MR, Duewer DL Associating gunpowder and residues from
commercial ammunition using compositional analysis. J Forensic Sci 2002;47(2):260-
266.
37. Koons RD, Grant DM. Compositional variation in bullet lead manufacture. J Forensic Sci
2002; 47(5):950-958.
38. Peters CA. The basis for compositional bullet lead comparisons. Forensic Science
Communications 2002; 4(3).
39. Stupian GW, Ives NA, Marquez N, Morgan BA The application of lead isotope analysis
to bullet individualization in two homicides. J Forensic Sci 2001; 46(6):1342-1351
40. Cheylan P, Dobney AM, Wiarda W, Beijer R, Peijl GJQ. Fundamental processes in GSR
formation as deduced from ICP-AES and SF-ICPMS experiments. AAFS meeting,
Atlanta, Georgia, USA 2002
41. Gulson BI, Eames JC, Davis JD. Evaluation of exhibits from a murder case using the lead
isotope method and scanning electron microscopy. J Forensic Sci 2002; 47(5):1015-
1021.
42. Zeichner A, Ehrlich S, Shoshani E, Halicz L. Application of lead isotope analysis by
MC-ICP/MS in shooting incident investigations. Submitted for publication in J Forensic
Sci.
43. Andrasko J, Stahling S. Time since discharge of pistols and revolvers. J Forensic Sci
2003;48(2):307-311.
44. Wilson JD, Tebow D, Moline KW. Time since discharge of shotgun shells. J Forensic Sci
2003;48(6):1298-1301.

Firearms –Wound ballistics

1. Haag-L-C, Balloting Bullets: Exterior and Wound Ballistics of Balloted Bullets Physical
Characteristics of Balloted Bullets and Associated Cartridge Cases, AFTE; 2002; V34
(4); P375-378 AN: 89352
2. Haag-L-C, The Exterior and Terminal Ballistics of 00 Buckshot, AFTE; 2003; V35 (1);
P25-34 AN: 90353
3. Fackler-M-L; Welch-N-E; Dahlstrom-D-B; Powley-K-D, Shot Cup Petal Distortion
Separates Contact from Two Foot Distant Shotgun Wounds, J-INT-WOUND-
BALLIST-ASSOC; V2 (3); P37-41 N: 90161
4. Koffman-A; Zeichner-A; Glattstein-B; Kahana-T , Firearms Report - Speaking Paper
1998-2001,AFTE; 2002; V34 (4); P362-367 AN: 89350
5. Dobosz T, Jaworski R, Kawecki J, Semiczek W, Trnka J.Katedry i Zakladu Medycyny
Sadowej AM we Wroclawiu., Enforcement of type M 20 cal. 4 mm cartridges ,Arch Med
Sadowej Kryminol. 2002 Jul-Sep 52(3): 155-62
PMID: 14669686

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6. Havel J, Energy-dispersive x-ray fluorescence spectrometry--a forensic chemistry method
for determination of shooting distance, Soud Lek. 2003 Oct;48(4):57-60 PMID:
14661530
7. Plattner T, Kneubuehl B, Thali M, Zollinger U., Gunshot residue patterns on skin in
angled contact and near contact gunshot wounds., Forensic Sci Int. 2003 Dec 17;138(1-
3):68-74.PMID: 14642721
8. Reis EL, Sarkis JE, Neto ON, Rodrigues C, Kakazu MH, Viebig S., A new method for
collection and identification of gunshot residues from the hands of shooters., J
Forensic.Sci. 2003 Nov;48(6):1269-74, PMID: 14640269
9. Puskas CM, Rumney DT, Bilateral fractures of the coronoid processes: differential
diagnosis of intra-oral gunshot trauma and scavenging using a sheep crania model., J
Forensic Sci. 2003 Nov;48(6):1219-25.
PMID: 14640263
10. Havel J. Energy dispersive x-ray fluorescence spectrometry--a forensic ecrochemical
method for determination of entry and exit of gunshot wounds, Soud Lek. 2003
Jul;48(3):42-4. PMID: 14631712
11. Corbett H, Paulsen EK, Smith RS, Carman CG., Paradoxical bullet embolus from the
vena cava: a case report. J Trauma. 2003 Nov;55(5):979-81.PMID: 14608178
12. Bhana BD, Kirk GM, Dada MA, Fatal firearm wounds: a clinicopathologic study.Am J
Forensic Med Pathol. 2003 Sep;24(3):273-6.PMID: 12960664
13. Kluger Y. Bomb explosions in acts of terrorism--detonation, wound ballistics, triage and
medical concerns. Isr Med Assoc J. 2003 Apr;5(4):235-40 PMID: 14509125
14. Prahlow JA, Allen SB, Spinder T, Poole RA, Pseudo-gunpowder stippling caused by
fragmentation of a plated bullet. Am J Forensic Med Pathol. 2003 Sep;24(3):243-7.
PMID: 12960660
15. Verhoff MA, Karger B ,Atypical gunshot entrance wound and extensive backspatter Int J
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.PMID: 12836037
16. Pabuscu Y, Bulakbasi N, Kocaoglu M, Ustunsoz B, Tayfun C.,A different approach to
missile induced head injuries ,Comput Med Imaging Graph. 2003 Sep-Oct;27(5):397-
409PMID: 12821033
17. Bartlett CS, Clinical update: gunshot wound ballistics Clin Orthop. 2003 Mar;(408):28-
57..PMID: 12616039
18. Thali MJ, Kneubuehl BP, Vock P, Allmen G, Dirnhofer R, High-speed documented
experimental gunshot to a skull-brain model and radiologic virtual autopsy. Am J
Forensic Med Pathol. 2002 Sep;23(3):223-8.PMID: 12198345
19. Thali MJ, Kneubuehl BP, Zollinger U, Dirnhofer R, The "skin-skull-brain model": a new
instrument for the study of gunshot effects. Forensic Sci Int. 2002 Feb 18;125(2-3):178-
89..PMID: 11909661
20. Rainio J, Lalu K, Ranta H, Penttila A., Morphology of experimental assault rifle skin
wounds, nt J Legal Med. 2003 Feb;117(1):19-26. Epub 2002 Oct 30
PMID: 12592591
21. Peleg K, Aharonson-Daniel L, Stein M, Michaelson M, Kluger Y, Simon D, Noji EK;
Israeli Trauma Group (ITG). Gunshot and explosion injuries: characteristics, outcomes,
and implications for care of terror-related injuries in Israel. Ann Surg. 2004
Mar;239(3):311-8.PMID: 15075646
22. Hiss J, Kahana T, Confusing exit gunshot wound--"two for the price of one". Int J Legal
Med. 2002 Feb;116(1):47-9. .PMID: 11924709
23. Grimm U, Zollinger U, Lodged bullet or bullet penetration? Re-entry of a projectile and
pseudo-shot, Arch Kriminol. 1996 Mar-Apr;197(3-4):89-96. .PMID: 8687277

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24. Karger B, Billeb E, Koops E, Brinkmann B., Autopsy features relevant for discrimination
between suicidal and homicidal gunshot injuries., Int J Legal Med. 2002 Oct;116(5):273-
8. Epub 2002 Aug 16 PMID: 12376836
25. Slobodan S, Slobodan N, Djordje A., Popliteal artery bullet embolism in a case of
homicide: a case report and review of the tangible literature., Forensic Sci Int. 2004 Jan
6;139(1):27-33.PMID: 14687770/
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69
Forensic Examination of Fibres

— A Review: 2001 to 2004 —

Adj. Prof. James Robertson

National General Manager, Forensic and Technical
Australian Federal Police, GPO Box 401
Canberra ACT 2601, Australia
E-mail: jim.robertson@afp.gov.au

Prof. Claude Roux

Director, Centre for Forensic Science
University of Technology, Sydney, PO Box 123
Broadway NSW 2007, Australia
E-mail: claude.roux@uts.edu.au

This report is dedicated to the memory of Mike Grieve

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INTRODUCTION:

This report covers advances in scientific methods applied to the forensic examination of fibres
reported since the 13th INTERPOL Forensic Science Symposium in October 2001. A literature
review was conducted covering articles published in the principal forensic science journals over
the period in question (up to May 2004). This was supplemented by an extensive search of
Internet sources, for articles related to fibre examination in the forensic arena. Major textile
magazines and some relevant books were also consulted to provide useful background. The final
report is a collation of information received from these various sources.

GENERAL:

Scientific working groups in Europe and North America have been active to coordinate training,
research efforts and develop protocols for forensic fibre examination, including laboratory
analysis and determination of the evidential value. The two major groups are the European
Fibres Group (EFG) of the European Network of Forensic Science Institutes (ENFSI) and the
Fiber subgroup of the Scientific Working Group for Materials Analysis (SWGMAT) led by the
FBI.

Wiggins (1) outlined the history of the European Fibres Group including its aims and
achievements since its formation in 1993. This paper emphasised the critical need for promotion
and exchange of information, standardisation, training and research and development. To
achieve these aims this group meets annually and publishes sought after proceedings within three
months of the meeting ((2) to (4)). The EFG also published in late 2001 the Manual of Best
Practice for the Forensic Examination of Fibres (5). This document significantly raised the
standard of forensic fibre examination on a world basis.

Since its inception, the EFG acknowledged that the main knowledge gap was on the subject of
the evidential value of fibres. The EFG became the prime driver for significant collaborative
research. In 2001 the group identified a R&D programme dealing with the following topics:
textile pattern recognition, colour in clothing, Raman spectroscopy and dyes used on blue denim
textiles.

Following the successful publication of its Forensic Fiber Examination Guidelines (6), the
SWGMAT Fiber subgroup focussed on the development of a training program. The latter
includes an extensive training manual (7) and is expected to make a significant contribution to
the forensic fibre community.

The status of textile fibre examination across USA and Europe was compared and discussed by
Wiggins (8). The standard of forensic fibre examination was found to be generally high and the
works of the EFG and SWGMAT were praised as major contributors for such quality. More fibre
casework was carried out in Europe than in the USA. Small differences were also highlighted in
the instrumentation and in the method of collection used. Contamination was found to be a major
issue. Careful consideration should also be given as to whether legitimate contact could have
occurred prior to an offence being committed.

In recent years, the emphasis on DNA technology has sometimes led actors of the Criminal
Justice System to believe that trace evidence such as fibres may be of little value. Grieve and
Wiggins discussed this challenge extensively and proposed suggestions for improving the use of
fibres as forensic evidence (9). This paper summarised offences where fibres may be the only
type of physical evidence. Deficiencies were highlighted and ways to correct them were

71
suggested. According to the authors, the efficiency of the examination should be improved and
the evidential value of the findings should be expressed in a clearer way. Areas where particular
progress could be made are: improved communication and exchange of information between the
investigator and the scientist, streamlining analysis by using the latest equipment, effective case
management, better use of existing data pertaining to fibre frequencies, accumulating new data
by using the resources of working groups and improving training procedure especially in the area
of evidence interpretation. Similar comments and general conclusions were made in separate
papers by Grieve (10) and Biermann and Grieve (11).

FIBRE RECOVERY:

Fibre recovery is a crucial step for any forensic fibre examination. Common methods include
manual recovery with tweezers, tape lifting, scraping and vacuuming. Wiggins (9) highlighted
differences between European and American practices: many American laboratories performed
all methods while European laboratories favour tape lifting and, where appropriate, manual
recovery.

Roux et al. (12) investigated fibre movement within and out the search room when performing a
garment examination. In addition to various findings and recommendations, this study
highlighted the increased risk of contamination when the scraping method is used because of an
increased number of loose fibres transferred onto the examiner’s clothing and fibres exiting the
search room. This paper concluded that it is unlikely that a completely clean search room can be
obtained. However, with proper precautions it is possible to minimise and monitor the
contaminant fibre population.

Recent times have seen the advent of 1:1 tape lifting, a fibre recovery technique whereby one
area of tape correlates to an equal area of the taped surface. In this way, information about the
density, position and distribution of each fibre type on an item or area is retained. Grieve (10)
pointed out that obvious advantages include assistance in reconstructing the events and possible
investigative leads. However, the large number of tapes to be used creates a significant logistical
issue. It has been suggested that a compromise may provide the best answer, whereby the body is
subdivided into small areas and a smaller number of tapes is used (about 34). A similar approach
was used by Causin et al. (13) in a case study reporting a double murder where fibre evidence
found on a suspect vehicle was the only useful trace to reconstruct the dynamics of the
transportation of two bodies. Coyle et al. (14) recently reported the first UK case where 1:1
taping had been successfully applied.

Automatic search methods have been identified as a way to reduce the manual workload and
hence assisting to achieve more efficiency in the examination (9). These systems have been
described in the literature published during the previous reporting period. Langdon et al. (15)
performed an evaluation of the Maxcan fibre finder version 3.3 on cotton fibres. Their results
showed that the system performed effectively in most situations, although it did have some
problems with some search combinations that a human operator would also find difficult in a
manual search. The ability of this system to perform large batch searches unattended and achieve
consistent results is very useful for casework with a large number of tapes or in research where
large quantities of data need to be gathered within a reasonable time.

Unfortunately, most systems have been plagued with both software and hardware problems
which have not yet been fully resolved, and most systems have not fully met the original
expectations. Overall, the initial high level of interest for automatic search systems has decreased
in recent years. This may change again in the future depending on the manufacturers’ response to

72
these criticisms. In this context, Kolar (16) reported a promising use of a hyphenated fibre
finder-microspectrometer based on the Lucia fibre finder and Spectral (CCD) systems. Such a
system could be the first step for an integrated fibre workstation consisting of a fibre finder, an
optical microscope and an image processing system.

ANALYTICAL METHODS:

Publications in this area generally report improvement of existing techniques or technology

transfer from other analytical disciplines and rarely describe totally new methods. The pool of
existing methods for the forensic examination of fibres are in general so efficient to identify and
compare fibres that only a few real advances really took place. One of them is Raman
spectroscopy, the interest being the potential to gather chemical information on fibre dyes in situ.

However, early works using Raman spectroscopy mainly focussed on the analysis of man-made
fibres (17). Jochem and Lehnert (18) analyzed pigmented polyacrylonitrile (PAN) and cellulose
viscose fibres. They noticed that for highly pigmented fibres, the signal of the polymer matrix is
totally hidden by the spectra of the main pigment present. These results suggest that the
identification of at least the main pigment component should be feasible by Raman. This was
confirmed by Thomas et al. (19) who analysed blue, black and grey cotton fibres dyed with
reactive dyes. In this study, Raman spectroscopy usually enabled the identification of the main
dye present.

Macdonald et al. (20) applied Raman spectroscopy to the identification of pigments on 250-year
old Chinese painted silk. Low laser power and short exposure have been shown to allow
unambiguous pigment identification in situ. Operating in confocal mode improved the spectral
quality, principally by reducing the amount of background fluorescence.

The growing interest for Raman spectroscopy in the fibre arena prompted the European Fibres
Group to create a Raman sub-group and to support the largest collaborative study undertaken on
the topic (21). Three dyed fibers: two red acrylics and one red wool were analysed by Raman
instruments from six different manufacturers as well as nine different laser wavelengths ranging
from blue (458 nm) to near infrared-NIR (1064 nm). This represents the largest comparison
study of Raman analytical parameters carried out on identical fibre samples. In this study, blue
(488 nm) and green lasers (532 nm) globally gave the best quality spectra. Luminescence
problems were often encountered with some of the excitation wavelengths and therefore the
authors recommended a flexible Raman instrument equipped with different lasers and a
microscope to measure forensic fibre samples. This study also showed that Raman spectroscopy
usually enables the identification of the main dye present in a coloured fibre however minor dye
compounds are much more difficult to detect. SERRS (Surface Enhanced Resonance Raman
Scattering) techniques gave an improvement of the dye’s spectral quality but no spectral
improvement was observed for the two red acrylic and red wool fibres tested.

The comparison of spectra (MSP or Raman) is traditionally performed visually. This is not
practical when dealing with a large number of spectra and could also be regarded as subjective.
For this reason there is a recent interest in using Chemometrics. The latter may be used to
simplify complex spectra to facilitate interpretation and sample matching. In particular, principle
components analysis (PCA) reduces the dimensionality of spectra by sequential linear
transformations of the spectra, where the first few transformations retain most of the variation of
the original signal. Calculation of the principal component scores allows organization of results
in lower dimensional space for quick interpretation of results. Linear discriminant analysis
(LDA) is a classical statistical approach for classifying samples of unknown classes, based on

73
training samples with known classes. Thomas et al. (22) analysed Raman spectra from one
hundred (100) random black and blue cotton samples with PCA and subsequent discriminant
analysis. This study showed the successful use of Raman spectroscopy, combined with
chemometrics, for the characterization of the major dye component present in each fibre sample.
This method of data analysis proved to be a rapid and reliable tool for the classification of a large
sample set.

Grieve et al. (23) made a significant contribution to the research effort in the area of the in-situ
analysis of fibre dyes, especially in relation to the determination of the evidential value of
common fibres such as black cotton. In this study 88 known black cotton dyes and 225 samples
of black cotton were analysed by UV-visible microspectrophotometry. Spectra originating from
sulphur dyes and from the great majority of reactive and direct dyes could be easily recognised,
while vat dyes presented a little more difficulty. The discriminating power of the technique
varied from 0.13 for sulphur dyes to 0.93 for reactive dyes. From 99 textiles dyes with reactive
dyes, the spectra could be divided into at least 40 varieties showing that these fibres have a high
degree of individuality. The authors found that spectral information below 400 nm (UV) is
important and even critical in the case of direct dyes.

The same authors also examined samples of orange and green cotton fibres by UV-visible
microspectrophotometry (24). In both colours, spectra from reactive and sulphur dyes were the
easiest to recognise but could not be classified with the same reliability as seen in black cotton
fibres. This study emphasised again the importance of spectral information in the UV range.

Suzuki et al. (25) analysed single wool and cotton fibres dyed by indigo and derivatives by
ultraviolet-visible microspectrophotometry in transmission in the 240-760 nm region. The
authors found that glycerine was the most suitable embedding solvent. Detailed observation of
maxima, minima and minute shoulder peaks enabled them to discriminate each single fibre from
each other non-destructively even though these fibres were dyed by structurally similar indigo
derivatives.

One promising new technology whose applications go well beyond the forensic examination of
fibres is Chemical Imaging. This technology combines molecular spectroscopy and digital
imaging. This combination provides information on morphology, composition, structure and
concentration from one analysis. Chemical Imaging provides both spatial and spectral
information detecting light intensity, as a function of wavelength as in spectroscopy and also as a
function of location, as in imaging to form a data set. Payne et al. (26) used Chemical Imaging
for colourmetric and fluorescence microscopic analysis (400-720 nm) of red and black cotton,
wool, acrylic and polyester fibres. The technique performed as well as, and even sometimes
better than some conventional microspectrophotometers. The results were especially promising
for fluorescence and reflectance analyses. More research is obviously needed, but in the future
this technique might potentially replace conventional microspectrophotometry.

Tuinman et al. (27) applied electrospray ionisation mass spectrometry (ESI-MS) and tandem
mass spectrometry (ESI-MS/MS) to analyse acidic dyes used to colour nylon-based fibres, as
well as extracts from dyed nylon fibres. The combination of these two techniques has been
shown to provide both qualitative and quantitative information about the dyes present on a sub-
millimetre single fibre. The combined sensitivity and selectivity ESI-MS/MS is of particular
interest. The latter can offer insights into the chemical structure of the compound that is not
available from chromatographic techniques alone.

74
Huang et al. (28) also used electrospray ionisation mass spectrometry to analyse dyes from a
number of chemical classes including acid, direct and disperse dyes. These authors combined
liquid chromatography separation (LC-MS) with an on-line UV-visible absorbance detection to
monitor elution of dyes in the presence of other non-dye components extracted from the coloured
textile fibres.
Cho et al. (29) showed that attenuated total reflection (ATR) is a convenient mode for single
fibre analysis by infrared microspectroscopy (FTIR). This study demonstrated that nylon,
acrylic, cotton, polyester and olefin fibres too thick for transmission could be analysed
successfully by ATR. Because ATR is a surface analysis technique, it can reveal spectral
information about the surface treatment chemicals (eg. spin finishes, anti-static finishes,
permanent press finishes). This method can provide useful additional comparative features in
some cases, for example when dealing with colourless fibres. Another finding of this study was
showing that ATR can be used with transmission spectra to identify the core and sheath portions
of a bicomponent fibre.

INTERPRETATION:

The interpretation of fibre evidence has long been recognised as the most challenging topic
related to the forensic examination of fibres. A great deal of modelling and empirical research
has occurred in the last 15 years. The last three years have not been different and a number of
studies have been reported during this period.

The question of commonality is often posed to the expert with regards to fibre evidence, with the
aim of suggesting that the acquired evidence is not significant. Knowledge of the frequency of
occurrence of fibre types in a given population and of the chance of a random non-discrimination
are therefore required in order to assess the evidential value of finding fibres that could not be
differentiated from a suspect source. This information becomes increasingly important when a
Bayesian model is applied to the interpretation of fibre evidence.

Cantrell et al. (30) investigated the fibre population on textile cinema seats in Sydney, Australia,
in winter. 3025 fibres were classified according to colour, generic class and fluorescence
properties (the latter for 100 grey–black cotton fibres only). The recovered fibres were mostly
natural fibres (84%) with cotton the most common generic type (70%). On the contrary, man
made fibres were relatively rare (15%) with rayon constituting the majority of these (51%). The
most common colour/generic class combinations were grey–black cotton (33%) and blue cotton
(30%) accounting for 63% of the total population. All other frequencies were below 5%, most
below 1% using only the two properties of colour and generic class. Fluorescence properties
were found to be very discriminating as far as grey–black cotton fibres were concerned. A
similar study was subsequently undertaken by Cresswell et al. (31) in Glasgow, Scotland.

Dignan and Murphy (32) examined fingernail clippings from 36 subjects for the presence of
fibres. They determined it was not unusual to find fibres under fingernails and that
colourless/white, blue and grey/black cotton fibres were the most common. No significant
differences were identified with respect to gender of the subjects and the dominant hand did not
seem to play a significant role in the number of fibres. Children had more fibres under their nails
than adults.

As part of their study into orange and green cotton fibres (24), Grieve et al. carried out a survey
of 112 seats within the German Federal Police Office (including 100 canteen seats and 12 break
room seats). They showed that the percentage of all orange and green cotton fibres in random
population is very low even before they are subdivided according to spectral class, the

75
percentages varying from 0.4% (orange cotton on the canteen seats) to 1.27% (green cotton on
the break room seats).

Palmer and Oliver (33) undertook a population study focussing on textile fibres found in human
hair of 26 volunteers. Over 12,000 fibres were recovered and the most common fibre colours
were black/grey (48.0%), blue (29.1%) and red (12.7%), the least common being green,
orange/brown and yellow which each accounted for less than 5% of the total. Natural fibres
(mainly cotton) were predominant (72.3%) and man-made fibres were considerably less
frequent. The most common generic classes and colour were black and blue cottons. Fibre loads
carried by long hair were significantly less than that carried by short hair.

Watt et al. (34) surveyed the coloured fibre population that may be expected to exist in both
front-loading and top-loading domestic washing machines during Spring, in Sydney, Australia.
12,178 fibres were classified according to length, colour and generic class. Cotton fibres were
most prevalent (69.4%), followed by man-made (24.2%). The most common colour/generic class
combinations were black/grey cotton (27%), blue cotton (20%) and red cotton (15.6%). Other
combinations generally represented under 2% of the total fibre population. Two-thirds (65.9%)
of the recovered fibres were under 2mm in length, the proportion of fibres decreasing with
increasing fibre length. Variations in machine type did not effect the distribution of fibres with
respect to fibre type, colour or length.

Wiggins et al. (35) undertook a target fibre study whereby 58 items of outer clothing originating
from English households were taped to search for the presence of three types of commonly
encountered fibres (blue wool, black and grey polyester) and one less common fibre type (blue
acrylic). The tapes were searched using a combination of automatic and manual searches. One
matching polyester fibre, four acrylic fibres and 11 wool fibres were found. One item had six
matching wool fibres and another had the polyester fibre and one acrylic fibre. The remaining
eight items were each recovered from individual items. The main results of this study are similar
to those of previous target fibre studies: finding a large number of fibres that match a control is
unlikely to happen by chance. It is also unusual to find fibres from two different sources, even
though they may be commonly occurring, on one item by chance. This study was subsequently
published in Science & Justice incorporating a review of previous target fibre studies (36).

Houck (37) cross-compared foreign fibres recovered from one item from each of 20 unrelated
crimes. Colourless and denim fibres were excluded from the study. In total, 2,083 fibres were
compared using a standard analytical procedure including light microscopy, fluorescence
microscopy and microspectrophotometry. This resulted in 2,168,403 comparisons. No two fibres
were found to exhibit the same microscopic characteristics and analytical properties and the
author concluded that it is rare to find two unrelated items to have foreign fibres that are
indistinguishable. These results corroborate other population or target fibre studies conducted in
other parts of the world.

A study by Grieve and Biermann (38) went a step further. 256 samples of blue polyester fibres
obtained from case work controls and personal belongings were examined and compared using
microscopy and microspectrophotometry (310-750 nm). The 256 samples of blue polyester,
giving a total 32,640 possible comparisons, show that even within a very narrow segment of the
whole general fibre population, many examples of a specific colour/type of manmade fibre taken
from random sources can be compared and the chance of any two being the same is very low.
These studies should help to show the specificity and value of transferred fibres in providing
forensic evidence.

76
Studies into the transfer and persistence of fibres are equally important to assist in assessing the
evidential value of fibre evidence. In this category, Merciani et al. (39) studied the cross transfer
of fibers and especially the dependencies that could exist between the number of fibers
transferred in one direction and the number of fibers transferred in the other direction. Simulated
contacts between a car seat and three different woolen pullovers were carried out. The fibers
from the pullovers recovered on the car seat and the fibers from the seat recovered on the
pullovers were searched and counted. For two combinations seat/pullover, the correlation
between the numbers of fibers recovered on both side were strong, and for the third combination
this correlation was weaker. Moreover the number of transferred fibers from the seat was clearly
different for each of the pullovers. This confirms the importance of the recipient structure on the
number of transferred fibers. The authors also presented these results as examples within a
Bayesian framework.

Marshall et al. (40) undertook transfer and persistence studies involving carpet fibres (tufted pile
construction and short pile) and shoes. The results showed that most of the fibres were
transferred from the carpet with a tufted pile. In general the fibres were transferred to the sole of
the shoe with a significant proportion also found on the edges of the sole and on the fabric upper
of the training shoe. Only a few fibres, on average 3 fibres, were transferred from the short pile
to the shoes. It was also found that the fibres were lost rapidly from the heel and toe with a
slower loss observed from the fabric uppers. The initial loss of fibres from the shoes was rapid
with greater than 50% of the fibres lost after 30 seconds and 90% after 5 minutes. All of the
fibres were lost after 30 minutes of walking and running on different surfaces. These results
correspond to those obtained by similar previous studies. It is unlikely that fibres would be
recovered on shoes after contact with a carpet unless the suspect is arrested within a short time
after the incident, at or close to the scene.

Akulova et al. (41) studied the persistence of wool and acrylic fibres transferred on 23 recipient
garments in normal wear situations. The main result confirmed previous studies: most of the
fibres are lost quickly in an exponential manner (>75% after 8 hrs; 5-10% after 16 hrs). Fibres
were lost at a higher rate when public transport was used. The persistence of fibres depended
more on the surface structure and texture of the recipient garment and the location of donor
fibres rather than on the type of fibre. These results reinforce the importance of collecting
clothing from suspects as rapidly as possible following the event.

Watt et al (42) investigated the influence of several factors on the redistribution of extraneous
fibres on garments during machine washing. The persistence of target fibres was low (generally
<10%), but never zero. Between 50% and 100% of recovered fibres were redistributed away
from the primary contact area. A secondary transfer of target fibres always occurred to at least
one accompanying garment, 90% of experiments resulting in fibres transferred to the inside
surface of the accompanying garment. This implies that whilst valuable fibre evidence may be
recovered from garments after machine washing, the location of recovered fibres should not be
relied upon to corroborate alleged scenarios when it is known or suspected that the garment
under investigation has been laundered.

Causin et al. (13) reported a case study where fibres were the only type of evidence found on a
suspect vehicle in a double-murder case. The 1:1 taping concept was used to reconstruct the
spatial distribution of the traces and to further strengthen the support for one of the hypotheses.
In particular, this approach enabled a map to be drawn of the frequency of the different fibres
involved and to establish its compatibility with the wrapping used to transport the corpses. A
Bayesian approach was also used to interpret the findings and a Likelihood Ratio (LR) was

77
calculated, in order to quantify the support given by forensic evidence to the explanations
proposed. The authors also derived a LR equation that can be applied to similar cases.

TEXTILE / FIBRE DAMAGE:

A number of authors researched into the effect of various environmental conditions on textiles
and fibres. For example, Roux et al. (43) and Thomas et al. (44) investigated the degradation of
textiles and fibres due to natural environmental damage (mainly sunlight, water and burial in
soil). The former study focussed on changes observed using traditional equipment (brightfield
and fluorescence microscopy, microspectrophotometry, FTIR microspectroscopy), while the
latter demonstrated the use of Raman spectroscopy for the analysis of fibres that have undergone
environmental degradation.

Was-Gubala and Krauss (45) investigated the action of fire and high temperature on the most
popular colours and types of textiles and single fibres in a series of controlled experiments.
Changes in the chemical fibre structure were recorded by FTIR microspectroscopy and their
colour alterations using UV-visible microspectrophotometry. Differences were found between
characteristic changes in textile structure and colour after their exposure to different degrading
factors such as: open fire, a hot plate and vapour cloud explosion action. Valuable information
was also gathered about the potential identification of degraded textiles and fibres.

The same authors (46) also researched into the very specific damage to single textile fibres
caused by vapour cloud explosions using a selection of 41 garments differing in colour, fibre
composition and textile construction. Fibres subjected to a vapour cloud explosion became wider
at the end, often taking the form of a ball, bulb or shovel, while the morphological structure of
the remaining part of the fibre remained almost unchanged. Because in such situations the heat
wave goes through the textile very quickly, many fibres of the yarns remained unaffected. This
research may be helpful in providing a link between suspects and the scene of an explosion.

Almer reported a two-part study about textile damage prompted by actual cases. In the first study
(47), experiments were undertaken to determine if distortion of an elastic waistband of
underwear could occur through natural wear or through a sudden pulling force. This was crucial
in a sexual assault case where consent was the issue. New and worn women’s cotton underwear
with elastic waistbands were examined and tested. The buckling effect could not be reproduced
when forceful pulling was applied in the waistband seam area of undamaged underwear. On the
other hand, this type of damage was observed in worn underwear, even those that otherwise
appeared relatively new. The author concluded that the elastomer fibres work their way out of
the waistband side seam during normal wear, and that this can occur even before there are other
obvious signs of wear.

The second study (47) investigated the effect of cigarette burns on textiles after an alleged victim
of sexual assault (deceased) had been found away from the location of a fire scene with burn
holes on her underwear. Fabrics of different compositions, textures and thicknesses were tested
up to 20 seconds with the burning end of a cigarette, both while the fabrics were held up and
while resting on a corduroy-covered counter surface. When the fabrics were held up, the
cigarette burnt through the fabric at a rate varying from less that a second to 17 seconds. When
the fabrics rested against a surface, the results varied from less than a second to burn through, to
just mild charing. The author concluded that the composition, texture thickness and position of a
fabric may influence the burning effect of a cigarette upon it, and that testing may be warranted
in casework.

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TEXTILE TECHNOLOGY:

Background knowledge in textile technology is important for the forensic fibre examiner as such
information is needed if one wishes to keep abreast of recent technological developments (eg.
UV absorbers, new finishing agents) and hence optimise the forensic analytical work. It is also
often crucial for the assessment of the evidential value through information about production
figures, fashion changes, sudden arrival of new material, dye variability, etc.

For example, Nehse (49) presented valuable background information about textile colour and
colouring and their significance in forensic fibre examination. This study highlighted the large
number of factors influencing the final colour and shades including wear and tear. The
significance of this variability becomes obvious when considering the empirical studies
presented above.

Useful resources in this category include:

• Textile Technology Catalogue (50).

• International Textile Bulletin (51).
• European’s Fibres Group’s website and links (52) to (67).
• Three recent books on textile technology (53) to (70).

MISCELLANEOUS:

With the increasing use of modern technology for surveillance such as Closed Circuit Television
(CCTV) the question commonly arise as to whether captured images or video footages could be
linked to a particular piece of clothing. Morley (71) studied the evidential value of comparison of
clothing taken from a suspect(s) to clothing worn by the offender(s) on CCTV images. The
author concluded that the value of the evidence depends on two factors: (1) the degree of
correspondence between the images and the actual clothing and (2) an assessment of the degree
of commonness of those items. Despite the fact that a particular item of clothing can rarely
uniquely be identified from video images, there is value in carrying out this type of examination.
Valuable intelligence information and corroborative evidence can be obtained. Nehse and
Wendt (72)further presented a theoretical examination aiming at answering the question: how
individual are textiles? Design, colour, construction / textile patterning, individual fibres and
characteristics such as labels, repairs, defects, buttons, folds and creases, accessories, etc. are all
presented as valuable identifying features.

A number of articles were published about knots and ropes and may have some forensic
significance. Examples include references (73) to (78).

SUMMARY:

Significant progress has been made in the last three years in placing the forensic examination of
fibres on a sound basis. The work of peak bodies such as the ENFSI European Fibres Group
(EFG) and the Fiber subgroup of SWGMAT has been central and has resulted in a manual of
best practice and a comprehensive training manual.

The role of the late Mike Grieve in advancing the cause of forensic fibre examination cannot be
over-stated. Along with Ken Wiggins of the FSS, Mike provided exceptional leadership to the
EFG and was the ‘glue’ that brought together the EFG and SWGMAT to collaborate for the key
projects mentioned above. In this review the final product of Mike’s research collaborations are

79
detailed. He was particularly interested in the interpretation of fibres as evidence and promoted
the need for more work in this area of research from different parts of the world. Mike’s
influence will be felt for many years to come and, for those of us who had the privilege to know
him, and to work with him, we owe it to him to develop the next generation of fibre examiners.

Mike would have been pleased to see progress in the research reviewed in this paper, on areas as
diverse as fibre recovery, interpretation, textile and fibre damage, textile technology and
analytical methods.

Fibre examination is a mature field of forensic endeavour but there remains plenty of scope for
further study which we look forward to reviewing in 2007.

REFERENCES:

(1) Wiggins KG. The European Fibres Group (EFG) 1993-2002: Understanding and
Improving the Evidential Value of Fibres. Analytical and Bioanlytical Chemistry 2003
376, 1172-1177.
(2) Proceedings of the 9th European Fibres Group meeting, Vantaa, Finland, 2001.
(3) Proceedings of the 10th European Fibres Group meeting, Rosny-sous-bois, France, 2002.
(4) Proceedings of the 11th European Fibres Group meeting, Istanbul, Turkey, 2003.
(5) European Fibres Group. Manual of Best Practice for the Forensic Examination of Fibres.
2001.
(6) Scientific Working Group for Materials Analysis (SWGMAT). Forensic Fiber
Examination Guidelines. Forensic Science Communications 1999: V1, N1, online at
www.fbi.gov.
(7) Scientific Working Group for Materials Analysis (SWGMAT). A Forensic Fiber
Examiner Training Program. January 2004 Draft.
(8) Wiggins KG. Forensic Textile Fiber Examination Across the USA and Europe. Journal of
Forensic Sciences 2001, 46, 1303-1308.
(9) Grieve MC, Wiggins KG. Fibers Under Fire: Suggestions for Improving Their Use to
provide Forensic Evidence. Journal of Forensic Sciences 2001, 46, 835-843.
(10) Grieve MC. The Changing Face of Fibre Examination in Forensic Science. Z.
(11) Biermann T, Grieve MC. Die Zukunft der forensische faseranalyse. Kriminalistik 2001,
5, 337-340.
(12) Roux C, Huttunen J, Rampling K, Robertson J. Factors Affecting the Potential for Fibre
Contamination in Purpose Designed Forensic Search Rooms, Science and Justice 2001,
41(3), 135-144.
(13) Causin V, Schiavone S, Marigo A, Carresi P. Bayesian Framework for the Evaluation of
Fiber Evidence. Forensic Science International 2004,141, 159–170.
(14) Coyle T, Smith K, Mayo S, Chan A, Hunt N. Fibre Mapping – A Case Study. Science
and Justice 2004. 44(3), 179-186.
(15) Langdon S. Maynard P. Robertson J. Roux C. An Evaluation of the Maxcan Fibre Finder
Version 3.3, Forensic Science International 2003, 135, 137-145.

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(16) Kolar P. Lucia Fibre Finder with Spectrophotometer – Is it Reasonable? Forensic Science
International 2003. 136(1), 124.
(17) Miller JV, Bartick EG. Forensic analysis of single fibers by Raman spectroscopy.
Applied Spectroscopy 2001, 55(12), 1729-1732.
(18) Jochem G, Lehnert RJ. On the Potential of Raman Microspectroscopy for the Forensic
Analysis of Coloured Textile Fibres. Science & Justice 2002, 42(4), 215-221.
(19) Thomas J, Buzzini P, Massonnet G, Roux C, Reedy B. A further look at Raman
spectroscopy for the forensic examination of fibres. Forensic Science International 2003.
136(1), 125.
(20) Macdonald AM, Wyeth P, Rogerson C. Raman Spectroscopy Interrogating Historic
Painted Textiles. Asia/Pacific Microscopy and Analysis 2003, 35, 9-11.
(21) Massonnet G, Buzzini P, Jochem G, Stauber M ; Coyle T; Roux C, Thomas J, Leijenhorst
H, Van Zanten Z, Wiggins K, Russell C, Chabli S, Rosengarten A. Evaluation of Raman
Spectroscopy for the Analysis of Coloured Fibres: A Collaborative Study. Journal of
Forensic Sciences. Submitted in 2004.
(22) Thomas J, Doble P, Roux C, Robertson J. Chemometrics and Raman Spectral Data from
Dyed Cotton Fibres. Proceedings of the 17th International Symposium on the Forensic
Sciences (Australian & New Zealand Forensic Science Society Symposium), Wellington,
2004.
(23) Grieve MC, Biermann TW, Davignon M. The Evidential Value of Black Cotton Fibres.
Science & Justice 2001, 41, 245-260.
(24) Grieve MC, Biermann TW, Davignon M. The Occurrence and Individuality of Orange
and Green Cotton Fibres. Science & Justice 2003, 43(1), 5-22.
(25) Suzuki S, Suzuki Y, Ohta H, Sugita R, Marumo Y. Microspectrophotometric
Discrimination of Single Fibres Dyed by Indigo and Its Derivatives Using Ultraviolet-
Visible Transmittance Spectra. Science & Justice 2001, 41, 107-111.
(26) Payne G, Reedy B, Lennard C, Exline D, Roux C. Evaluation of the CI Trace for Fibre
Analysis. Proceedings of the 17th International Symposium on the Forensic Sciences
(Australian & New Zealand Forensic Science Society Symposium), Wellington, 2004.

(27) Tuinman AA, Lewis LA, Lewis SA Sr. Trace-Fiber Color Discrimination by Electrospray
Ionization Mass Spectrometry: A Tool for the Analysis of Dyes Extracted from
Submillimeter Nylon Fibers. Analytical Chemistry 2003, 75, 2753-2760.
(28) Huang M, Yinon J, Sigman ME. Forensic Identification of Dyes Extracted from Textile
Fibers by Liquid Chromatography Mass Spectrometry (LC-MS). Journal of Forensic
Sciences 2004, 49(2), 238-249.
(29) Cho L, Reffner JA, Gatewood BM, Wetzel DL. Single Fiber Analysis by Internal
Reflection Infrared Microspectroscopy. Journal of Forensic Sciences 2001, 46(6), 1309-
1314.
(30) Cantrell S, Roux C, Maynard P, Robertson J. A Textile Fibre Survey as an Aid to the
Interpretation of Fibre Evidence in the Sydney Region. Forensic Science International
2001, 123, 48-53.

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(31) Cresswell SL, Cunningham D, Nic Daeid N. Textile Survey of Cinema Seats in Glasgow.
Forensic Science International 2003. 136(1), 117.
(32) Dignan SJ, Murphy KJ. Fibre Evidence from Fingernail Clippings. Canadian Society of
Forensic Science Journal 2002, 35(1), 17-21.
(33) Palmer R, Oliver S. The Population of Coloured Fibres in Human Head Hair. Science &
Justice 2004, 44(2), 83-88.
(34) Watt R, Roux C, Robertson J. The Population of Coloured Textile Fibres in Domestic
Washing Machines. Proceedings of the 17th International Symposium on the Forensic
Sciences (Australian & New Zealand Forensic Science Society Symposium), Wellington,
2004.
(35) Wiggins K, Drummond P, Hicks-Champod T. A Study in Relation to the Random
Distribution of Four Fibre Types on Clothing. Forensic Science International 2003.
136(1), 121.
(36) Wiggins K, Drummond P, Hicks-Champod T. A Study in Relation to the Random
Distribution of Four Fibre Types on Clothing (Incorporating a Review of Previous Target
Fibre Studies). Science & Justice 2004, 44(3), 141-148.
(37) Houck MM. Inter-Comparison of Unrelated Fiber Evidence. Forensic Science
International 2003, 135, 146-149.
(38) Grieve MC, Biermann TW. The Individuality of Blue Polyester Fibers Used to Provide
Forensic Evidence. Forensic Science International 2003. 136(1), 121-122.
(39) Merciani P, Monard Sermier F, Buzzini P, Massonnet G, Taroni F. A Study of the Cross
Transfer of Fibers. Forensic Science International 2003. 136(1), 123.
(40) Marshall L, Griffin RME, Robinson K Recovery of Transferred Carpet Fibres from
Shoes, Their Persistence on the Outer Surfaces and the Value of Fibres Recovered from
the Inner Surfaces of the Shoes. Forensic Science International 2003. 136(1), 123-124.
(41) Akulova V, Vasiliauskiene D, Talaliene. Further Insights into the Persistence of
Transferred Fibres on Outdoor Clothes. Science & Justice 2002, 42(3), 165-171.
(42) Watt R, Roux C, Robertson J. The Influence of Front-Loading and Top-Loading Washing
Machines on the Persistence, Redistribution and Secondary Transfer of Textile Fibres
during Laundering. Proceedings of the 17th International Symposium on the Forensic
Sciences (Australian & New Zealand Forensic Science Society Symposium), Wellington,
2004.
(43) Roux C, Favaloro K, Doble P, Robertson J, Lennard C. Implications of Environmental
Impact for the Forensic Examination of Textile Fabrics and Fibres. Proceedings of the
16th Meeting of the International Association of Forensic Sciences, 38, Montpellier,
2002.
(44) Thomas J, Roux C, Reedy B. Raman Spectroscopy of Environmentally Degraded Fibre
Samples. Forensic Science International 2003. 136(1), 118-119.
(45) Was-Gubala J, Krauss W. The Degradation of Coloured Textiles by the Action of Fire
and High Temperature. Forensic Science International 2003. 136(1), 122.
(46) Was-Gubala J, Krauss W. Damage Caused to Fibres by Vapour Cloud Explosions.
Forensic Science International 2004. 141, 77-83.

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(47) Almer J. Textile Damage I – A Case of Distorted Waistband, Natural Wear or Sudden
Force? Abstracts from the 48th Annual Meeting of the Canadian Society of Forensic
Science, Toronto, 2001.
(48) Almer J. Textile Damage II – Cigarette Burns. Abstracts from the 48th Annual Meeting of
the Canadian Society of Forensic Science, Toronto, 2001.
(49) Nehse K. Coloured Textiles – What Makes the Difference? Differences in Colour and
Shade Through Various Influences During Production and Wear. Forensic Science
International 2003. 136(1), 122.
(50) Textile Technology Catalogue, Woodhead Publishing Ltd., Cambridge, England, yearly
catalogue.
(51) International Textile Bulletin, International Textile Service, ITS Publishing,
Schlieren/Zürich, monthly journal.
(52) http://www.enfsi.org/cms.php?cp=efg
(53) http://www.eurotexx.com/
(54) http://www.fashion-links.de/
(55) http://www.fashionseek.net/
(56) http://www.ita.rwth-aachen.de/
(57) http://www.techexchange.com/
(58) http://www.texdata.com/
(59) http://www.texi.org/
(60) http://www.textile.fr/
(61) http://www.textileweb.com/
(62) http://www.textileworld.it/
(63) http://www.textilexpert.com/
(64) http://www.textilserver.de/
(65) http://www.texweb.de/
(66) http://www.ivc-ev.de/HTDOCS/index.html
(67) http://www.trevira.de/
(68) Fung w. Coated and Laminated Textiles, Wool Science and Technology. Woodhead
Publishing Ltd., Cambridge, England, 2001.
(69) Tao X. Smart Fibres, Fabrics and Clothing. Wool Science and Technology. Woodhead
Publishing Ltd., Cambridge, England, 2001.
(70) Simpson WS, Cramshaw GH. Wool Science and Technology. Woodhead Publishing Ltd.,
Cambridge, England, 2002.
(71) Morley J. Comparison of Clothing to Video Images. Forensic Science International 2003.
136(1), 123.
(72) Nehse K, Wendt C. Wie individuell sind Textilien. Kriminalistik 2002. 6/02, 391-395.

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(73) Tanislav E, Tanislav Junior E. Forensic Interpretation of Knots and Ties Used to Restrain
Hands and Legs of the Victim. Z. Zagadnien Nauk Sadowych (Problems of Forensic
Sciences) 2001. 47, 67-70.
(74) Hopkins R. Bowstrings – Part I. Some History and Crossbow Strings. Knotting Matters
2002. 76, 38-43.
(75) Fidspike J. Webbing Knots – Part 1. Knotting Matters 2003. 78, 36-39.
(76) Fidspike J. Webbing Knots – Part 2. Knotting Matters 2003. 79, 37-41.
(77) Pawson D. Some Notes on the Rogue’s Yard. Knotting Matters 2003. 79, 16-20.
(78) Matesanz Arribas AJ, Atoche Garcia C, Two Singular Cases. Forensic Science
International 2003. 136(1), 120-121.

84
 Paint & Glass

— A Review: 2001 to 2004 —

Dr. Stefan Becker

Wolfgang Langer
Christine Wohlwend

Bundeskriminalamt
Forensic Science Institute
Thaerstr. 11
65193 Wiesbaden, Germany
Phone: +49 611 55-1 27 37 or 1 37 53
Fax: +49 611 55-1 38 75

E-mail: Stefan.Becker@bka.bund.de
Wolfgang.Langer@bka.bund.de
Kt13@bka.bund.de

85
Acronyms
AFM Atomic force microscope
ASTM American Society for Testing and Materials
ATR Attenuated total reflectance technology
BKA Bundeskriminalamt, Germany
CCD Charged Coupled Device
CL Cathodoluminescence
CM Confocal microscope
CRM Certified reference materials
DTR-MS Direct temperature resolved mass spectrometry
EDXRF Energy dispersive X-ray fluorescence
EDS Energy dispersive X-ray spectroscopy
EMA Electron microprobe analysis
ENFSI European Network of Forensic Science Institutes
ESEM Environmental Scanning Electron Microscope
EUCAP European Collection of Automotive Paint Collection
FTIR Fourier transform infrared spectroscopy
GC Gas chromatography
GC-MS Gas chromatography - mass spectrometry
GD-OES Glow discharge - optical emission spectroscopy
GFAAS Graphite furnace atomic absorption spectroscopy
GRIM Glass Refractive Index Measurement
GSR Gunshot residue
LIBDS Laser induced break down spectroscopy
ICP-AES Inductively coupled plasma-atomic emission spectroscopy, also ICP-OES
ICP-MS Inductively coupled plasma-mass spectrometry
ICP-OES Inductively coupled plasma-optical emission spectroscopy, also ICP-AES
ID Isotope dilution
IR Infrared
IRCGN Institut De Recherché Criminelle De La Gendarmerie Nationale, France
LA-ICP-MS Laser ablation-inductively coupled plasma-mass spectrometry
MSP Microspectrophotometry
NAA Neutron activation analysis
NICC National Instituut voor Criminalistiek en Criminologie, Belgium
NIST National Institute of Standards and Technology
OM Optical microscopy
PCA Principal component analysis
PIXE Particle induced X-ray emission
PPG Pittsburgh Plate Glass Industries
Py-GC-MS Pyrolysis gas chromatography - mass spectrometry
RBS Rutherford backscattering spectrometry
RI Refractive index
SEC Size exclusion chromatography
SEM Scanning electron microscope
SIMS Static secondary ion mass spectrometry
SKL Statens Kriminaltekniska Laboratorium, National Lab. of Forensic Science, Sweden
SR-XRD Synchrotron radiation X-ray diffraction
SWGMAT Scientific Working Group for Material Analysis
TEM Transmission electron microscopy
THM-GC-MS Thermally assisted hydrolysis and methylation – GC-MS
TLC Thin layer chromatography
TOF-SIMS Time-of-flight secondary ion mass spectrometry
UV Ultraviolet
UV-Vis Ultraviolet-visible
Vis Visible light
XPS Photoelectron spectroscopy
XRF X-ray fluorescence
XRD X-ray diffraction

86
FORWORD:

As once before, the Bundeskriminalamt (BKA) has been chosen to act as co-ordinating
laboratory for the sections paint and glass. This report covers significant advances in scientific
methods applied to the forensic examination of paint and glass reported since the 13th Interpol
Forensic Science Symposium in October 2001.

Colleagues from all around the world were contacted and asked for new trends in the field of
paint and glass examination. All contributions from national and international forensic science
symposia and meetings as well as internal research projects whether published or unpublished,
was of interest.

As a by-product it was hoped, that by this means the international co-operation and discussion
could be intensified, however, unfortunately, we received only 4 responses out of more than 50
callings.

Various resources were checked and relevant findings were imported into our literature database.
After the three years period, the most frequently cited periodicals in our collection are: Farbe &
Lack, Journal of Analytical Chemistry, Journal of Analytical Atomic Spectrometry, Paint &
Coatings Industry, JOT-Journal für Oberflächentechnik, Kunststoffe, Progress in Organic
Coatings, Journal of Forensic Sciences, Nachrichten aus der Chemie, Spectroscopy Europe, GIT-
Labor-Fachzeitschrift, Fresenius Journal of Analytical Chemistry, Analytical and Bioanalytical
Chemistry, Science & Justice, Problems of Forensic Sciences, LABO, Forensic Science
International, The Analyst, Journal of Raman Spectroscopy, Glass Science Technology and
Glass & Ceramics.

More than a thousand literature entries in our paint and glass database were made during the
period from January 2001 to March 2004. To squeeze this huge quantum of information into a
brief review is an extraordinarily difficult task and one cannot avoid to admit a small facet of
subjectivism in this choice. The aim of this selective review is to highlight the most interesting
contributions.

This review is divided into four parts, the first two dedicated to paint and glass subjects
respectively, the third part to interpreting evidence and quality assurance topics and finally the
fourth part to paint and glass subjects on the World Wide Web.

PART I: PAINT

Since the last Interpol Forensic Science Symposium in 2001, a number of advances have been
made in the forensic examination of paint. In the last review, one focus was set on the
identification of art forgeries and examination of materials with historical interest as well as new
paint raw materials. Due to the mass of information provided, we are constrained to confine our
review in this fields. A large number of forensic related field are nevertheless extensively
discussed.

Paint Formulation & Technology

Raw materials

Additives, binders, extenders and pigments are subjected to the continuous market change. Some
interesting raw materials are presented in relevant trade journals dedicated to manufacturers of
diverse paint products, such as the Paint & Coatings Industry or the European Coatings Journal.

87
Recommendable is the 2003 additives guide presented by the Paint & Coatings Industry in
glossary form presenting from A-Z the various additives in use in the paint and coatings industry
(1). In an article by Hare and Beck, the principal extender types (whiting, talc, chlorite, silica,
china clay (kaolin), minex, mica, wollastonite and barytes) are summarised in a table and their
typical properties and utilities are described (2). Recent pigment developments, namely the use
of coloured alumina flakes, mica based pigments and in general the chemistry and physics of
special effect pigments and colorants are frequently encountered in the literature. A summary of
effect pigments is presented by Becidyan (3). Especially daylight fluorescent pigments, UV-
fluorescent pigments, optical brightening agents, IR fluorescent (Anti-Stokes) pigments,
phosphorescent pigments, optically variable pigments, photochromic colorants and
thermochromic colorants are described.

Coating types

An overview of the new trend in powder coatings is presented by Kiefer (4). His article surveys
the major technical advances in powder coatings over the past 40 years. Looking towards the
future, Kiefer remarks that much remains to be done and that powder coatings will continue to
offer positive economical finishing solutions if certain technical hurdles can be overcome. A
state of the art of UV-powder coatings is given by Kersten (5). He discusses the potential of UV-
powder coating formulations. Könnecke presents a more car-coating related aspect of powder
coatings and informs about innovations and perspectives of powder coatings in automotive
coating (6).

„Smart“ or „intelligent“ coatings have become the subject of global research interests. An
interesting application is presented by Xanthos, Chouzouri, Kim, Patel and Young (7). They
report about specific nano-scale additives which permit to formulate a coating reaction
sensibility on pH-changes appearing in a colour change. Such coatings could for example be
introduced to provide early diagnostics of corrosion damages in coatings. Other possible
automotive applications are presented by Bayer Polymers (8).

New colour trends

Surveys show that colour trends are “uncoloured”. So the most popular colours of the last years,
as stated by PPG and DuPont, where silver and black (9,10,11).

Plastics / Polymers

Plastics found their way in the automotive industry, principally in the coating and glazing
sectors. Kouleshova presents new trends for plastic coatings (12). Other discussions about plastic
coatings and their future in the automotive manufacturing are made by Grefenstein (13) and
Barth (14). Daimler Chrysler already introduced plastic coatings in their Mercedes Benz A-
Class and the Smart (15,16).

Art and painting analysis, archaeological analysis

Over 50 articles concerning art and archaeological material analysis were found. Most of
them discuss a very narrow subject, such as the analysis of one specific painting or one
specific archaeological site. This kind of information would not usually be very useful to the
forensic scientist. However, it is very interesting to be aware of the in most cases non-
destructive techniques applied to the analysis of ancient pigments, resins or binder types.
The following table lists the most commonly used techniques for the analysis of ancient
pigments, binder and resins with the relevant citations.

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Pigments # of Citations
citations
Raman Spectroscopy 16 (17,18,19,20,21,22,
23,24,25,26,27,28,29,30,31,32)
EDXRF 6 (24, 33,34,35,36,37)
X-ray Diffraction 5 (19, 20, 21, 32, 38)
IR Spectroscopy 5 (20, 32,38,39,40)
Scanning Electron Microscope 4 (18, 19, 20, 34)
FT-Raman Spectroscopy 4 (38,41,42,43)
Gas Chromatography 2 (44,45)
Optical Microscopy 2 (18, 34)
Laser Induced Break Down Spectroscopy 2 (27, 29)
Particle Induced X-ray Emission 2 (25,46)
Direct Temperature Resolved Mass Spectrometry 2 (47,48)
UV-Fluorescence 1 (45)
Electron Microprobe Analysis 1 (18)
Stable Isotope Analysis 1 (18)
X-Ray Mapping 1 (34)
Py-GC-MS 1 (48)
Rutherford backscattering spectrometry 1 (46)
Synchrotron radiation X-ray diffraction 1 (38)
Elemental Phase Analysis 1 (49)
Voltammetry 1 (49)

Binder
IR Spectroscopy 2 (20, 41)
Gas Chromatography 2 (44, 45)
Thermally assisted hydrolysis and methylation – GC- 2 (47,50)
MS

Resins
Raman Spectroscopy 9 (17, 18, 19, 20, 21, 22, 23, 24, 32)
Thermally assisted hydrolysis and methylation – GC- 3 (45, 47, 50)
MS
Direct Temperature Resolved Mass Spectrometry 2 (47, 48)
Size Exclusion Chromatography 1 (47)

Furthermore, García provides a general overview of the chemical analysis applied to the study
of works of art from the point of view of applications carried out at the conservation and
restoration department of the National Museum Queen Sofia (51).

In order to learn about the material composition of a work of art, one will basically have two
supplementary information sources. The first is an approach of general nature, based on the
use of electromagnetic radiation in a wide range of wave length which allows to generate the
image of other visible objects at sight. Tests of this kind can be included in a general analysis
group. These tests are absolutely necessary and should always be performed before the use of
a second information source, with the help of which the material composition of areas - small,
but representative - is fixed by analytical methods. The techniques included, among others,
are light microscopy, infrared spectroscopy, gas chromatography or electron microscopy, the
application of which will be put forward later.

Kotrly and Turkova also treat a subject related to art analysis, e.g. the pigment analysis of
objects d’art in forensic casework (52).

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They note that the examination of pigments of objects of art is not performed often at forensic
workplaces. It represents a relatively complicated area, in which top instrumental equipment
is not sufficient - large comparative databases and expert experience being necessary as well.
In the author’s opinion close co-operation with top-class restorers and art historical
organisations is essential. Methodology for separation, identification and comparison of paint
systems layers is continuously being specified on the basis of experimental data results. It is a
complex system based on optical methods of transmitted and incident light microscopy,
electron microscopy, microanalysis and XRD analysis. The method of analysis has been
verified on differentiated sets of samples from different historical periods that differ markedly
in the character of used pigments as well as fillers. For collecting samples from artistic objects
a method is employed that eliminates the damage of the examined object. Following a visual
examination and a detailed documentation, the samples from special-interest pigments are
taken under a microscope - primarily from the picture edges and where cleavages or other
damages are visible. These micro samples are photographed and visually described. This is
followed by evaluation with transmitted and incident light microscopy with polarised light. If
the quantity of the sample is sufficient, and if the consistence makes it possible, the separation
of component sample layers can be carried out. Chemical content of individual inorganic
components can be analysed by electron microscopy. It is often possible to isolate separate
particles of inorganic pigments. FTIR analysis is very significant not only for identifying
inorganic component particles, but especially for possible organic phases. In some cases it is
even possible to identify organic binders. GC-MS is used for organic phases in case of
sufficient amount of the material XRD analysis of the phases enables, again in case of
sufficient amount of the material, the performance of detailed phase identification. Micro-
chemical and biochemical reactions are complementary methods. In the case of minimum
material quantity it is preferable to use the technology of pouring the samples with resin and
then processing their section by a rotatory microtomy. The samples can then be directly
examined by optical and electron microscopy and FTIR. A standard application of XRF and
GC-MS methods is not possible in this case.

Keune and Boon introduce static secondary ion mass spectrometry (SIMS) as an analytical
technique for the examination of paint cross sections in order to obtain simultaneous
information about the nature and distribution of pigments and the binding medium from a
single sample (53). From the resulted mass-spectra, images of the elemental distribution of
pigments and the molecular signature of the binding medium were produced. SIMS images
correlate well with SEM/EDX, FTIR, and light microscopic images and the SIMS spectral
data additionally support the identification of pigment particles, lead soaps, and other binding
medium components.

General Paint Analysis and Instrumental Techniques

Colour Measurement and Microspectroscopy (MSP)

At the 3rd European Academy of Forensic Science Meeting in Istanbul (Turkey) 2003,
Piotrowski and Majewska presented a poster concerning Fibre and Automotive Paint Colour
determination with the aid of microspectrophotometry (MSP) (54). They conclude that MSP
in UV-Vis light is the fundamental method for determining the colour of forensic trace
materials such as fibres and automotive paints. The presented poster includes results of
colorimetric examinations aimed at determining colour variation parameters in fibres and
automotive paints, depending on the sample inclination angle and density of pigment
distribution in paint and fibre samples. The degree of similarity between samples is presented
by means of statistical methods.

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A very interesting new setup for reflection Vis-light imaging MSP as well as its evaluation
and applications is described and tested by Van der Weerd, Van Veen, Heeren and Boon (55).
The spatial resolution of the used system is ~1 µm at a spectral resolution of 4 nm. The
optical contrast between different coloured particles in the surface of a sample is optimised
with a new image processing method for mapping of the distribution of the identified pigment
particles. The potential of Vis-imaging in the study of paint cross sections obtained from
paintings is explored. Spectra obtained from pigment particles in these cross sections result in
classification or identification of several pigments. The investigated paint samples are
challenging test cases, as they contain several coloured materials with a very fine distribution.
Vis-imaging can identify and map the most common traditional blue pigments, i.e. smalt,
azurite, ultramarine, and indigo in 17th century oil paintings. Smalt can be identified even
after complete discoloration. Vis-imaging analysis also assisted in the identification and
mapping of modern synthetic red and yellow pigments in a 20th century painting.

Gilchrist speaks about characterising special-effect colours (56). Measurement and

characterisation of these colours is generally done using multi-angle spectrophotometry.
Several instruments are available from different manufacturers. This paper highlights some of
the problems and difficulties in multi-angle measurement and in the interpretation of the data
obtained from such measurements.

Microscopic Examination

Scanning Electron Microscope (SEM), Atomic Force Microscope (AFM) and Confocal
Microscope (CM)

Sjastad, Jacobsen, and Wibetoe discuss the use of SEM as a quantitative tool in paint analysis
(57). Their work presents results from a project in which SEM and an energy dispersive X-ray
analysator have been utilised for quantitative analysis of inorganic material in paint. The
primary target of this work was to investigate whether or not SEM/EDS is suitable for
quantitative or semi-quantitative determination of inorganic components in paint. Different
methods for sample handling and instrumental conditions are investigated to obtain reliable
data and minimise the time-consumption. Different reference-samples containing inorganic
constituents usually found in household paint were prepared in their laboratory. Various
methods for preparation and instrumental settings for the analysis have been tested. In order to
evaluate the discrimination power, the samples were selected with slight differences in
quantity of the same inorganic elements. Prior to the analysis the different quantities of the
element were verified by the use of atomic spectroscopy. To investigate the reliability of the
EDS method for paint, simple statistical calculations were made for each paint sample and the
different technique-regimes under which they were investigated. Another aspect of the
modern scanning electron microscope is the possibility of the analysis of non-conducting
samples without coating of the samples. This is possible when a small pressure of nitrogen is
introduced into the sample-chamber. This instrumental method generates a spread of the
focused beam, which in turn generates a "false" X-ray excitation volume (skirt effect). To
investigate the skirt effect on paint, simple analyses on uncoated paint samples were done to
check the responsibility and to attain reliable quantitative data.

Cathodoluminescence

Götze describes the potential of Cathodoluminescence (CL) microscopy and spectroscopy for
the analysis of minerals and materials (58). He notes that CL can be used both in a purely
descriptive way to detect and distinguish different minerals and as an effective method for

91
spatially resolved analysis of point defects in solids by spectral CL measurements. He
concludes that CL spectroscopy is an outstanding method to characterise the degree of purity
of materials or to detect trace elements in natural and synthetic minerals.

Stoecklein, Franke and Goebel show possible applications for this method in the field of
forensic sciences (59). They note that CL can reveal textures and variations in the chemical
composition of solids such as ceramics, refractory materials, glasses, bio-materials, and
certain minerals which cannot be detected with other analytical methods. Therefore CL has
become a standard technique for mineralogical and petrologic investigations but as yet has not
often been used in forensic science. The authors have therefore examined how this non-
destructive method can provide information specific in the analysis of glass and paint. In this
report the capabilities and limitations of CL-microscopy for classification and discrimination
of sheet and container glass are discussed. These are the most common types of soda-lime
glass found in forensic investigations. In addition the use of CL in examining multi-layered
white/beige paint chips is illustrated.

Chromatography

PY-GC-MS

Challinor describes pyrolysis techniques for the characterisation and discrimination of paint
(60). The author introduces the different pyrolysis techniques for forensic paint analysis and
develops the advantages and disadvantages of such a method.

Armitage et al. also discuss the analysis of forensic samples using laser micro-pyrolysis
GC-MS (61). This technique is used for the analysis of paint, photocopier toner, and synthetic
fibre materials to test the forensic potential of this emerging technology. It uses a laser
Microprobe to selectively target very small parts of the materials for GC-MS analysis.

Whereas the paint and the toner samples were amenable to direct laser pyrolysis, the synthetic
fibres proved transparent to the 1064 nm laser radiation. A vast array of hydrocarbon
pyrolysates was detected from the different materials studied. Unique product distributions
were detected from each sample in sufficient detail to facilitate individual molecular
characterisation (i.e. molecular fingerprinting). The integrity of the laser data was confirmed
by comparison to data obtained from the same samples by the more conventional pyroprobe
pyrolysis GC-MS method. The high spatial resolution and selectivity of the laser method may
be advantageous for specific forensic applications, however, the authors claim that future
work may be required to improve the reproducibility of the data.

Spectroscopic Methods

Infrared Spectroscopy

Beveridge, Fung and MacDougall summarise the use of IR-spectroscopy for the
characterisation of paint fragments (62). They review sampling and analysis techniques,
interpretation of IR-spectra and application of IR-data to the identification and comparison of
paint samples.

Chromex also describes the forensic analysis of automotive paints and pigments by using the
line focus sampling method (63). As Raman spectroscopy requires no sample preparation and
as spectra of intact panels can readily be obtained, this method offers an excellent means to
rapidly screen panes from a reference collection for the presence of certain pigments and the

92
identification of unknown samples or finishes. The key to using Raman spectroscopy in this
application is to limit the power density delivered to the sample while maintaining the same
total number of photons hitting the sample. This is most efficiently accomplished using larger
area illumination with macro-line focusing. In addition, the use of Raman microscopy only
for the analysis of paint samples is implausible due to sample damage and destruction caused
by the intense power density created by the microscope.

Spectra of intact panels and pigments, including samples with clearcoats, were easily
obtained. For certain finishes, which contain pigments that are strong Raman scatters, data
can be obtained in collection times of one second or less. Several examples have been
presented of finishes which have the same Reference Collection of Automotive Paints colour,
but which have different pigment compositions as indicated by their Raman spectra. Raman
spectroscopy when used in conjunction with infrared is a powerful tool for the identification
of unknown paint finishes (64). Furthermore, they specify that Raman and IR-spectroscopy
are complimentary tools that can provide information about the molecular structure of a
sample.

A more specific method of IR-spectroscopy is described by Fabbri et al. (65). They state the
mid-infrared fiber-optics reflectance spectroscopy as a non-invasive technique for remote
analysis of painted layers.

By coupling this technique with Fourier transform infrared (FTIR) benches it has been
possible to perform non-invasive reflectance measurements of layers of paint. The technique
has potential applications for non-invasive analysis of works of art. These measurements can
present large distortions in the spectrum, both in band shape and absorption frequency, which
may depend on the band strength, on the concentration of the sample, or on the optical layout
of the measuring system. Therefore, it is difficult to compare reflectance spectra with those
collected in the transmission mode and, consequently, with the available databases. The work
deals with an overall survey of the limits and problems involved in the application of this
analytical technique, an estimate of the reproducibility of the measurements, and the
development of a correct measurement procedure.

The analysis of spray paints has been initiated by several research projects over the last three
years. Govaert, de Roy and Decruyenaere present their analysis of black spray paints by FTIR
spectroscopy, X-ray fluorescence and visible microscopy (66).

In their searching, black spray paints from different European manufactures were
characterised to investigate various types of criminal offences. A total of 40 black spray paints
were analysed by three techniques: 1. Fourier transform infrared spectrometry (FTIR) using
the attenuated total reflectance technology (ATR), 2. X-ray fluorescence (XRF) and 3. visible
microscopy of a coated surface. The results of the quantitative analysis permitted to classify
spray paints according to binder type and elemental composition. A searchable spectral library
was created. Variations of the paint composition due to can shaking prior to spraying were
taken into consideration. A visible microscopic analysis of a coated surface characterised the
morphology of the paint layer leading to a further discrimination of spray paints. The results
of the latter analysis strongly depend on the structure under a questioned paint coating. This
can severely hamper a comparative study.

Govaert and Bernard (67) report the characterisation of 51 red spray paints from different
European suppliers in order to determine the discriminating power of the sequence of
analysing techniques optical microscopy, Fourier transform infrared spectroscopy and X-ray
fluorescence. Infrared spectra were classified according to binder type, filler and pigment

93
composition and a searchable database was created. Due to the difference in the elemental
composition of spray paint, a further discrimination was possible.

Zieba-Palus (68) as well as Buzzini, Massonnet and Mizrahi (69) discuss the application of
FTIR in examination of spray paints used in criminal offences.

The mainspring force of Zieba-Paulus´ research was the assessment that there is little
information regarding the chemical characteristics and their variation in a population of spray
paints. The identification of the paint visible on the wall as signature or graffiti is very
difficult, because the paint layer is thin and sometimes several layers of different paints are
present in the same place.

Zieba-Palus applied micro-techniques with the aim to estimate the usefulness of FTIR micro-
techniques in examinations of spray paints directly on walls. A model experiment was carried
out. About 20 paint samples which represent different types of paint available on the Polish
market were sprayed on the surface of various kinds of materials, i.e. brick, parget, rough-
cast, stucco, plaster board. The coatings obtained were examined by means of reflection
techniques. The paint samples on the plaster were placed directly on the microscopic stage of
the spectrometer or in the DRIFT attachment, in the infrared beam. The results were
compared with transmission measurements performed for paint micro-fragments separated
from a particular plaster and placed on a KBr plate under the microscope.

The differences observed in the IR spectra of the examined paints were small. However, it
was possible to classify them into five groups according to binder type. The paint samples
belonging to the majority of them contained alkyd resins modified with different agents. Only
one group contained silicon resin. Information about the elemental composition obtained by
means of X-ray spectrometry confirmed the paint characteristics. By analysing the paint
samples directly on plasters it was observed that the results obtained strongly depend on the
structure and the type of the plaster under the questioned paint coating. The binders and fillers
were visible in IR spectra in the case of bricks and parget. However, in most cases the bands
of the basis overlie the absorption bands of the paint components. Thus, it could be concluded
that the reflection techniques of IR method may provide valuable information in the case of
brick and parget, while if the surface of plaster is very rough, the transmission technique is
irreplaceable.

Buzzini, Massonnet and Mizrahi analysed green spray paints in forensic casework (67). Paint
samples from green graffiti and tags on different churches in the region of Lausanne
(Switzerland) were collected and analysed by FTIR. Non-differentiated spectra were obtained
for samples of three churches. A population study was carried out in order to assess the
frequencies of the different green spray paints encountered in Switzerland. Forty reference
green spray paints were analysed with FTIR. Three different binder types were observed, each
of these three categories represents about 1/3 of the population. In each category, subgroups
were created based on the visual comparison of the infrared spectra obtained. In this case, it
was possible to provide the police with information concerning the brand names of the spray
paints used as well as a list of the different shops were such paint could be purchased. Raman
spectroscopy was also carried out on the forty reference paints in order to determine their
pigment contents. In situ analysis was carried out using two different laser sources (514 nm
and 633 nm). The two applied techniques are considered complementary. In their study
infrared spectroscopy principally supplied information about the binder and some extenders
present in spray paints, whereas Raman spectroscopy was providing information concerning
their pigment contents.

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Raman Spectroscopy

The growing importance of Raman spectroscopy as a forensic tool has been evaluated by
Harvey et al. (70). They performed a blind field test evaluation of Raman spectroscopy. The
test utilised two instruments and two operators to analyse a matrix that consists of 58
unknown samples. Samples were searched against a custom hazardous materials reference
library (Hazardous Material Response Unit (HMRU) Spectral Library Database).
Experimental design included a number of intentionally difficult situations including binary
solvent mixtures and a variety of compounds that yield medium-quality spectra that were not
contained in the HMRU library. Results showed that over 97 % of the samples were correctly
identified with no occurrences of false positive identifications. Statistical analysis indicated
equivalent performance for both the operators and instruments. These results indicate a high
level of performance that should extrapolate to actual field situations. Application of Raman
techniques to emergency field situations should proceed with a corresponding level of
confidence.

Bell, Fido and Speers describe Raman Spectroscopy as a rapid, non-destructive, one-step
technique for the analysis of paint (71). They state that Raman spectroscopy can
simultaneously detect both organic and inorganic components within paint samples. It thus
has the potential to give high levels of discrimination between different paints without the
need to use different techniques (FTIR, pyrolysis GC-MS, energy dispersive X-ray analysis
etc.) for the organic and inorganic components.

The authors report on the first phase of a long-term project aimed at establishing the viability
of Raman spectroscopy as a routine analysis of trace paint samples that can replace the
sequence of techniques that is currently used. This programme involves development of
optimised instrumentation followed by extensive studies on variability between samples from
different sources and the factors that may alter the composition of paint after application.

Raman spectra of a large set of commonly-used household paints were measured with
variation of laser irradiance at the sample and the excitation wavelength. It was found that a
tightly-focused laser spot damages domestic paints in the same way as it is known to occur for
automobile paints. The illuminated sample area was therefore increased by using a line-
focused laser (ca. 4 mm x 100 mm), rather than a conventional 100 mm diameter spot.

Very pronounced differences between the Raman spectra to different shades of the same
colour of paint from the same manufacturer are found since. Even if the same constituents are
present, the relative proportions of the various inorganic and organic components varied
between different shades. Of course, the differences between the same colour of paint from
different manufacturers and between different colours were typically larger as entirely
different components had been included in the formulation.

The spectra typically show large numbers of well-defined and identifiable peaks that are a
superposition of the sets of bands from each of the constituents. These change not only when
the nature of the constituents is altered but also when the same constituents are used. They
also change when the same constituents are used but their relative proportions are altered to
give different paint formulations.

Muench (72) also presents the strength of Raman spectroscopy in forensic pigment analysis.
He points out that Raman spectroscopy is a powerful tool to identify substances simply and
fast, to compare substances and to find information not supplied by FTIR or similar

95
techniques. He concludes that Raman spectroscopy is a method of choice to compare
pigments in paint.

X-ray Spectroscopy

The Scientific Working Group for Material Analysis (SWGMAT) Standard Guide for Using
Scanning Electron Microscopy / x-ray Spectrometry in Forensic Paint Examinations has been
published (73). This document is an outline of methods for SEM intended for the use by
forensic paint examiners. The methods employed by each examiner and/or laboratory depends
upon sample size, sample suitability, and laboratory equipment. The term SEM occasionally
refers to the entire analytical system, including energy dispersive X-ray spectrometry and/or
wavelength dispersive X-ray spectrometry. This guide does not cover the theoretical aspects
of many of the topics presented. It does not purport to address all of the safety concerns, if
any, associated with this technology.

X-ray Diffraction

Mazurek, Piotrowski and Miron report of determining crystalline automotive paint

components by the X-ray diffraction (XRD) method (74). They signalise that identifying
crystalline components involves not only elemental composition but its real crystalline form
as well. E.g. titanium dioxide (TiO2) is encountered in polymorph varieties such as rutile and
anatase in tetragonal system and orthorhombic brookite.

The following crystalline components were found in respective paint coats: one component -
barite BaSO4, two components: rutile TiO2 and barite, barite and mica - phlogopite KM3
[F]2[AlSi3O10]; three components : rutile, barite and serpentine variety Fe3[(Si,Fe)2O5](OH)4;
rutile, chlorite (Ni,Mg,Al)6[Al,Si)4O10](OH)8, and talc variety willemseite
(Ni,Mg)3[Si4O10](OH)2; mica-phlogopite, rutile and chlorite-ferrous clinochlore
(Mg,Fe,Al)6[(Si,Al)4O10](OH)8; talc Mg3(OH)2[Si4O10], chlorite-ferrous clinochlore and
rutile.

They conclude that XRD makes an easy identification of relatively isometric form crystals
(e.g. barite and rutile) possible. The crystals appear in specimens in disordered position.
Moreover, plate-like crystals such as mica - phlogopite, talc, chlorite - clinochlore and
cronstedtite that can be found mainly in "metallic" paint coats show a significant texture
effect. These plate crystals are easy to identify in specimens prepared directly from cut out
metal sheet fragments. They can be found in outer automotive paint coats.

LA-ICP-MS

Hobbs and Almirall introduce the trace elemental analysis of automotive paints by laser
ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) (75).

They intend to develop a method to complement the commonly used techniques in a forensic
laboratory in order to better characterise paint samples for forensic purposes. A laser ablation
method has been used to simultaneously sample several layers directly prior to introduction
into an inductively coupled plasma-mass spectrometer for the detection and qualification of
the trace metals present in the layer(s). Time-resolved analysis plots displaying the elemental
response and quantification of selected metals are compared to associate or discriminate paint
samples. Matrix-matched standards were successfully incorporated into the analysis scheme
for quantification of lead in the solid paint samples. Preparation of new matrix matched
standards for quantification of additional element developed for this study are also presented.

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A sample set of eighteen survey automotive paint samples have been analysed with the
developed method in order to determine the utility of LA-ICP-MS for trace element analysis
of paints.

Sequences and Comparisons

Brettell, Inman, Rudin, Saferstein 2001, and Brettell, Rudin and Saferstein 2003 present a
forensic science review over 2 years. The aim of the review is to present a concise survey of
articles appearing in publications that primarily appeal to forensic practitioners. In order to
accomplish this objective the authors have focused their attention on the following journals:
Journal of Forensic Sciences, Science & Justice, Forensic Science International, Journal of the
Canadian Society of Forensic Science, Forensic Science Review, Analytical Toxicology,
Electrophoresis, and BioTechniques, as well as Chemical Abstracts Selects: Forensic Chem.
The first survey encompasses the period from January 1999 through December 2000 (76).
The second review encompasses the period from January 2001 through December 2002 (77).

In order to enlarge the discriminating power of a sequence’s, the complementarity of two

methods is examined. Giang et al. evaluated and combined three complementary methods in
the order of stereomicroscopy, micro-FTIR spectroscopy and solubility tests for the purpose
of matching known and questioned paint samples in an auto accident case (78). Greyish green
paint smears scattered on a silvery grey coated plastic bar were taken from a blue car and
referred to as questioned samples. Green paint chips were collected as known samples from a
green car. These were analysed to determine whether the paint smears found in the blue car
could have been transfers from the green car. Although each of the three methods, when used
alone, suffered from unequal bases for making a comparison (i.e., layering whole paint vs.
smeared paint), insufficient specificity of methodology and the interfering background coating
beneath & smeared paint, the limitations were significantly relieved when three methods were
used in combination. Based on the results presented in this report, the questioned greyish
green paint smears collected from the blue car and the known green paint chips from the
green car are of the same class of paint, i.e. the possibility of the above stated paints transfers
cannot be eliminated.

Ertan and Ertan compared the FTIR spectroscopy and the thin layer chromatography (TLC) in
discriminating various paints in forensic cases (79).

The paint samples used in the study are obtained from the commercial market and car paint
suppliers in Turkey. Depending on the type of paint, different TLC systems are used. The
results showed that the two techniques are complementary to each other as expected.
However, TLC was found to be more effective especially when using more than one TLC
system for a comparison case.

Adamsons reports about a chemical depth profiling of multi-layer automotive coating systems
(80). He notes that detailed chemical analysis of high performance automotive coating
systems can be done with available and relatively affordable set of measurement technologies
including infrared (IR), ultraviolet-visible (UV-Vis) and optical microscopy (OM) based
methods. These tools are very versatile in the ability to do both surface and interface
characterisations, as well as depth profiling. Their utility is illustrated using a broad range of
applications: surface-specific defect analysis, stratification/segregation of network
components, mechanisms/kinetics leading to coating degradation and material loss, UVA
permanence in coating systems and UVA interphase mixing between clearcoats and BCs.
Many of the studies were conducted as a function of exposure time and conditions (i.e.
outdoor/field environments, accelerated ageing) or application conditions.

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Specific Issues in Paint Investigation

Helstroffer, Espanet and Milet present a class identification of rockets types by paint analysis
(81). 22 rockets of 15 different types, coming from 6 countries, have been studied. Sample
paints have been scrapped directly on original rockets or have been taken from fragments of
fired rockets. Quantitative analytical methods employed are: infrared spectroscopy and SEM
with X-ray microanalysis. It could be observed, that infrared spectra of rockets paint systems
are different from other IR spectra of paints: vehicle paints, tool paints, aerosol paints, etc.
This may show, that manufacturers of rockets have to study compatibility with paints and
explosive substances. SEM with X-ray microanalysis give some information about presence
of several elements: lead, zinc, calcium, copper, chrome. It is possible to find, after launch,
some pieces with unmodified paint system qualitative composition (organic and inorganic).
Two rockets of the same type and the same origin have the same paint system. Some samples
cannot be discriminated with the two analytical methods. Some limits subsist in rockets
identification by paint analysis. 3 rockets of different types and different origin could not be
discriminated by the analytical methods. The authors intend to build up a database of infrared
spectra of rockets paints.

Kotrly reports on the documentation of known particle types that are used in the production of
plate-like pigments (82). Image documentation includes visible light microscopy in
transmitted light and polarisation, reflected light and polarisation, mirror objectives and also
particle morphology documented by scanning electron microscope. Spectra from EDS and
FTIR are included. XRD, which is capable of a exact determination of all components,
enables to determine the exact mineralogical variety of mica in the particle matrix, and to
determine the structural modification of titanium oxide, iron oxide.

For the precise colour measurement of these particles a prototype equipment working with
spectrophotometer AVANTES with a CCD scanning element with 2048 channels was
developed. This prototype equipment allows arbitrary tilt and sample rotation towards the
illuminating and measurement fibre optics plane, and independent movement of both fibre
optics in the range of plus ± 90 degrees. The measurement results can be represented by a
graph of absorption in the range of visible light.

Stoecklein reports about the analysis of new plate-like pigments in automotive coatings (83).
He notes that the first step in classifying and identifying plate-like pigments is microscopy
(200-500x). To maintain a library of prepared slides of various plate-like pigments would be
very useful. Exact identification of plate-like pigments is only possible with the application of
a combination of analytical methods: SEM /EDX, MSP and XRD.

Databases

Castro et al. present a FTIR Spectra database of Inorganic Art Materials (84). They have
created a Web-based database containing FTIR spectra of pigments and artist’s materials,
which is called e-VISART (e-vibrational spectroscopic database of artists materials). In their
article, they describe why this database is needed, explain how to use the website and provide
example applications. In Part III: Paint and Glass on the WWW, this website is also
discussed.

Burgio and Clark present a library of FT-Raman spectra of pigments, minerals, pigment
media and varnishes, and supplement to existing library of Raman spectra of pigments with
visible excitation (85).

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Sixty pigments, minerals and media have been analysed by Fourier-transform Raman (FT-
Raman) microscopy in order to assemble a database of reference FT-Raman spectra for
scientists working at the arts-science interface. An earlier library of Raman spectra compiled
using visible excitation has been extended by the addition of 22 further reference spectra
obtained with 780.0, 647.1, 632.8 and/or 514.5 nm excitation. The relative merits of 1064 nm
and visible excitation are discussed.

Govaert presents results about the establishment of a database of spray paint characteristics
(86). Spray paints from different European suppliers were characterised by three analysing
techniques: 1) optical microscopy 2) Fourier transform infrared spectrometry and 3) x-ray
fluorescence. Other European forensic institutes (BKA, Germany and SKL, Sweden) gave
assistance in sampling spray paints and sent them to the NICC. The IR spectra were classified
according to binder type, filler and pigment composition of the spray paint. For the sequence a
discriminating power of 0.988 was calculated. A CD-ROM with a database containing the
spectra of any kind of spray paint coming from co-operating European forensic institutes and
additional information about their elemental composition is available on request at the NICC.
Each year this database will be updated.

Geyer-Lippmann reports about low temperature pyrolysis of polymers (87). At a pyrolysis

temperature of 450° most of the analysed additives decompose into a few compounds. In a
second step the same sample was pyrolised at 800°C, producing nearly the same pyrogram as
observed at 800°C in a one-step process. For the identification of the products by low
temperature pyrolysis, additives for polyolefines from Ciba-Geigy and additives for all kinds
of coatings and polymers from Byk were measured. In the common MS-libraries the spectra
of the additives are not included. Thus, a library with about 100 entries was built up. With this
method an excellent discrimination power is reached in the analysis of polymers and coatings.

A very valuable resource is the FORS literature database provided by the Forensic Science
Service (FSS, England). This database is updated four times a year and can be purchased and
covers the main relevant forensic periodicals. An enumeration of the different periodicals can
be viewed online on the FSS homepage (http://www.forensic.gov.uk/forensic/entry.htm).

EUCAP Background Info

Depriester from the IRCGN notes, that the contacts with the French partners of the agreement
and our European colleagues - specially those of the BKA - provided food for thought and
allowed IRCGN to create the “FRCAP” tool which is now a module of EUCAP (88). Within
the framework at forensic casework, investigators and prosecutors expressed a wish for
intelligence requirements related to paint chip or paint marks from automotive plastic
accessories. The paint plastic accessories are very numerous on the recent vehicles (bumper,
front valence panel, body shell of outside mirror, door handle, etc).

In fact, there are increasingly more plastic parts in modern vehicles. The automotive
manufacturers supply car manufacturers with paint for outside accessories which match in
term of colour an imposed topcoat. Therefore the paint systems of outside accessories are
characteristic of a time period, a vehicle type, a commercial name of a car manufacturer
colour etc. The “FRPLAST” project began in 2000. It is in keeping with the development
pattern of the French collection and the European collection. It corresponds to the usual
method of obtaining exhaustive references of automotive paint systems. There are 1021
physical samples in the “FRPLAST” collection.

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The EUCAP collection includes over 25 000 original paint samples, product information and
analysis data of 23 different Japanese and European car manufacturers since 1975 (21 000 IR-
spectra of clearcoats, basecoats of metallic and pearl effect coats, uni coats, fillers, 1000
X-ray diffraction data as well as several thousand data of colorimetric examination). This data
amount is annually updated with approximately 500 new coating systems, whereby various
samples of one product originating from different cars have to be analysed. Furthermore there
is access to more than 33 000 IR-spectra of US and Canadian car coating collections.

Interesting Cases

Rott present a case work problem including the comparison of two primers (89). In their
routine infrared spectroscopy they used the diamond anvil cell for sample preparation. Since
the phosphate layer is not visible when using low power microscopy, not attention was paid to
a phosphate layer when a sample was prepared for infrared spectroscopy.

The problem was that different infrared spectra of primers were found when comparing paint
samples which made more analytical work necessary. For the detection of a phosphate layer
SEM-EDS is the method of choice but it is also possible to detect a phosphate layer with
ATR-microscopy-FTIR. When paint flakes are separated from coated sheet metal car parts the
phosphate layer may remain on the metal or may be on the underside of the primer.

Depending on the amount of the phosphate-layer residues on the underside of the primer and
on the applied sample preparation different infrared spectra of primers showing the main
difference at 950 cm-1 can be found. Possible solutions for this problem are: Preparing a thin
section using a microtome or mechanically removing the phosphate layer from the underside
of the primer before taking a sample for infrared spectroscopy of a primer.

Books

The book „Forensic Examination of Glass and Paint” edited by Caddy covers two important
areas of forensic science evidence which are often examined by the same forensic scientist
(90). Following an introductory chapter on trace evidence analysis, the book goes on to cover
the manufacturing processes of glass and paint before discussing analytical techniques and
methods for interpreting the data. Chapters on paint cover analytical techniques based on
colour analysis, pyrolysis, infrared spectroscopy, scanning electron microscopy and X-ray
methods. Also, one chapter describes the interpretation of paint evidence.

Another remarkable book is: “Mute Witnesses: Trace Evidence Analysis” by Houck (91).
Each chapter presents the facts of the case, the progress of the investigation and how trace
evidence assisted, and highlights some important aspect of trace evidence as a teaching
module. The chapters are written in a style that is accessible to trace analysts, crime scene
investigators, lawyers and students.

The Forensic Science Handbook published by Saferstein is of general forensic interest and
covers all main fields of forensic topics (92). Chapters are devoted to discussion of
examination techniques for a wide range of evidence found in the modern crime laboratory -
DNA, hair, paint, soil, glass, petroleum products, explosives, alcohol in blood and breath, and
questioned documents. The expanding applications of mass spectrometry, capillary
electrophoresis, high-performance liquid chromatography, and the visible micro-
spectrophotometer are covered.

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PART II: GLASS

Since the last review in 2001 the application of new or improved methods for forensic glass
analysis and new material developments have been observed.

General

An overview of the production of glasses including a table with the applications and
compositions of different glass types is given by Copley (93).

Frequency of occurrence / Transfer and persistence

Roux et al. examine a total of 776 pairs of shoes collected from random members of the
public in south-eastern Australia for the presence of glass fragments (94). From the samples
collected a total of 110 fragments were recovered from 57 pairs of shoes (7.3 % of the pairs
examined). The prevalence of glass fragments in footwear is dependent upon the area of the
shoe from which the fragments were recovered. A much higher percentage of shoes were
found to have fragments embedded in the sole (5.9 %) than in the upper area of the shoe
(1.9 %). These shoes were also more likely to contain multiple fragments from multiple
sources of glass. Only a very small percentage of shoes contained fragments in both the upper
and the sole (0.3 %). These findings and their significance for the interpretation of glass
evidence involving footwear are discussed.

Coulson et al. report on fragments of glass on the outer clothing and footwear of 122 people
attending a gymnasium (95). Both the surfaces and the pockets of the clothing and the uppers
and soles of the footwear were searched. It is reported that New Zealand forensic glass cases
have been reviewed in order to determine the amount of non-matching glass present on the
clothing of people who are suspected of committing crimes. Data from 114 suspects who had
no matching glass on their clothing and shoes have been accumulated. Statistical modelling
techniques have been applied to the data collected.

Massonet et al. collect information on the background population of glass found on the front
seats and carpets of 27 cars (96). Glass was found in 80 % of the cars and a total of 215
fragments was recorded. More glass was recovered in vehicles related to crime than in the
average population of vehicles. About 60 % of the glass fragments were located on the
driver’s floor and 40 % on the passenger’s floor. Only 3 % of them were located on the
driver’s seat and none on the passenger seat. The size of fragments were usually greater than
2 mm. The distribution of the refractive index (RI) is similar to other population studies
carried out in Switzerland. The secondary transfer experiments showed that there is a
secondary transfer of glass fragments from the breaker’s clothing to a car seat/floor but the
amount of glass transferred has been found to be usually low.

Biedermann et al. have performed breaking experiments in order to study the distribution of
glass fragments transferred to headwear, outer clothing and shoes (97). Particular attention
was paid to the relation between quantities of fragments of glass recovered on different
receptor items after variable periods of time. On each experiment at each point of time,
fragments of glass were located on headwear, upper and lower clothing, and shoes.
Coefficients of correlation between quantities of fragments of glass found on headwear and
upper clothing, upper and lower clothing, and lower clothing and shoes respectively, were
found to be positive for those experiments where items were removed immediately after
breaking a window (0 minutes), but turned out to be highly variable for those experiments
including activity (5, 15, 30 minutes). Even under controlled experimental conditions, the

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quantity of fragments of glass found on a given item does not seem to allow predictions to be
made concerning the amount of glass which one should expect to find on another receptor
item from the same person. Nevertheless, fragments of glass may be recovered on several
parts of a person after breaking a window. These distributive aspects represent valuable
information for case-pre-assessment and refinement of conclusions in cases involving glass.

Distribution of refractive index and databases

Koons and Buscaglia evaluate the alterations of the distribution of RI utilising the FBI
laboratory glass database consisting of RI measurements of 2337 samples of glass (98). To
determine whether trends can be found among these data, the database was divided into glass
received before and those received in 1980 and later. The range of measured RI values does
not change appreciably, but the distribution of samples around the most frequently observed
values is much marrower in the post-1980 samples than in those received prior to 1980.
Another clear difference is that in the older glass population there is a greater number of
samples having RIs that are quite different than the most frequently occurring RI. It is pointed
out that using large databases collected during long periods of time, variation over time may
occur, which renders these databases unsuitable for statistical calculations.

Becker et al. present the work of the German project group GRIM. A RI database for scene of
crime and suspect glass material was established (99). The database includes information on
refractive index, standard deviation, number of measurements, annealing, origin, colour,
thickness, glass type, type of crime, date of measurement. The aim of this centralised database
is to enhance the evidential value of a given case regarding the frequency of occurrence and
further relevant questions. Statistical calculations (t-test) and several grouping algorithms are
also integrated into this software.

In order to assure the integrity and quality of the data input, the project group outlined
minimum criteria for case working ("eleven laws" of refractive index measurements), taking
into account existing documents like ASTM E 1967-98. In co-operation with the glass
manufacturer SCHOTT AG a glass standard with a controlled variation of the refractive index
of less then 7*10-6 was obtained. This BKA-K5 standard was distributed to all German
forensic state laboratories. This glass is to be used as an external standard in order to supply
quality control charts and is used as a control standard for the entry of new RI measurements
into the database.

Wachowicz reports on the influence of production technology on the variation of refractive

index of bottle glass (100). The article presents a study of the relationship between production
technology of glass and the refractive index. The study is based on review of literature as well
as measurements of bottles and, additionally, float glass. The work is the first attempt to give
an overview of forensic examinations of glass in Poland, therefore it is addressed mainly to
Polish forensic experts in chemistry and technicians. The major part is dedicated to
fundamental issues such as methods of RI measurement, calibration and validation, procedure
of recovering glass from garments and quality control issues.

GLASS ANALYSIS:

Microscopic investigations

Hamer focuses on the use of different microscopic techniques used for glass examination
starting from the recovery of glass, surface examination, surface luminescence, interferometer

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and the refractive index measurements (101). Also, the procedure of annealing has been
briefly described.

Elemental analysis

The elemental analysis of glass is described by Almirall (102). Beside the forensic and
analytical implications of the composition of glass, the most important techniques such as
atomic spectroscopy (AAS; GFAAS, ICP-OES), X-ray methods (SEM/EDX) and
radiochemical methods (NAA), followed by inorganic mass spectrometry (ICP-MS) are
described.

In order to evaluate differences in the discrimination power of various elemental analysis

techniques for glass, a proficiency test was carried out by Becker et al. (103). Three pairs of
glass samples with similar refractive indices were to be examined using refractive index
measurements and elemental analysis. In this study SEM/EDX, µXRF, and ICP-MS were
used for the elemental analysis. Based on the refractive index measurements alone a complete
differentiation of the glasses was not possible. Annealing of the glass enabled further
differentiation. After the use of the elemental techniques a full differentiation of the six
glasses was possible. The strategies used by different laboratories to discriminate between the
samples and the merits of the various techniques applied are discussed.

SEM

Krüseman reports on the use of Environmental Scanning Electron Microscope (ESEM) in

forensic science (104). ESEM technology combines three microscopy modes in one
instrument and therefore allows the widest range of samples to be investigated. The ESEM
allows imaging and analysis of uncoated, otherwise vacuum unstable, specimens. The SEM is
very suitable for imaging non-conducting materials at high kV. For many materials such as
plastics, polymers, glass, wood, paints, etc., the ESEM allows these types of specimen to be
viewed in the natural uncoated state.

Gaenzle and Blackledge report the application of SEM-energy dispersive spectroscopy (EDS)
to clearly distinguish self-cleaning window glass from ordinary window glass chemically and
visually (secondary electron image) (105). Self-cleaning window glass is only intended for
windows, with the side of the pane having self cleaning properties facing out. The self
cleaning-treated side is always opposite the float glass side. Titanium dioxide at or near the
outside surface interacts with ultraviolet rays from the sun to produce a catalytic effect that
gradually breaks down organic dirt and grime to carbon dioxide and water. Because the
treated surface is hydrophilic, rain (or water from a hose) sheets down the plane washing
away any residues and leaving a surface free of water spots upon drying.
Zadora et al. advocate the use of SEM-EDX followed by cluster analysis for the
differentiation of glass objects revealing the same results for qualitative analysis (106).
Analysis of glass microtraces by means of SEM-EDX method provides an information about
their main elemental content. The lack of information on the trace elements becomes a
difficulty in the case of differentiation of glass objects revealing similar chemical contents,
e.g. vehicle windows and ordinary window sheets. The differentiation of glass objects
revealing the same qualitative elemental composition (determined with SEM-EDX) can be
achieved using an approach based on cluster analysis.

Zadora et al. propose a scheme of glass classification (107). The scheme is based on results of
the quantitative analysis of 153 glass objects of the following categories: car windows, car
headlamps, external glass of car bulbs, internal glass of car bulbs, external glass of ordinary light

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bulbs, internal glass of ordinary light bulbs and window sheets. With the use of the SEM-EDX
method concentrations of aluminium, barium, calcium, iron, lead, magnesium, potassium,
sodium, and zinc were determined. The concentration ranges for each element in each category
of glass were listed and the elements for which the concentration ranges did not overlap were
selected. With this non-statistical approach to the problem of glass microtraces classification a
collection of 153 glass samples was divided into six sets. Then the cluster analysis was applied
for classification within these separated sets. In this approach raw analytical results were
normalised and the Tukey HSD test was used to choose significant variables. The presented
approach leads to the correct classification of the most of the glass samples studied.

XRF

Hicks et al. describe the classification and discrimination of glass fragments using non
destructive energy dispersive X-ray µ-fluorescence (108). Elemental analysis was used both for
classification and discrimination of glass fragments. Classification of fragments has been
achieved using Fisher’s linear discriminant analysis (LDA) and neural networks (NN).
Discrimination was based on Hotelling´s T2 test. Only pairs that were not differentiated by RI
followed by the Welch test were studied. The results show that neural network and linear
discriminant analysis using qualitative and semi-quantitative data established a classification of
glass specimens with a high degree of reliability. For discrimination, 119 windows collected
from crime scenes were compared: using RI it was possible to distinguish 6892 pairs. Out of 129
remaining pairs, 112 were distinguished by µXRF.

Micro x-ray fluorescence analyses were undertaken on individual glass particles of different
compositions for selected particle size between 50 µm and ≥ 1 mm. These experiments reported
by Roedel et al. revealed a complex behaviour in the fluorescence spectra; this behaviour is
influenced by the glass matrix, topology, particle volume, energy range and polycapillary
properties and cannot be corrected by simple approaches (109). The quantitative µ-XRF analyses
of glasses measured as fragments of arbitrary size without additional sample preparation proved
to be difficult because of the diverse nature of influencing factors (energy of excitation and
fluorescence lines, matrix composition and spot size relative to particle size). The resulting
complex behaviour of the fluorescence intensities as a function of the particle size could be
explained, but they are not readily predictable for irregularly shaped glass fragments.
Quantitative determinations with good precision and reasonable reproducibility generally seem
to be possible for fragments of a minimum size at 1 mm, owing to sufficient thickness and
reduced morphological effects. However, significant improvement of the quantification can be
expected if the fragments are additionally embedded in a resin block and ground flat, a relatively
simple form of sample preparation.

Interpretation / ICP-AES

Koons and Buscaglia report the use of inductively coupled plasma-atomic emission spectrometry
(ICP-AES) for glass investigations and assess the discriminating power of this method (110).
The concentrations of ten elements in 209 unrelated glass specimens received were used to
assess the frequencies of errors of false association (Type II errors) using several comparison
criteria at specified significant levels (Type I errors). Pairwise comparisons of the samples using
either the equal-variance t-test or Welch's modification (unequal variances) result in a small
number of errors of false association, even when adjusting the significance level (Bonferroni
correction) for multivariate comparisons. At the 95 % confidence level (overall Type I error of
0.05, or individual element comparison error of 0.005), only two Type II errors are observed in
21 736 comparisons (0.009 %) when using the equal-variance t-test for comparison of sample
means. In this study, the range overlap test using three replicate measurements per specimen

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results in no errors of false association. Most specimen pairs in this data set are readily
discriminated either by differences in the concentrations of several elements or by an extremely
large difference in the concentrations of one element or more.

Zachariadi, Anthemidis and Stratis repot on a study of the effect of the calibration strategy
followed in multi-element analysis of glass matrices by inductively coupled plasma atomic
emission spectrometry (ICP-AES) (111). The accuracy of the determination of two major (Ca,
Na) and four minor constituents (Al, Fe, Mg, Ba) was evaluated by analysing two certified
reference glass materials (SRM 620 and SRM 621) by three different calibration methods
including multi-element and single-element standards. The three calibration methods were
applied successfully in the analysis of archaeological glass fragments and glassy specimens from
an excavated ancient oven.

ICP-MS / Case

Duckworth et al. report work on the assessment of the discriminating power of ICP-MS via the
analysis of variance and pairwise comparisons (112). Glass fragments from 81 automobile side
windows were collected and analysed using ICP-AES. 9 elements (Al, Ba, Ca, Fe, Mg, Mn, Na,
Sr and Ti) were selected for the discrimination among the glass samples. This multi-element
discrimination showed a significant improvement in the discrimination statistics over using only
RI measurements. Fragments from 76 of the original side window fragments using ICP-MS were
analysed. The ICP-MS analyses measured 45 elements using a hierarchical sampling scheme to
estimate variances due to sampled population, variance due to sample dissolution and within
sample heterogeneity, and variance due to replicate measurements. RI measurements along with
ICP-AES and ICP-MS elemental analyses were used for pairwise comparisons of all possible
pairs of the 72 glasses that had a complete set of measurements. The pairwise comparisons used
Turkey's HSD method to compare RI and element-by-element discrimination potential of ICP-
AES and ICP-MS for analysing glass in forensic casework.
ICP-MS was used by Montero et al. to analyse glass evidence from a case in which a person
broke a window in each of 15 vehicles in a parking lot in order to gain entry into the vehicles
(113). The results of the measurement of the properties of colour, thickness, density and
refractive index are reported. A total of 15 known samples representing the windows of the cars
and 42 questioned glass fragments recovered from the suspect and the area at the police vehicle
where the suspect was sitting were submitted for analysis. Density comparisons separated one of
the known samples into three samples, increasing the number of known samples from 15 to 17.
The concentration of 16 elements were measured for all but three of the samples using an
external calibration ICP-MS method with internal standardisation. Colour assessment (non-
instrumental) separated the 17 known samples into two groups, refractive index measurements
resulted in six groups when the Emmons double variation method was used, ten groups were
found when the Glass Refractive Index Measurement 2 (GRIM2) system was used. Elemental
analysis, by itself, differentiated all of the known samples from each other and associated four of
the known sample fragments with several of the questioned sample fragments. The informing
power of RI, density, and elemental analysis comparisons is evaluated and a summary of the case
results is reported.

LA-ICP-MS

Almirall et al. compare the discrimination potential of LA-ICP-MS methods with reported ICP-
MS methods using external calibration with internal standardisation and a solution isotope
dilution method (114). The laser ablation method was simpler, faster and produced comparable
discrimination to the EC-ICP-MS and ID-ICP-MS. It is concluded that LA-ICP-MS provides for
an excellent alternative to solution analysis of glass in forensic casework samples.

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Aeschlimann et al. assess the trace elemental quantification by LA-ICP-MS without matrix-
matched solid standards (115). Desolvated particles from a Teflon microconcentric nebulizer and
particles ablated from a localized position on a solid sample are mixed and introduced
simultaneously into an ICP MS. A two-point calibration method for laser ablation-inductively
coupled plasma-mass spectrometry (LA-ICP-MS) was investigated. The relative accuracy for the
quantitative analysis of NIST SRM 612 glass reaches up to 3 % for concentrations measured in a
concentration range from 15 to 52 ppm.

Trejos et al. present the analysis and comparison of glass fragments by laser ablation-inductively
coupled plasma mass spectrometry (LA-ICP-MS) and ICP-MS (116).

While the solution sample introduction methods using external calibration and isotope dilution
presented excellent sensitivity and precision, these methods have the disadvantages of destroying
the sample and also involving complex sample preparation. The laser ablation method was
simpler, faster and produced comparable discrimination to the external calibration-ICP-MS and
isotope dilution-ICP-MS. LA-ICP-MS can offer an excellent alternative to solution analysis of
glass in forensic casework samples.

Aeschlimann et al. go into a different direction and use LA-ICP-MS in forensic case work
without quantitative analysis, but using PCA to compare the results of different glasses (117).
LA-ICP-MS is used with two variations of principal component analysis (PCA) for objective,
routine comparisons of forensic materials (glass and others) without time-consuming and
destructive sample dissolution. The relative concentrations of trace elements in a solid sample
are examined to provide a "fingerprint" composition that can be used for identification and
source matching of the material. Residue samples are matched to bulk materials using PCA. Four
sets of glass fragments (10 mm2) are investigated. Nine replicates are acquired for each sample
and thirty-two elements are monitored. Despite the close chemical similarity of the four glass
samples, all four glasses are dissimilar at the 95 % confidence level.

Baldwin et al. report on LA-ICP-MS analysis on standard residential window and tempered
glass, indistinguishable by refractive index measurements (118). After the elemental fingerprints
(i.e., mass spectra) and concentrations are acquired for the provided samples, the criteria for
comparison and matching were determined. The primary approach evaluated for
classification/differentiation were: the presence or absence of elements; comparison of the
abundance of selected elements; comparison of relative abundance of selected elements for
specific association patterns; and multivariate analysis of the complete mass spectrum. PCA as a
tool for data compression and information extraction was used for rapid analysis of samples
without time-consuming pair-wise comparison of samples.

Trejos and Almirall study the effect of fractionation on the forensic elemental analysis of glass
using LA-ICP-MS (119). Two different approaches are used to evaluate the fractionation:
fractionation index and U/Th ratios. The standard reference materials NIST 612, 610, and 1831
are analysed in triplicate by both methods (n=55) along with a set of 10 casework samples
originating from different automobiles. The resulting fractionation index values indicate low
fractionation for the majority of elements evaluated, ranging between 0.8 and 1.2. The U/Th ratio
suggests a higher fractionation at the beginning of the ablation process. The authors conclude
that forensic analysis of glass can be performed by LA-ICP-MS with high confidence when
elemental analysis is required.

Becker et al. report on the improvement of quantitative analysis of float glasses by LA-ICP-MS
by the production and use two matrix matched standards (120). These forensic float glass
standards (FGS) resemble float glass (soda-lime glass) composition, but vary in their

106
concentration of the added elements by a factor of 5. Elements such as Al, K, Fe, Li, Ti, Mn, Rb,
Sr, Zr, Sn, Ba, La, Ce, Nd, Hf, Pb have been included bases on their abundance in glass and their
good variation between different glasses (discrimination potential). Activities regarding the
validation of the two new float glass standards carried out by participants of the EU-funded
NITE CRIME network (Natural Isotopes and Trace Elements in Criminalistics and
Environmental Forensics) for typical glass case-work using LA-ICP-MS are described.

Mason and Monk use LA-ICP-MS as a tool for depth-resolved analysis of glass and metal
samples (121). Layered experimental samples of known thickness are ablated using 266 nm and
193 nm laser systems. The controlling parameters are power density of the laser, crater geometry
and gas medium. Layers at depths of up to 200 µm can be identified, but accurate determination
of the composition of the underlying layer in the material is strongly dependent on the
parameters used. Continued ablation of material from the upper layer is observed for up to 200
laser pulses after penetrating the underlying layer. Depth resolution is limited by the mixing of
material between shallow and deep levels in the ablation crater. Optimum conditions are
determined for reducing the mixing effects and for accurate compositional analysis.

Schultheis et al. report the application of laser ablation- magnetic sector field inductively
coupled plasma mass spectrometer (LA-ICP-SF-MS) for the characterisation of historic glass
samples by Pb isotope ratios (122). Iridescent Art Noveau lead crystal glass samples were
analysed and it could be proved that the material of the single layers originates from different
glass sources. A successful differentiation of samples the archeological site in Ephesos was
achieved by Pb ratio measurements whereas multi element pattern did not allow grouping the
data.

Miscellaneous techniques

Stoecklein, Franke and Göbel investigate the use of cathodoluminescence (CL) of glasses by
SEM (123). The authors examine how this non destructive method can provide information
specific to the analysis of glass and paint. The capabilities and limitations of CL-microscopy for
classification and discrimination of sheet and container glass are discussed. A wide band with a
maximum of 495 nm was characteristic for the tin(II) luminescence of float sides of soda-lime
glasses. A high tin count in soda-lime glass leads to a depression of the CL signal. It appeared
that ions with a higher tin concentration tin(II) were oxidised to tin(IV) that do not contribute to
CL.

Anfone and Marcus report the analytical characteristics of rf-GD-OES for the elemental analysis
of bulk solid glass specimens (124). Linear calibration curves over the range on ~1-500 ppm are
obtained using the Ar(I) signal emission as the normalising internal standard. The samples used
in this study were a NIST 1412 multicomponent glass standard and NIST Trace Elements in
Glass reference series 610 (3 mm thick), 611, 613, 615, and 617 (1 mm thick) glass wafers, and
ordinary plateglass samples (1-~5 mm thick).

Tibi and Heumann report that the determination of trace elements in pure quartz glass samples
has been performed by coupling an ICP quadrupole mass spectrometer with the LINA-Spark-
Atomizer, an IR laser ablation system dedicated to direct bulk and surface analysis of solid
samples (125). Unlike LA-ICP-MS, currently the preferred method for the direct analysis of
solid samples, LINA-Spark-ICP-MS is unable to perform analyses with high spatial resolution
because of a lack of optical devices.

Fernandez et al. report the direct solid quantitative analysis of glass by radio frequency (rf) glow
discharge-optical emission spectrometry (GD-OES) (126). The calibration using special silicate

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glasses of very different composition (e.g., the SiO2 content varied from 0 to 75 %, the CaO
content from 0 to 25 %, etc) is investigated in detail. Results for the simultaneous determination
of the glass major components (SiO2, Na2O, CaO, MgO, Al2O3, and K2O) in two samples of
different thickness showed good agreement with expected results.

Dexian, Litang and Shanwu used polarography for the determination of iron (127) and selenium
(128) in flat glass.

Glass treated on its surface with silver compounds and an aluminosilicate, such as ochre or clay,
at higher temperatures (between 550 and 650°C) accepts a wide variety of a yellow colour.
Jembrih-Simbürger et al. investigate the parameters of the manufacturing process affecting the
final colour of silver stained glass and to correlate them with the final colour and colour
intensity. Energy dispersive X-ray fluorescence analysis (EDXRF), scanning electron
microscopy (SEM/EDX), transmission electron microscopy (TEM), as well as ion beam analysis
(IBA) with an external beam. Particle induced X-ray emission (PIXE), particle-induced gamma-
ray emission (PIGE), and Rutherford backscattering spectrometry (RBS) were carried out in
order to obtain the thickness of the Ag-rich surface layer and the depth distribution of Ag.
Results obtained with SEM/EDX at cross-sections of the glass samples could be confirmed by
PIXE, PIGE, RBS, and TEM. (129)

Interpretation

Thornton covers physical aspects of glass evidence (130). The significance of physical matches
of fractured glass is discussed and the different kinds of fractures in flat glass, container glass
and automobile glass are described. Furthermore the glass fractures caused by firearms and other
issues such as glass in fires and the retention and persistence of glass fragments on clothing are
described.

Bennett et al. study the spatial variation of refractive index in a pane of float glass (1.2 m x 1,2 m
x 4 mm) (131). It is found that, although there were no systematic differences in refractive index,
there were observable differences across the pane.

Curran et al. have published a book on the forensic interpretation of glass evidence (132). In six
chapters a wide range of topics of glass investigation has been presented. Starting with the
examination of glass, the conventional approach to evidence interpretation is presented. The
Bayesian approach to evidence interpretation was presented for improvement. A discussion of
frequency of occurrence studies and transfer and persistence studies is followed by a chapter on
statistics. The book ends with a report on glass evidence with a focus on the verbalisation of a
likelihood ratio.

Bottrell and Webb have reviewed the book stating that rather than being a treatise on the forensic
interpretation of glass evidence as the title indicates, this book clearly advocates the Bayesian
method (133). They state, that neither the strengths of other methods nor the weaknesses of the
Bayesian approach has been addressed. The value of this book is that it presents many of the
considerations that must be made in the interpretation of glass evidence. These considerations
are an integral part of both the traditional and Bayesian approaches to evidence interpretation.
Therefore, the concepts presented in this book should be of interest to all trace evidence
examiners, but an impartial critical review of the strengths and weaknesses of the various
methods of interpretation would, ultimately, better serve the forensic science community.

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Maxwell has also reviewed the book and declares it to be an outstanding text book for trace
examiners who provide a statistical analysis of their data, or for those who wish to learn about
the statistical treatment of evidence (134).

NicDaéid covers the statistical interpretation of glass evidence (135). She outlines the issues of
grouping, coincidence probabilities and the Bayesian approach for glass investigations.

According to Newton et al., in forensic cases the variance of the recovered glass refractive index
(RI) has been observed to be larger than the variance of the control glass RI (136). This has
consequences for subsequent interpretation. To investigate this phenomenon, a study is
undertaken of the probable distributions of refractive indices of the recovered glass given a range
of casework type scenarios involving breakage and backscatter. An investigation of the
consequences of any distribution differences with regard to casework is also carried out. It is
discovered that the inclusion of surface fragments from the float surface of the glass can have a
profound effect on the comparison of recovered and control glass samples. The effect is largest
when a breaker strikes the float surface of a window. In particular, it is found that with the
inclusion of a few surface fragments even post grouping alone is sufficient to explain the
observed difference in variance of RI between control and recovered groups. Surface fragments,
if present, are very likely to be treated as outliers and to be deemed as non-matching. The
findings of this paper challenge routine glass examination procedures and suggest that
knowledge of which surface is facing the striker is valuable information in interpretation.

Collins et al. describe a previously unreported type of GSR particle consisting of glass fused
with other primer components (137). In many types of 0.22 caliber rimfire ammunition, the
cartridge contains a primer sensitised with glass. Scanning electron microscopy with energy
dispersive X-ray detection (SEM-EDX) and time-of-flight secondary ion mass spectrometry
(TOF-SIMS) were evaluated for the characterisation of glass-containing GSR particles. The
occurrence of glass-containing GSR particles was established in the residue from various brands
of 0.22 caliber ammunition, and several sub-types were identified.
Studies on float glass

Ma et al. investigate the bloom on float glasses (138). Bloom is an interference pattern of optical
wave caused by the wrinkling surface of the heat treated float glass. The ratio of transmittance of
float glass after heat treatment to that before, =Tafter/Tbefore is used to describe the bloom
and it is defined as the bloom parameter for the float glass. The following results were obtained
for the bloom parameter by experiments and calculations: The bloom parameter is a good
description the light or heavy level of the glass bloom. The smaller the parameter, the heavier the
glass bloom. The parameter is approximately proportional to the total amount of tin in the glass;
it decreases by exponential law as the treatment temperature increases; no definite relation exists
between it and the tin concentration on the glass surface.

Moseler, Heide and Frischat investigate the topography and nanostructure of several technical
borofloat and soda-lime-silicate float glasses by a high-resolution atomic force microscope
(AFM) (139). In analogy to thin film technology a simplified model was developed and a free
buckling length of ~ 2,3 m was estimated for the bloom surface, which is in reasonable
agreement with the experimental finding. It was further shown that a sol-gel derived SiO2
coating of the bloom surface could enhance the optical transmission of the glass considerably.
The irregular ripple pattern of the as-received atmosphere an tin bath side surfaces were
measured as well as also the topographies of fracture surfaces. Inhomogeneities like precipitates,
crystals, phase separations or pores, caused by the in-diffusion of tin into float glass, could not be
evidenced. After annealing the float glasses in air several of them showed bloom, which
produces a greyish haze. The borofloat glasses and the silicate float glasses with a high Fe2O3

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content (>0.5 wt.%) did not develop bloom, whereas the Fe2O3-poor glasses displayed -
depending on sample size and annealing conditions - a pronounced bloom effect. In depth
analysis of the glasses showed that in the case of the Fe2O3-poor silicate float glasses a reversed
Sn2+ diffusion from the interior to the surface occurs, forming there a very high and steep tin
(Sn2+) hump.

Hayashi, Matsumoto and Kudo discuss mechanisms and chemical effects resulting from the
surface tin enrichment on float glass (140). Concentration depth profiles of tin, measured by XPS
in the near surface region, have shown that the tin concentration in the first few manometer at the
surface is extremely high compared to that deeper into the bulk. It has been shown through heat
treatment of glass containing tin oxide as a bulk component, that the surface tin enrichment
arises from the migration of Sn2+. towards the surface during the annealing lehr process. It was
also found that the amount of tin enrichment at the surface had an inverse correlation to the
surface iron concentration. The reason for dependence on surface iron concentration is explained
in terms of a redox reaction between Fe3+ and Sn2+ and a relatively low diffusion coefficient of
Sn4+ compared with Sn2+.

Gläser reports the influence of low-emissive coatings on the outer surface of window glazing
(141). Low-emissive coatings on the base of SnO2 are on the market (K-glass and SolarE) which
partly fulfil the requirements of such an application. The development of better coatings is a
demand for the future. On the base on the reported benefits of low-emissive coatings on the
outdoor surface a new generation of insulating glasses for window glazing can be created. The
basic construction of the window with the low-emissive coating on the outdoor surfaces is
reported.

Holland et al. employ photoelectron spectroscopy (XPS ) in order to derive chemical state
information from which the structure of oxide glasses can be determined (142). Photoelectron
spectroscopy is proving to be a powerful tool for the study of the chemical state of species at or
near the surface of a glass. For the first time it has been shown, that the technique itself can be
used to modify a glass surface and in so doing, generate additional information about the various
structural species in the glass. A specific example of the use of XPS to study chemically induced
changes to a glass surface has been given.

Nemilov deals with the physical ageing of silica glasses (143). The presented review has been
devoted to the problem of volume-determined properties relaxation of silicate glasses at room
temperature. A system of calculated parameters is proposed which characterises the
completeness of ageing and its rate at any glass age. Optical and thermometric glasses have been
ranked by their tendency to ageing.

International networks:

SWGMAT

During the reporting period the glass subgroup of the Scientific Working Group of Materials
Analysis (SWGMAT) met on an annual basis. Subgroup members originate from forensic
laboratories around the U.S.A. and Canada. The main focus of the group was the production of
Guidelines for forensic glass analysis. These guidelines are separated into the sections:
Introduction to Forensic Glass Examination; Collection, Handling, and Identification of Glass;
Initial Examinations of Glass; Fractures; Density Determination; Refractive Index
Determination; and Elemental Analysis of Glass. Final drafts of these documents have been
presented for voting in 2004 and in case of acceptance these documents will be presented online
on Forensic Science Communications.

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ENFSI - European Glass Group (EGG)

The ENFSI glass group (EGG) associated with the ENFSI paint group (EPG) meets on an annual
basis. Experts from most of the 51 ENFSI institutes attend these meetings. During the reporting
period the main activities were the organisation of proficiency tests for refractive index
measurements on an annual basis and two proficiency tests for the use of scanning electron
microscope (SEM) for quantitative analysis of glass. Best practice guidelines for several areas of
forensic glass analysis have either been completed or are still under preparation. These
guidelines are separated into the sections: Introduction; Forensic aspects of glass; Technical
methods (SEM, statistics, Microscopic techniques). Information on ENFSI can be found under
www.enfsi.org.

Books:

Lee and Harris give an overview on the treatment of glass evidence including documentation and
collection and laboratory analysis of glass evidence in easy terms (144).

Höland and Beall have published a book on glass-ceramic technology (145). The book covers
various aspects of glass-ceramics. Besides the principle of glass-ceramic formation and the
microstructure of glass-ceramics, it focuses on the composition systems for glass-ceramics and
the applications of glass-ceramic.

Lohmeyer et al. have edited a book in which a variety of glass related topics are covered in 20
chapters (146). The topic range from special glasses for high tech applications, methods for the
hardening of glasses, sol-gel and CVD coatings on glass surfaces, the use of foam glass for heat
insulation, and other areas.

In the Color Atlas and Manual of Microscopy Petraco and Kubic cover the area of specimen
preparation and characterisation of glass (147).

Brill reports the results of chemical analysis of 3300 samples of early glass and related materials
im two volumes (148,149) Volume 1 describes the origin and the types of glasses including
results of oxygen isotope analysis of early glasses, whereas volume 2 consists of tables of
elemental analysis of the glasses.

PART III: QUALITY MANAGEMENT AND INTERPRETING EVIDENCE

Robertson states that we must respond to new challenges and opportunities if we are to embrace
the notion of forensic science being a truly integral component of the future law enforcement
environment (150). This will require us to rethink what our success measures are. In this
environment our aim should be to produce adequate solutions that are an integrated component
of intelligence as well as the investigative process. Our challenge will be to maintain our
standards. With this in mind, quality assurance and interpreting evidence become a central topic
in forensic sciences.

Reference materials (RM)

Meyer and Matschat report on reference glasses for the glass industry. Selected reference
materials for different types of glass are listed with their elemental composition (151).

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Barwick et al. repot the use of reference materials including the use of certified reference
materials (CRM) for instrument calibration, the assessment of the accuracy of analytical data,
and the assessment of uncertainty (152).

Buzoianu reports about reference materials and certified reference materials for spectrometry in
Romania (153). Several reference materials (RMs) and certified reference materials (CRMs) are
widely used in Romania as measurement standards in different spectrochemical measurements.
A short review of the locally available elemental RMs and CRMs used in atomic spectrometry or
in other analytical techniques, in which aqueous standard solutions are required, is given. The
experience of the INM in preparation and certification of such materials is described. Some
aspects regarding their use for ensuring the accuracy and for confirming of the traceability of
analytical measurements, especially through calibration and metrological validation of main
instrument performances, are discussed.

Interpreting Evidence

A general consideration of evidence evaluation is made by Aitken (154). He elucidates that the
evaluation of evidence requires consideration of scientific evidence under two propositions, that
of the prosecution and that of the defence, and is often concerned with the evaluation of so-called
transfer evidence or trace evidence for identification purposes. Bayesian methodology does not
lead to "true" probabilities: it is an effective method to analyse, criticise, check the "coherence"
of peoples opinions and help people revise their opinions in a coherent ways.

Garbolino and Taroni present the evaluation of scientific evidence using Bayesian networks
(155). Bayesian networks provide a valuable aid for representing epistemic relationship in a
body of uncertain evidence. The paper proposes some simple Bayesian networks for standard
analysis of patterns of inference concerning scientific evidence, with a discussion of the rationale
behind the nets, the corresponding probabilistic formats, and the required probability
assessments.

The same authors remark that it has been shown that Bayesian networks provide a valuable aid
for representing relationships between characteristics in situation of uncertainty, unpredictability
or imprecision.

Their poster proposes a further development of graphical methodologies using probability trees
which can help to explain the rationale behind the Bayesian networks and the relative formulas,
to make clear the meaning of the variables and of the required probability assessments (156).

Evidential Value of Paint

Edmondstone et al. discuss the assessment of the evidential value of automotive paint
comparisons (157). The study was undertaken to assess the probability of encountering
automotive paints that cannot be distinguished from one another in randomly selected samples.
A set of 260 automobile samples was collected at an impound yard from recently damaged
vehicles. The samples were compared along each other using optical microscopy and when
required, infrared spectroscopy. This represents a total of 33.670 samples per comparisons. Only
one sample pair, originating from vehicles manufactured at the same assembly plant in the same
year, could not be distinguished. These results provide the forensic paint examiner with
information with which to assess the evidential value of automotive paint.

Buzzini et al. present a survey of crowbar and household paints in burglary cases, especially
population and transfer studies and a bayesian approach to paint transfer in such cases (158).

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Concerning the population study, the most common combination of blue tool paint observed by a
Swiss Police has been “Blue” and “NCL+AlkOph+PB” as the chemical composition (after visual
comparison of IR spectra). The rarest combination was the “Blue” and “AlkOph” as the chemical
Composition (after visual comparison of IR spectra). It was observed that the quantity of paint
transferred depends on the type of paint, age of paint, type of material of surface receptor. It does
not depend on the location of paint on blades, type of blade of tool (single or double bladed end)
and the form of paint (fragments or abrasions). The authors propose a bayesian approach to the
problem first at the source level and then at the activity level with consideration of the estimated
parameters. They also consider cross transfer evaluation evidence found on the crowbar. They
conclude that rarity of paints expressed by the relative frequencies is confirmed to be the most
important parameter for paint interpretation. They also conclude that every simulation produced
a transfer of paints following the Locard´s exchange principle and that a cross transfer
framework could be supplied by a likelihood ratio, resulting from two conditional likelihood
ratios for direct and respectively inverse transfer.

Buzzini, Massonnet and Ferrari discuss the interpretation of household paint transfer in a
burglary case with foreign paint traces found on the blade of a crowbar (159). The paint traces
were blue, pink, and white in colour. The forced door at the burglary scene presents a two layer
paint system with a blue external layer and a pink internal layer. These paints were analysed
using infrared (FTIR) and Raman Spectroscopy (laser source: 514 nm). The infrared spectra of
the blue and the pink traces were indistinguishable from the respective layers of the reference
paints originating from the forced door. Raman spectra were also recorded for the blue paints
and were indistinguishable from the trace and the control samples. Pink paint samples fluoresced
and could not be recorded. Some of the pink paint particles found on the crowbar blade presented
small blue inclusions: the Raman spectra of these blue micro-fragments were also
undifferentiated from the blue control layer, supporting the hypothesis that the pink and the blue
paint traces originate from the same source.

Considering the non-differentiation observed between the trace and the control, what should the
forensic scientist conclude? In this case, the scientific evidence was evaluated at the Source level
based on the hypothesis that the paint traces originate from the forced door and the alternative
hypothesis stating that the paint traced does not originate from the forced door. The likelihood
ratio was estimated on the basis of the relative frequency of the encountered paints expressing
their rarity. Frequency distributions were estimated on the basis of two different population
studies: The first, based on colour distribution, concerned the foreign paint groups present on the
blasted of 207 crowbars seized by Swiss police on suspects or abandoned on burglary scenes.
The second concerning the combination of colour, layer sequence and chemical distribution of
household paints taken from doors and/ or windows forced with a tool during burglaries. These
paint samples were taken by the Swiss police during their scene of crime examination.
Numerical likelihood ratios based on experimental data were calculated in order to help the
scientist to set his conclusion. This example shows the impact of paint evidence in a case where
it was the only element present in the investigation.

PART IV: PAINT AND GLASS ON THE WORLD WIDE WEB

The World Wide Web has become one of the most important communication and information
platforms of the 21st century. Almost every manufacturer represents and provides his products on
an official website or can at least by contacted by an official email address.
For the forensic scientist innumerable links, discussion forums and information panels exist in
every imaginable field of research. But it is a difficult task to epitomise the actual state of
Internet resources available as the web is continuously subject to change and updates.

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Nevertheless we decided to briefly represent some interesting websites in this paint and glass
review.

General analytical links:

General links on technical resources and tutorials concerning separation and spectroscopic
analysis techniques can be visited at http://www.uni-wuerzburg.de/mineralogie/links/tools. At
the same address you will also find links to glossaries, dictionaries and encyclopædias
concerning microscopy and chemistry.

On Reddy´s Forensic Page (http://www.forensicpage.com/new16 ) one can visit a link collection

to mass spectrometry, X-ray fluorescence, FTIR, etc. A similar site for microscopy and imaging
resources on the WWW is available at
http://www.swehsc.pharmacy.arizona.edu/exxpath/micro/index.html with distinguished links on
light microscopy, confocal microscopy and electron microscopy.

The two sites http://webmineral.com and http://mineral.galleries.com/minerals cover the

inorganic chemistry.

At http://www.spectroscopynow.com the freely registered visitor can find an interesting source

of information regarding spectroscopic fields such as Raman spectroscopy or IR spectroscopy
with suitable tutorials.

Paint:

The excellent site http://www.coatings.de provides a comprehensive link collection, meeting and
conference reviews and a lot of manufacturer links. The most exciting part of this website might
be the archive keyword search modus of the two journals “Farbe & Lack” and “European
Coatings Journal”, two periodicals including actual market information and paint innovations.

Of course, a large number of manufacturers present their products on the WWW. At irregular
intervals, the Journal “Paint & Coatings Industry (PCI)” publishes a website locator containing
information on new interesting homepages with a short content description. The forensic
examination of paint with various analytical techniques requires reliable background information
concerning spectra.

On the Motor Web (http://www.geocities.com/paranders/plus.html) a world-wide car

manufacturer link collection can be found.

www.autointell-news.com supplies recent global production information of the most important

car manufacturers.

http://www.ppg.com/MaxMeyer/CarColourRange provides the solid coating colour of diverse

car manufacturers up to the year 2001.

http://chem.ucl.ac.uk/resources/raman/speclib.html presents an online Raman spectra library of

ancient pigments before 1850 AD.

Another library that is accessible free of charge is the database for certified reference materials at
http://www.comar.bam.de.

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At http://www.fis.unipr.it/~bersani/raman.html a free database containing 197 Raman Spectra of
minerals is available.

For IR and Raman spectra standards and comparative spectral data of the study of works of art,
architecture and archaeological materials, contact: http://www.irug.org, an online user group
offering a spectra database which is searchable free of charge.

A general overview of diverse spectroscopic databases available on the WWW is given by H.

Lohninger at http://www.lohninger.com/spectroscopy/dbsurvey.html.

At http://www.colour-index.org it is possible to subscribe to the Colour Index International.

Glass:

A must is the page http://www.glassonweb.com with an outstanding link collection including

sites of every important glass manufacturer or other related suppliers as well as a glass manual
and an extensive glass glossary. Visiting the websites of glass manufacturers allows to spot new
technical inventions on the glass market as well as to download internal research publications.
Every link is accompanied by a short description of the manufacture’s main activities.

The elaborated manual includes all main glass types. Every type is specified both with a brief
description and various web links. You are thus automatically forwarded to a8manufacturer’s
website if this site encloses for instance images or technical descriptions with regard to the
chosen subject.

Even if it were superfluous to give detailed information about the numberless manufacturers
sites, it is advisable to spend time to follow the links in order to find educational resources such
as the nice and briefly commented flash animation of the float process on the Glaverbel
homepage at http://www.glaverbel.com or the new trends in automotive glazing from Saint-
Gobain Glass presented on their glass car on http://www.saint-gobain-
sekurit.com/anglais/metier/cptcar.asp.
Another remarkable manufacturer website is http://www.schott.com of the Schott concern and
the PPG website http://www.ppg.com with technical reports that can be downloaded.

At http://www.netnz.com there is an interesting link collection treating glass art sites. Similar
information on various glass museums such as the Corning Museum of Glass (NY, USA)
www.cmog.org, or the Schott Glass Museum (Jena, Germany) www.schott.com/museum can be
found.

At http://www.xtek.net/catalogue/forensic/grim2.shtml a short presentation of Foster and

Freeman´s GRIM 3 can be found including the GRIM3 brochure, the manual and the reference
oil data, which can be downloaded.

At http://www.fbi.gov/hq/lab/handbook one can consult the actual handbook of Forensic

Services revised in 2003 by the FBI.

With the link: http://www.stats.waikato.ac.nz/Staff/curran/index.html one reaches J. Curran´s

homepage with the software STAG (Statistical Analysis of Glass), Transfer (program for
exploring transfer probabilities) and his thesis concerning the applications of bayesian inference
to glass evidence. All information can be downloaded.

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Links for material analysis / Miscellaneous:

At http://www.nitecrime.eu.com information concerning the European Union-funded network

NITE CRIME (Natural Isotopes and Trace Elements in Criminalistics and Environmental
Forensics) can be found.

At http://www.forensic-isotopes.rdg.ac.uk the Network Developing Forensic Applications of

Stable Isotope Mass Spectroscopy can be found. A Newsletter informs about recent abstracts.
Following a link to the FIRMS (Forensic Isotope Ratio Mass Spectrometry) Conference the
according poster and presentation proceedings can be found.

The two sites http://www.uspto.gov and www.dpma.de represent the two patent search databases
(USA and Germany) are available.

Acknowledgements

We take the opportunity to thank Dr. Christa Dern for vigorous proof reading.
We would also like to thank the colleagues of the unit KT13 of the Forensic Science Institute,
especially Mrs. Katrin Prasch for the online literature search.

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 Forensic Geology

— A Review: 2001 to 2004 —

Ritusko Sugita, MSc 1) and Shinichi Suzuki, PhD 2)

1) Senior Scientist of Trace Evidence Section
2) Chief of Trace Evidence Section
National Research Institute of Police Science, Japan

Corresponding author:
Ritusko Sugita
National Research Institute of Police Science
6-3-1 Kashiwanoha, Kashiwa
Chiba, 277-0882, Japan

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INTRODUCTION:

The “Forensic geology” has a long history as stated in the former review of forensic
examinations of soil evidence (1) and Marumo (2). This review includes some older
publications, which were not covered by them because the review topic has changed to
“geology” from “soil”. Soil is known as complex of various organic and inorganic matters
derived from natural and artificial origins. The history of soil is reflected in its property, for
example colour, particle size distribution, minerals contained and invisible chemistry. The
studies on useful property are surely the important matter of forensic geology. It is also expected
to utilize new analytical methods and information of related sciences.

Meetings

The most significant event during the review period was the meeting “Forensic Geoscience:
Principles, Techniques and Applications” held on 3-4 March 2003 at Burlington House of the
Geological Society, London by the effort of Pye and Croft (3). It was probably the first
international meeting focused on only forensic geoscience to share knowledge and experiences.
Two full days meeting was filled with various topics, for example, basic techniques, researches,
and applications to case works. Delegates were not only from forensic laboratories but also from
academic fields and private companies. Their study fields consisted with wide fields: such as
geology, microscopy, archaeology, botany, geography and others. There were twenty-five oral
and sixteen poster presentations by the scientists from Canada, Italy, Japan, the Netherlands, UK,
and the USA. The overview of forensic science was stated by Murray (4), importance of
microscopy and a technique for microscopy was explained by Palenik (5), further new
techniques and applications were reported by these delegates.

Study group of trace evidence of natural origin has established in 2002 as a part of the Japanese
Association of Science and Technology for Identification. The aim of the group is to share their
knowledge and information required for examination of trace evidence of natural origin, for
example soil, rocks, minerals, plants and so on. This meeting has been held annually( 6).

Soil transfer

Soil transfer is often recognized on many substances in many cases, and the recovered soil
evidence is examined and compared to control samples. While performing examination, forensic
geologists concern if the property of recovered soil from clothes or tools of the suspects are the
same to the origin, and if not so how much difference there are. However, it had not been closely
studied yet. Recently, soil transfer to footwear was studied by Chazzottes et al. (7) and Croft and
Pye (8). They compared recovered soil from footwear to original soils in experimental cases.
Chazzottes et al. (7) statistically discussed discrimination potential of particle size analysis. Croft
and Pye (8) compared four different methods, namely color analysis, particle size analysis, stable
isotope ratios and bulk chemistry. They are preliminary studies and it is expected it will be
continued to clarify the property of recovered soil evidence.
Bebris (9) approached this problem by the different way. Experiment of dust transfer from
unpaved road to a car rear bumper and wheels was performed. Dust collected from the car was
analyzed by powder X-ray diffraction method (XRD) and compared mineral assemblages to dust
samples from roads. Relative intensities of dolomite and calcite to quartz (Hdol and Hcalc
respectively) were calculated and dust samples were classified by Hdol and Hcalc values. Driving
condition and other factors, which should be concerned on examination of such evidence, were
also discussed in this paper.

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Inorganic Analysis

Although significant improvement of traditional methods was rather scarce in this period, some
new analytical techniques were introduced into this fields.

Small amount of minerals were analyzed using standardless synchrotron radiation X-ray
fluorescence (SR-XRF) by D’Angelo et al. (10) and thickness of the sample and the
concentration of element was calculated. The method is on the way of improvement and seeking
to use thin solid such as thin sections. SR-XRF has high potential to analyze small samples, and
it has already applied to various trace evidence (11). This technique is also expected to apply in
forensic mineral analysis. Gorunushkin et al. (12) conducted an experiment to identify
particulate of geological materials using microscopic laser induced breakdown spectrometer by
comparing with spectral libraries. Four iron ores supplied from National Institute of Standard
Techniques (NIST, USA) and six iron ore samples were analyzed and identified very well and
chemical speciation of iron was also successful. This method will be useful for the identification
of contaminants in soil and sediments.

Croft and Pye (13) examined the potential of stable isotopes in forensic soil analysis. Carbon and
nitrogen isotopes in soil samples were analyzed and as the result of experiments, discrimination
of soil types was successful and close agreement was found between “source soil” and “one-
stage transferred soil to footwear”. Potential of continuous flow isotope ratio mass spectrometry
was also promoted by Fourel et al (14).
Sandorani et al. (15) has developed microwave digestion technique to measure heavy metals in
sediments and soils. Acid mixture of HNO3, HF and distilled H2O was used and condition of
digestion was determined. The digests were analyzed by inductively coupled plasma – optical
emission spectrometry (ICP-OES). The results obtained showed good agreement to those of
obtained by previous methods.

Sutherland et al. (16) and Sutherland (17) have studied metal extraction from soil and road
sediments using different strength reagents. Solubility of elements to different strength acids was
determined. Stronger digestion resulted higher concentration of elements and for the screening of
degree of pollution extraction with0.5M HCl was considered most suitable. As the results, this
method will be applicable for the forensic differentiation the property of soil by chemical
extraction.

Terashima et al. (18) reported a new geochemical reference material for soil analysis. The
suggested values and the results of evaluation values by several organizations were described

Microscopy and Particle Analysis

Microscopy is still the most important technique for forensic geological examination, even many
sophisticated analytical equipments are introduced.

The mounting method for small particles was described in detail by Teetsov (19). The technique
is considered applicable to various kinds of particles. It also provided a lot of information in
regard with the preparation of tools and equipments.

Gunter and Twamley (20) has developed a new method to determine orientation of biaxial
minerals using spindle polarized microscope. Bandli and Gunter (21) and Brown and Gunter (22)
applied the method to determination of morphological and optical characterization of asbestos
and amphiboles from Libby, Montana, USA.

127
Petraco and Kubic (23) shared large volume of pages to minerals and matters included in soil
with clear and beautiful photographs by the microscopic observation of soils. The atlas shown in
this paper provides very useful information to those who are not familiar to microscopy and
gives a lot of suggestion to microscopists for the methods of description of the observed
materials under microscopes.

Blott et al. (24) has applied laser diffraction method to particle size analysis of forensic soil
discrimination. This technique was considered suitable for particles in size from 0.04µm to
2000µm and was applicable to samples with quite small amount.

Trace of Biological Substances and Organic matters

There are various properties in organic matters of soil. They are as important as inorganic
components but are not utilized very much in forensic examinations because of the chemical
complexity and seasonal change of biological communities.

Pollen analysis is one of the most applied botanical methods for the forensic investigations.
Wiltshire explained the importance of palynological approach even to determine the season of
the event (25).

Plant phytolith is often found in soil and sometimes plays important role in forensic
examinations. To provide much attentions for this purpose are derived from grass leaves, which
have been well studied. Kondo et al. (26) and Kondo et al. (27) studied phytolith of Pinaceae
leaves to differentiate three genera, but as there were little research has been accomplished.
Series of studies by Ogura (28-31) have described morphology of microscopic charcoal, the
original vegetation and the morphological change due to the different burning temperature. A
study of the relationship between pollen and microscopic charcoal from a certain area was also
carried out (32).

Micro algae in soil were also studied in the period by Sugita et al (33). Classification according
to morphological features of these materials for forensic examination was proposed. It was
applied to cultured algae from soil samples, and the original soils could be discriminated by the
classification method. Krstic et al. (34) have studied diatoms related to drowning cases.

DNA technique was applied to soil samples by Horsewell et al. (35). DNA profiling of a
microbial community in soil samples recovered from a sole of a shoe, collected from a shoe print
and reference sites was analyzed and showed good discrimination potential.
Application of Microbial Community Profiling and Characterization (MCPC) was introduced by
van Haeringen (36). The technique will be able to handle many soil samples and comparison is
possible.

The acid fraction of humus extracted from soil samples was examined by UV-Vis
spectrophotometry (37). Samples from five different areas were discriminated by 85% correct
classification. Gerin et al. (38) has analyzed surface of soil material by X-ray photoelectron
spectroscopy (XPS). There were concentration of carbon up to 1000 times more than bulk
concentration and some significant difference was found in Andosol from other types of soils.
This approach may be applicable to determine the type of soil evidence with small amount.

Branches of Eucalyptus camaldulensis grown at the same site from seeds of different origin were
analyzed by pyrolysis-gas chromatography (Py-GC) (39). Discrimination among the samples
was successful using syringyl propane unit and guaiacyl propane unit when principal component
analysis (PCA) to the results of Py-GC was applied.

128
Several experiments were conducted to characterize organic components in soil from graves.
Characteristics of microbial activities in soil from experimental graves were examined (40). Pigs
were buried and total C, biomass C, Total N, amino acid, NH4+, and NO3- were analyzed after
430days of burial. Quantitative analysis of trace level of adipocere in grave soils by GC-MS
method was successfully detected. Tuller (41) indicated the possibility of detection of human
blood proteins and volatile fatty acids from soil of murder site after the body was removed.
Forbes et al. (42) examined to detect adipocere from grave soils collected from exhumation
conducted in cemeteries using gaschromatograpy-mass spectrometry. Trimethylsilyl ester
derivatives of fatty acids (fatty acid TMS) were prepared using
bis(trimethylsilyl)trifluoroacetamide (BSTFA) and the result of analysis was better than fatty
acid methyl esters (FAME) because fatty acid TMS was easier to prepare and loss of intensities
was smaller than FAME.

Database, Geochemical Maps, and Urban Soil

A practice by Russian railway police is undergoing using a database “SOIL-RAILWAY” (43) to

search a point of illegal penetration of thieves onto a freight train. The system includes
information of elements, magnetic properties, mineralogical compositions, and some others of
samples collected from the path of railways.

Geochemical maps have been used by geologists for ore exploration. Importance of the use of
such maps were recognized to maintain environment and the project of creating global scale
geochemical maps has started in 1988 (44, 45). Manuals of sampling and analysis were
established (46).
The use of such maps in forensic examination is discussed by Rawlins (47) and Saye (48).

As global and national scale mapping is mainly focusing elemental analyses, McGrath et al. (49)
examined soil organic carbon (SOC) in samples collected under permanent pasture with the
depth of 0-10cm. SOC was determined by Walkley-Black method. As the result, SOC in Ireland
show broad regional pattern in which generally consistent with the spatial distribution of
precipitation materials and geographic elevation in the country.

There are also many researches of distribution of substances in urban soil and sediments. The
results of these studies are indicating the correlation of land use and concentration of certain
substances.

Romic and Romic (50) have examined heavy metal distribution in agricultural topsoil in the
region of Zagreb, Croatia, which had been rapidly urbanized recently. Li et al. (51) has reported
the result of heavy metal (Cd, Cu, Pb, and Zn) analysis in urban parks soils, street soils and soils
from country parks in Hong Kong using ICP-OES. Bityukova et al. (52) has studied on elemental
distribution of Tallinn, Estonia and resulted that major elements concentration was consistent
with underlying rocks but the concentration of some trace elements was significantly over the
average in urban soils. Tijhuis et al. (53) has surveyed geochemistry of topsoil in the city of
Oslo, Norway and human activities were reflected to elemental composition of topsoil. Road
sediments and park soil samples were analyzed using the energy dispersive X-ray fluorometory
(EDXRF). As the result, samples near an ironworks contained Mg, Ca, Cr, V, Ti, Ni, Mn and Fe
by Adachi and Tainosho (54) in Kobe, Japan. As the result of this survey, concentration of heavy
metal elements was in good correlation with human activities.

Mielke et al. (55) has compared chemical composition of soils and sediments three sites in New
Orleans. They analyzed polycyclic aromatic hydrocarbons (PAH) and metals. As the result, PAH
and metal concentrations were associated in city soil but not clear in sediments and alluvium.

129
Platinum group metals (PGM) have been used in autocatalyst and deposition of PGM was
analyzed in many cities. High concentration was detected from road sediments and concentration
decreased as the distance was greater from roads (56-63).

A study aimed its goal as establishing material scientific databases for supporting crime
investigation is carried on (64, 65). As the basic study to accomplish its aim, analytical
techniques and parameters to characterize soil samples were examined. To characterize urban
soils and sediments from Tokyo and surrounding areas from the viewpoint of forensic science,
gravity analysis, magnetometer, microscopic observation, multiple analytical techniques were
applied, that is XRD, scanning electron microscopy with energy dispersive X-ray fluorometory
(SEM-EDX) and SR-XRF.

Case reports

Brown (66) reported a case which combination of soil and pollen analysis revealed grave site of
a murder. Soil analysis including colors, textures, minerals and inclusions as well as pollen were
carried out to soil samples collected from a car related to the crime. Result of soil analysis
provided information of area connected to the crime, and pollen spectra helped to narrowing the
area. As the result, grave site was found with a good matching of both soil and pollen
information. Horrock and Walsh (67) reported the result of examination of clippings of grass and
soil recovered from suspects shoes and jeans in a sexual assault case. It was proved that there
was a good correlation of pollen between retrieved from the scene of the crime and recovered
one.

Hopen (68) reviewed three effective cases of soil examination in crime scene investigation.
Eijkel (69) reported case of murder, in which analysis of communities of diatom was effective.
Comparison of diatom communities among samples from the burial site, suspect’s car and cloths,
and shovels were carried out. As the result, the burial site had quite characteristic community and
some of the samples from suspect’s car matched to it.

Successful and unsuccessful cases utilizing Computational Fluid Dynamics were introduced by
Hardisty (70). The system was used in murder cases to estimate the sites of dumping bodies into
rivers from the places and the time they were found.

Field Surveys

Buck et al. (71) reported ground penetrating radar, magnetometry, and electrical resistivity were
tested for forensic searching of graves. As the result, ground penetrating radar and electron
resistivity could detect some burials including graves. The author concluded that farther
experiments are required but the possibility of narrowing site has been proved. Davis et al. (72)
reported GPR was applied to search for graves of victims killed by Spanish flu in 1918. It could
detect burial sites of seven wooden coffins in the layer of disturbed soil on frozen soil. Several
applications of geophysical techniques for searching graves were also reported by Cheetham
(73), Donnelly and Fenning (74) and Scott (75).

Bisbing (76) had stated the importance of field survey on forensic soil analysis. The importance
of stratigraphic techniques was stated by Hanson (77) from his experience of excavating mass
murder sites. The technique will serve to reconstruct the behavior of the criminal at the
clandestine graves by searching trace of tools, steps and so on.

130
Miscellaneous

Hot spring water related to a crime was required to examine its origin(78, 79). Reference water
collected from 30 wells was analyzed using ion chromatography (IC) and atomic absorption
spectrometry (AAS). Cl- and SO4- varied in wide range when plotted on Cl-SO4-F triangle
diagram.

Acknowledgment

The authors would like to deeply appreciate kindly providing useful information from Dr.
Robertson, Dr. Croft, Dr. Wolf, Dr. Brocard, and Dr. Cordiner.

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135
INDIVIDUAL IDENTIFICATION
EVIDENCE

136
Recent progress in Forensic DNA
profiling

— A Review: 2001 to 2004 —

Dr. Peter Gill

Forensic Science Service

United Kingdom

137
INTRODUCTION:

This review focuses upon the major advances in DNA profiling technology during the last three
years. It is subdivided into several main sections: mixture interpretation using expert systems;
mitochondrial DNA; low copy number STR DNA profiling and its relationship to contamination;
population genetics and the relationship to correction factors of match probabilities; Y-
chromosome markers; autosomal SNPs and other new DNA methods. For a general review on
the forensic application of STRs in relation to national DNA databases see the review by Gill [1].

Mixture interpretation using expert systems

The original method of DNA mixture interpretation was proposed by Evett et al. [2]. Several
years ago, a theory to interpret mixed DNA profiles that included a consideration of peak area
using the method of least squares was proposed by Gill et al.[3]. This method of mixture
interpretation was not widely adopted because of the complexity of the associated calculations.
Currently, most reporting officers take account of peak area in an intuitive way based upon their
experience and judgement based approach to interpretation.

A formalised approach has been written into a computer program package called PENDULUM
[4]. This program uses a least squares method to estimate the pre-amplification mixture
proportion for two potential contributors. It then calculates the heterozygous balance for all of
the potential sets of genotypes. A list of “possible” genotypes is generated using a set of heuristic
rules. External to the program the candidate genotypes may then be used to formulate likelihood
ratios that are based on alternative casework propositions. The system does not represent a black
box approach; rather it has been integrated into the method currently used by the reporting
officers at the Forensic Science Service (FSS). The time saved in automating routine calculations
associated with mixtures analysis is significant. In addition, the computer program assists in
unifying reporting processes, thereby improving the consistency of reporting. Parallel
developments have also been undertaken by Perlin and Szabady [5] who also used the
minimisation of the sum of squared deviations across loci in their Linear Mathematics
Algorithm. This approach used an elegant mathematical procedure to search for possible
genotypes, and in addition it removed stutter before proceeding.

Mitochondrial DNA

The main uses of mtDNA testing are to analyse hair shafts and degraded remains. The control
region of human mtDNA, is the region most commonly analysed. The EDNAP group [6]
recently carried out a collaborative exercise in order to evaluate the distribution of mitochondrial
DNA (mtDNA) heteroplasmy amongst the hairs of an individual originally shown by Linch et al.
[7]. It has been demonstrated that mtDNA mutates at a substantially higher rate than autosomal
DNA e.g. Parsons et al. [8]. Consequently it is not unusual for differences to be observed
between different hairs and/or tissues within an individual. In the EDNAP study it was also
demonstrated that heteroplasmy was not just observed between hair shafts, but also along the
length of a single hair shaft. Linch et al. [7] highlighted that a significant proportion of the
mitochondria in hair shaft were likely to have originated from a relatively small number of
melanocytes, the remainder originating from keratinocytes. Melanocytes continue to produce
mitochondria until later in life when grey hairs are produced and then keratinocytes take over
production. This provides a mechanism that may explain a shift in heteroplasmic ratios within
and between individual hair shafts. Nevertheless, despite high levels of heteroplasmy observed in
the study, it was demonstrated by Tully et al. [6] that the maximum number of differences
between any single hair and the reference sample was one. Heteroplasmy has been found at
multiple positions within a single individual in previous studies [9-12]. In particular, Grzybowski

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[12] claimed to have found excessive heteroplasmic events in mtDNA – up to six positions in the
HVI region. These results have been challenged by Tully and Lareu [13] and Budowle et al. [14]
mainly on the basis of potential contamination or the amplification of nuclear pseudogenes. In
addition, Brandstatter and Parson [15] demonstrated that misinterpretation of data can arise from
the utilisation of nested PCR that gives substantially higher background noise compared to direct
PCR. With regard to taking account of mtDNA contamination, the EDNAP group [6] has
recommended that “in the event of duplication failing or where insufficient sample is present, the
report should clearly state the limitations of an unconfirmed result”.

To report mtDNA results, the aim of a mtDNA analysis is to provide evidence to support one or
two alternative propositions:

1) The contention that the evidential sample (Q) originated from the suspect (the donor of
K) or a maternally linked relative;

or

2) The contention that the evidential sample (Q) originates from the suspect’s sample (K)
originate from different individuals (of different maternal lineage).

The sequence is reported as a haplotype. Currently most laboratories use the counting method to
estimate evidential strength. This means that the result is compared to a database size (n) where
the number of matching sequences is reported.

If two samples (K and Q) do not match then this does not necessarily mean that they do not have
the same origin. There are ‘hotspots’ within the mtDNA genome where mutations are more
common. For example a difference at position 73 which is relatively stable provides stronger
evidence of exclusion than position 16,093, which is an apparent mutation hotspot where
heteroplasmy has been commonly observed [11]. However, this is difficult to quantify in
evidential statements. Tully et al. [16] suggest a likelihood ratio formulation to assess the
evidence for apparent simple mismatches. However, more data on mutation and demography are
needed before full LR approaches can be employed.

There are a number of data collections are available on the internet. For example: EDNAP
mtDNA Population Database (EMPOP) [17] www.EMPOP.org , and www.mitomap.org . The
biggest problem with database collections is ensuring their integrity. The EDNAP study
discovered submissions from laboratories contained a number of errors ranging from clerical,
interpretation and sample transpositions. It has been shown in an excellent study [18] that many
errors in databases that can be highlighted by phylogenetic analysis of closely related mtDNA
within the framework of an established world-wide phylogeny that is supported by coding
region. A series of general rules can be followed to detect potential errors. In particular, Bandelt
et al. [18] recommends that checks are made to determine whether a haplogroup motif is fully
represented in a sequence. For example, if numerous distinct transversions and indels appear in a
sample that is not represented in a database then this may indicate misreading of the sequence.
Sometimes new sequence variants are confirmed, however. Once highlighted, the sample may be
reinvestigated. The implementation of suggested guidelines is expected to reduce error rates by
at least an order of magnitude.

Low copy number STR DNA profiling and the relationship with contamination

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The definition of low copy number analysis is analysis of less than c.100pg DNA [19]. At low
levels, stochastic effects result in unequal amplification of allelic products. Consequently, alleles
at a heterozygous locus appear to be unbalanced. At the extreme, this leads to the phenomenon
known as allele drop-out where one allele at a heterozygous locus is missing altogether. The
interpretation of DNA profiles, especially mixtures, is dependent upon a full understanding of
the characteristics of the way heterozygous balance is related to the quantity of DNA template
available [20]. In addition, we can generalise that PCRs that have lower levels of DNA template
are more prone to contamination events. To minimise the impact, the LCN protocol requires
duplicate PCR of an extract – only those alleles that are duplicated are reported. A complex
statistical theory underpins LCN and is preferable to use. The method has been programmed into
a computer program called ‘LoComatioN’ [21]

This method factors in probabilities of allele drop-out p(D) and contamination p(C) into the
calculation of the LR. These parameters are calculated from experimental observations where
p(D) depends upon the size of the surviving heterozygotic allele, and p(C) can be estimated from
collation of negative control results. It is important to note that just because a reference profile
does not match the crime stain this does not result in exclusion, rather the probability of the
evidence is lowered as a result.

Increasing the number of PCR amplification cycles to 34 is sufficient to raise the sensitivity of
the test sufficiently to detect the PCR products of a single cell. In practice it is very unlikely that
a single cell would be successfully analysed from crime stain material– rather, it more likely that
several cells containing fragmented DNA would form the smaller samples analysed. The
increased prevalence of contamination at low level has to be addressed by duplicate analysis of
the result and also by careful conditioning.

Experience with LCN has implications for standard DNA analysis – companies that manufacture
STR multiplexes validate their multiplex systems down to c.250pg (the equivalent of c.50 cells).
However, it can be argued that conventional DNA profiling using 28 cycles is itself low copy
number testing when low levels of target DNA are analysed. Remembering that the key features
that distinguish LCN from conventional DNA profiling are the prevalence of contamination and
drop-out – it has been demonstrated that both of these features also exist with conventional 28
cycle DNA profiling as well. Recently, extensive investigations have demonstrated that a small
proportion of plastic tubes have been contaminated at the manufacturing source. Consequently,
DNA profiles that were originally attributed to case-work material were wrongly attributed and
the crimes were undetected as a result.

In order to minimise the impact of contamination, whilst recognising that it was impossible to
prevent it completely, over a number of years, the following measures were introduced by the
Forensic Science Service [22, 23]:

1) At crime scenes, investigating officers wear protective clothing and face masks. A study
of the effectiveness has been made by Rutty et al. [24]

2) Processing of samples is separated into extraction areas and amplification areas

3) Positive pressure laboratory conditions are used in laboratories, entry is restricted only to
personnel working in the unit

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 4) In the UK, a Police Elimination Database (PED) has been implemented. So far there are
c.65,000 contributors to this database. Samples from the crime scene are checked against
the database – but only against those officers who were investigating a given crime scene

5) A staff elimination database comprising staff working in the DNA unit has been
implemented. All samples are checked against the database. This database is extended to
visitors, maintenance staff etc.

6) Any ‘unexplained’ profiles – e.g. profiles appearing in negative controls or quality

control checks also go onto a searchable database.

7) As part of automation, which uses micro-titre plate format, software is used to highlight
potential ‘splash-over’ events where aerosol from one well may occasionally affect
adjacent wells - identified by profiles that contain matching alleles (albeit in admixture).

Nevertheless, no matter how many precautions are employed there is still a certain amount of
background contamination that is inevitable. Low level contamination tends to be sporadic (i.e.
tube specific) and partial. The logical consequence of this is that a negative control does not give
confidence that the associated batch of extractions is contaminant free [23]. The only exception
to this is when the contaminant is observed both in the negative control and in an associated
extraction tube(s), in which case the contamination is considered gross i.e. multiple events that
are possibly reagent based. Gill and Kirkham [22] suggest that negative controls cannot be used
to assign confidence that an associated extraction batch is contamination free. However, because
negatives controls are effectively a microcosm of casework samples (albeit supposedly DNA-
free) then by careful monitoring, they can be useful to measure the amount of contamination that
is pervasive in the process. Thompson et al. [25] suggest that any error rate must reduce the
likelihood ratio reported in a case. However, contamination rates do not equate to error rates.
Each case is effectively associated with a probability of error [22] that is dependent upon
multiple factors such as the quantity of DNA analysed; whether there are multiple stains; the
kind of stain analysed. To build an analysis based on multiple variables requires a different
approach. This can be accomplished by the use of probabilistic frameworks which are used to
simplify the data analysis, otherwise known as ‘Bayes nets’; see for example [26] for an
explanation and [27] for a practical illustration of its use in a forensic case that incorporated
multiple probabilistic variables.

Lowe et al [28, 29] showed that there is a difference between individuals in their tendency to
deposit DNA on an item when it is touched. A good DNA-shedder may leave behind a full DNA
profile immediately after hand washing, whereas poor DNA-shedders may only do so after their
hands have not been washed for c. 6h. Secondary transfer was also demonstrated – this is where
a good shedder’s-DNA (individual A) was transferred onto the hands of a poor shedder
(individual B), by hand-holding for 1 minute, and thence onto an object held by individual B i.e.
transfer follows sequentially: A⇒B⇒object. On analysis, DNA from individual A could be
demonstrated, but usually always in admixture with individual B. The persistence of A’s DNA
was short-lived on B’s hand such that periods of time >1hour after initial contact with B were
sufficient to greatly reduce the propensity of secondary transfer. In reality, secondary transfer is
unlikely to be realistic unless the contact of A with B has been immediately before the crime-
event itself, although [30] recently claimed the persistence of DNA for at least 10 days after
initial contact after simulated strangulation of a living ‘victim’. Alessandrini et al. [31]
compared recovery of fingerprint DNA from glass, wood, metal demonstrating that the “shedder
status” ie the ability of the donor to shed DNA was the most important contributing factor to
success rates. New extraction methods have been developed to remove DNA from latent
fingerprints on ordinary paper after chemical enhancement [32]. Elliott et al. [33] have adapted a

141
method known as laser micro-dissection (LMD) to analyse small numbers of cells by physically
picking them from a microscope slide. With old cases, the original microscope-slides used to
examine the presence of semen may often be the only evidence remaining in a case. The method
has proven to be a particularly useful way to separate sperm from vaginal cells, and was
demonstrably more efficient than the traditional method using preferential lysis. Interestingly,
there was a significant association between the quality of the male profile recovered and the time
since intercourse that was independent of the number of sperm analysed – suggesting that the
DNA was rapidly degrading in vivo. In addition, sperm were demonstrated to adsorb female
DNA, rather like an affinity matrix, hence male/female mixtures were often observed. Again this
was an in vivo reaction that was dependent upon time since intercourse.

To summarise, low copy number is synonymous with contamination because DNA is all
pervasive in the environment (in house dust for example). Evidence types most commonly
associated with LCN typing include finger-marks. The discovery that plasticware may be
contaminated at manufacturing source has led to a much greater awareness of the issues that
surround the management of contamination in relation to the interpretation of DNA profiling
evidence of all kinds.

Population genetics and the relationship to correction factors

When giving evidence in court, there is an onus on the forensic scientist to ensure that it is
presented in a manner that does not unduly favour the prosecution. Consequently, any statistical
analysis tends to err on the side of caution to favour the defence, rather than the prosecution
scenario. The practice of conservative reporting is universal, but the question is how
conservative should the assessment be in order to avoid undue bias towards the defence
scenario? After all, the wrongful exoneration of a guilty individual because of over-cautious
scientific evidence is also highly undesirable.

There has been much debate in the past about the use of match probabilities in relation to
reporting evidence. In particular, the use of the product rule was originally challenged many
years ago by Lander [34]. The argument followed that because populations are sub-structured,
then it does not follow that independence between alleles and loci could be assumed, hence the
product rule was invalid. The second, albeit related, question pertained to whether cosmopolitan
frequency databases used by forensic laboratories were representative of all possible sub-
populations that it comprises. Consequently Hardy-Weinberg equilibrium could not be assumed
and much debate revolved around the divergence of populations.

Subsequently a large number of studies have now been undertaken to estimate the levels of sub-
structuring in populations, estimated by θ, the inbreeding or co-ancestry coefficient. Balding and
Nichols [35, 36] proposed formulae that could be applied to correct genotype frequency
calculations for any given value of θ - these were adopted by recommendation 4.1 of the NRC II
report [37]. In addition corrections can be used to adjust sample bias, such as 95% confidence
interval.

Recently, Curran et al. [38] studied the magnitude of the subpopulation effect in relation to the
Balding and Nichols θ correction factor. In their review of θ values, almost all are less than 0.02
in Caucasian populations. Other studies support considerably lower values in Caucasian
European and North American populations. In accordance with NRC recommendations [37],
many laboratories use 0.01 for cosmopolitan (Caucasians) and an elevated 0.03 value for
populations that may exhibit increased inbreeding, such as immigrant communities from the
Indian sub-continent. Curran et al. [38] show by simulation, that application of the Balding and
Nichols θ correction acts in a very conservative way – i.e. it works strongly in the favour of the

142
defence, whereas the unbiased product rule estimator has a small bias in favour of the
prosecution that may be more than a factor of 10.

Gill et al. [39] compared 24 different European Caucasian populations collected by the European
Network of Forensic Institutes (ENFSI) group of laboratories. They found that all θ values were
less than 0.006. European laboratories use a variety of different methods to correct genotype
frequencies including a size bias correction [40]; θ adjustment [35, 36]; a minimum allele
proportion between 0.01 and 0.02, an upper bound of a 95% confidence interval [37]; and a
lower bound on the genotype match probability of 1 in 1 billion. Many laboratories use a
combinatorial approach, for example the FSS uses a size bias correction, a θ adjustment and a
lower bound on the genotype probability of 1 in 1 billion. The approach taken by Gill et al. [39]
was to test the effect of different correction factors against simulated populations. Essentially, all
adjustment factors used are arbitrary; however their effectiveness can be tested against simulated
populations. It was demonstrated that sample bias effects were exacerbated mainly by rare
alleles. Consequently, the application of a minimum allele proportion was sufficient to negate
this effect. The ENFSI STR databases can be accessed on www.str-base.org/index2.php . The
user can apply a variety of adjustment methods, discussed above, to calculate genotype match
probabilities.

Y-chromosome markers

Y-chromosome markers are useful to resolve cases that comprise mixtures where the major
component is female and present in excessive amounts, rendering mixture analysis impossible.
An elucidation of ethnicity is also possible. Recommendations on the forensic analysis of Y-
chromosome are published by Gill et al. [41]. This report considered nomenclature, use of allelic
ladders, population genetics and reporting methods. The counting method is usually used to
express the strength of evidence as described for mtDNA. Y-STR haplotype databases are
available online – for US populations (www.ystr.org/usa) and for European populations
(www.ystr.charite.de ). A number of commercially available Y-chromosome STR multiplexes
are now available. For example the kits from Reliagene Technologies [42, 43] allows
simultaneous amplification of 11 Y-chromosome loci that incorporate the 9 loci recommended
for the minimal haplotype identified by the International Y-STR user group [44]. In addition,
SNP based methods are being developed [45, 46]. These loci are highly non-randomly
distributed among populations and may contribute significantly to determining population of
origin prediction analysis. Eighteen major haplogroups are recognised by the Y chromosome
consortium [47]. Vallone and Butler [48] constructed multiplexes to examine 50 Y-SNP
markers. A total of 42 markers were assayed with a commercial available system - Signet™ Y-
SNP identification system (Marligen Biosciences, Inc, Ijamsville, MD) – using the Luminex®
100 flow cytometer

Autosomal SNPs and other new DNA methods

Recently there has been a lot of interest expressed in autosomal SNPs. Under the auspices of
ENFSI and SWGDAM, Gill et al [49] recently addressed the issue of whether SNPs would
replace STRs in national DNA databases. The consensus view is that this is unlikely to occur in
the short to medium term. The advantages of SNPs are potential rapid throughput, but
disadvantages include the difficulty of building large multiplexes required to give a
discriminating power equivalent to STRs [50]. In addition, the interpretation of mixtures is
problematical and much more difficult than for STRs. Consequently, to date, a fully validated
protocol for the analysis of crime-stains using SNPs has not been appeared. Of crucial interest is
the consideration of whether SNPs will out-perform STRs in terms of success rates. To discover
this, the ENFSI group has recently started a collaborative exercise to answer this question. In

143
particular, it is intended to test whether SNPs are useful to analyse highly degraded DNA where
template fragments sizes are significantly less than those that can be detected by conventional
DNA analysis. However, alternative strategies exist. For example, Butler et al. [51] described a
newly designed STR system where the amplicon sizes have been significantly reduced by
moving the primers closer to the repeat region. Improved signals from degraded DNA samples
were demonstrated. The utilisation of Y-SNPs and mtDNA SNPs has already been discussed but
these do not impinge upon the current debate relating to autosomal SNPs. In a separate
application, Frudakis et al. [52] screened 211 autosomal SNPs and demonstrated that a subset of
56 were dramatically different between 3 major race groups and could be used to classify
individuals accordingly. This system could be used as an adjunct to Y-chromosome and
mitochondrial markers.

In conjunction with development of new biochemistry there is considerable research into the
concept of a ‘lab-on-a-chip’. Such technology may offer the twin advantages of portability and
low cost. To date, a validated solution for forensic analysis has not emerged. However,
promising new areas of development include microfabricated capillary array electrophoresis for
the rapid analysis of STRs [53, 54]; Paegel et al. [55] have made an integrated platform that
extracts, PCRs and sequences in a single device. For further detailed information, the whole area
of microfabrication is extensively reviewed by Heller [56].

Finally, it is easy to forget that one of the most pervasive problems facing the forensic biologist
is the identification of body fluids. Jussola and Ballantyne [57] describe a promising new method
to identify blood, semen and saliva stains using mRNA analysis, having established that RNA is
surprisingly stable in body fluid stains. RNA is present in high copy number – consequently the
advantages of RNA based body-fluid markers are their specificity, stability and sensitivity.

Summary

There has been significant progress during the past 3 years in the field of forensic DNA typing.
The interpretation of STR profiles can be automated using expert systems, furthermore,
interpretation of complex mixtures and low copy number has been enhanced. The development
of Y-chromosome technology has led to the introduction of new commercial kits. Promising
advances have been made in the area of SNP-typing and associated lab-on-a-chip technologies,
although clearly this has not yet ‘come of age’ in forensic terms.

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 Biological Evidence – Hair

— A Review: 2001 to 2004 —

James Robertson BSc PhD

National Manager
Forensic and Technical
Australian Federal Police

This review is dedicated to the memory of the late Barry Gaudette. Barry stimulated a
renewed interest in the examination of hairs with his work in the late 1970’s and into the
1980’s in which he considered a statistical model for assessing the value of hair
examinations. His scientific papers remain the key works which still fuel debate on this
critical issue. Barry sadly passed away in 2003 from cancer. He is fondly remembered by
his many friends and colleagues.

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INTRODUCTION:

Interest in the forensic examination of hairs during the last three year reporting period has been
quite high although this has not yet been reflected in the number of published papers.

Hair examination continues to come under the Daubert microscope (Taupin, 2004). For
example, in the USA, hair evidence which is said to have contributed to the conviction of Jimmy
Ray Bromgard for the 1987 rape of an 8 year old girl, has been challenged following DNA
testing which proved Bromgard was not the offender. The hair examiner told the jury in the
original trial that there was a 1 in 10,000 chance that hairs found at the crime scene came from
someone other than Bromgard. His ‘probability theory’ was derived from his conclusion that
there was a 1 in 100 chance in each instance that head hairs and pubic hairs from a crime scene
could match head and pubic hairs from someone who was not the perpetrator. Hence, the
probability of a double match by chance would be 1 in 100 multiplied by 1 in 100, or 1 in
10,000! A panel of forensic experts who reviewed this work found that there was no scientific
basis for this reasoning.

The need to place hair examination on a sound foundation is certainly at the forefront of thinking
in some key groups.

West Virginia University (WVU) and the National Forensic Science Technology Centre
(NFSTC), members of the National Institute of Justice’s Forensic Resource Network, have been
developing resources for forensic hair examiners.

These resources include multi-day workshops, reference materials, and guidelines for the
examination of human and animal hairs. A panel of experts from the US and Australia has been
convened to advise the project. Workshops have been held at WVU, NFSTC, and at various
regional professional forensic science conferences in the US. For example, to date, over 50
forensic DNA analysts have attended a workshop on the evaluation and assessment of hair roots
for nuclear and mitochondrial DNA analysis. Electronic reference materials are being prepared
that will assist forensic scientists in their self-study and review of human and animal hair
characteristics. (For more information, please contact either Max M. Houck at WVU,
max.houck@mail.wvu.edu, or David Epstein at NFSTC, dme@nfstc.org.)

As a member of the above ‘panel of experts’, and having run a number of introductory hair
workshops, I would endorse the need for a standardised approach to hair examination,
underpinned by reference materials and training, which the above program is aimed at providing.

A personal observation is that it is surprising how many scientists, who are making decisions
regarding the selection of hairs from nuclear DNA (nuDNA) testing, are not able to confidently
differentiate hair roots in the anagen (growing) and telogen (resting) growth phases.

There also appears to be considerable confusion regarding which hairs are suitable for nuclear
DNA testing; ‘suitable’ being defined as ‘likely to yield a nuDNA result’. The most useful
publication, with excellent images, which details root types suitable for nuDNA typing remains
Linch et al., (1998). These authors have also published work on post-mortem microscopic
changes observed at the human head hair proximal end (Linch and Prahlow, 2001) and a review
of human hair histogenesis for mitochondrial mtDNA (Linch et al., 2001).

Other publications that assist in meeting the tenets of the Daubert decision include a hair
bibliography for the forensic scientist (Houck, 2002) and a review on the microscopy of hair by

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Deedrick and Koch from the FBI laboratory (2004). The latter is essentially an update of the
early publication by Hicks, “Microscopy of Hair: A Practical Guide and Manual,” from 1977.

Finally, Taupin (2004) has recently discussed the past, current and future role of forensic human
hair analysis and comparison in the context of its admissibility and reliability as evidence. She
discusses a number of cases in which hair evidence has been challenged and found wanting.
Taupin concludes that “rogue scientists and poor quality control should not be allowed to
discredit an entire discipline that still has the ability to provide valuable evidence in criminal
cases!”

DNA and hairs

DNA analysis continues to play a valuable role in hair examination. Notwithstanding the earlier
observation on the ability of forensic biologists to accurately select hairs suitable for nuDNA
testing, it can be reasonably said that, for anagen hairs, there is a strong possibility of obtaining a
nuDNA profile using any of the commercially available DNA analysis systems such as Profiler
Plus.

However, the reality is that in the order of 95% of hairs recovered in a forensic context will be
telogen hairs for which there is a very low, to nil, rate of success for nuDNA testing with
traditional approaches.

There have been relatively few reports of successful STR (short tandem repeat) genotypes from
telogen hairs. They generally have required modification of standard PCR processes like
extended PCR cycles (Barbaro et al., 2000) or primers designed to isolate very short amplicons
(Hellmann et al., 2001; Grubwieser et al., 2003; Butler et al., 2003).

As yet unpublished work by my group (McNevin, 2004) has looked at this problem from another
direction. Our work looks more closely at the processes of cleaning and subsequent extraction of
DNA from hair on the basis that no amount of subsequent clean up or fine tuning or extra PCR
cycles will deliver a DNA profile if undegraded genomic DNA is not initially present in the
extract. The location of DNA in the hair shaft becomes significant if cleaning and extraction are
to be balanced. The conclusions from a series of studies challenge conventional wisdom in that
we believe that the nuDNA which is being detected is located in, or on, the cuticle of the hair.
Hence, we do not recommend extensive pre-cleaning to remove exogenous materials. Our
protocol calls for extended PCR cycles (34) but we did not find any significant improvement in
reportable DNA profiles through the use of specifically designed primers aimed at producing
shorter amplicons. It is our belief that the nuDNA detected on hairs is in, or on, the cuticle. We
have limited evidence that success is donor dependent and further studies are underway to
examine the factors which might influence donor dependence.

There are probably no circumstances where nuDNA testing of human telogen hairs will be a
routine or simple matter in the foreseeable future. However, the ‘prize’ of nuDNA testing for
such samples will warrant continued research.

In the absence of a routine nuDNA test for telogen hairs, mtDNA testing remains of considerable
interest to hair examiners around the world. It is beyond the scope of this review to look at the
broad literature relating to mtDNA.

Primarily, interest in the last three years for mtDNA in hairs has involved debate regarding the
level of heteroplasmy in hairs (Grzybowski, 2000; Budowle et al., 2002; Grzybowski et al.,
2003; Brandstatter and Parsa, 2003).

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Although mtDNA testing is a well established technique, it is not universally successful. In an
extensive survey, Prieto et al., (2003) reported on the results of the Spanish and Portuguese
working group of the International Society of Forensic Genetics Collaborative Exercise (2001-
2002) on mtDNA analysis. They found that only 3 out of 23 laboratories were able to obtain the
consensus sequence for mtDNA analysis of hair shaft samples and 10 laboratories did not obtain
or report any result.

Houck and Budowle (2002) reported on the correlation of microscopic and mtDNA hair
comparisons. Of 170 hair examinations conducted in the FBI laboratory between 1996 and
2000, there were 80 microscopic associations. Of these, only 9 were excluded by mtDNA.
However, mtDNA results were obtained from a further 66 hairs which were considered
unsuitable microscopic examinations or yielded inconclusive results. In contrast to the results of
the collaborative Spanish and Portuguese study (Prieto et al., 2003), in only a very small number
of cases did hairs not provide sufficient mtDNA for analysis or yield inconclusive results.

Houck and Budowle conclude that microscopic examination can still play an important role,
particularly in exclusions, and that mtDNA sequencing combined with microscopy is a very
powerful tool.

Finally, Takayangi et al., (2003) report on three methods for the extraction of mtDNA from
hairs. They conclude that NaI and a silica-bead method are effective for old or degraded hairs,
with the silica-bead method offering the advantages of simplicity and speed. Phenol chloroform
extraction performed well with fresh hairs but not with old hairs.

General and microscopy

Bisbing (2002) has updated his review of the forensic identification and association of human
hair in Saferstein’s ‘Forensic Science Handbook’ series.

Rees (2003) reviews the genetics of hair and skin colour. This excellent review provides an up
to date and comprehensive background to hair and skin colour with a detailed consideration of
the melanocortin 1 receptor (MCR1) which has been identified as explaining the variation in the
normal population which results in red hair. The reviewer argues that the lack of a standardized
phenotype assessment is a major limitation in advancing an understanding of genotype-
phenotype relationships.

A number of abstracts relating to hairs appear in the Forensic Science International issue
dedicated to the 3rd meeting of the European Academy of Forensic Sciences (Anon, 2003).

(1) Verma et al., report on the development of a prototype automated system for
forensic hair comparison and analysis using neural networks – see also Verma et
al., 2002).

(2) Bunyator and Yusiffi report on a study of differential thermic and thermo
gravimetric methods for the analysis of human hair.

(3) Vits et al., report on the development of a simple method to make cross sections
of hair using a cryo-microtome.

Sato (2002, 2003) reports on the quantitative classification of hair form and its application to the
forensic comparison of Japanese head hair. Using a scheme based on 8 basic characteristics

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which describe and classify hair profile, along with cluster analysis of the data, it was possible to
successfully discriminate between 8 individuals.

Rowe (2002) reports on an unusual medulla morphology in Caucasian head hairs. He describes
a medulla containing alternating light and dark regions, in some areas resembling the universal
ladder medullas seen in some animal hairs. This feature did not appear to be related to severe
cosmetic treatment or any diagnostic abnormalities associated with diseases of human hair.

Brooks et al., (2004) have described their work on digital imaging and image analysis in forensic
hair examination. One of the problems encountered in the microscopic examination of hairs is
‘in and out of focus’ imagery especially at high magnification. This means it is only possible to
focus on a very limited depth of field. In practice a mental image is formed by the examiner
focusing through several layers of the hair. This ‘virtual’ image is assessed for the
microscopically observed features with pigment features being the most important for
discrimination. It would be highly desirable to be able to describe pigment features numerically
to reduce or eliminate the visual and subjective assessment. This work describes the use of
syncroscopy automontage software which combines manually selected focal plans through the
hair and vertically stacks them to produce a final single, and in focus, image. This image can
then be analysed to obtain colour densities and pigment numbers and distributions. Although
still in its early stages, this approach shows great promise.

Dachs et al., (2003) report on the persistence of scalp hairs on clothing fabrics. The fibre
composition and surface roughness were key factors affecting persistence. The exponential
decay pattern generally associated with loss of trace evidence was seen with most fabrics.
However, the rate of loss from woollen garments was found to be linear, indicating a different
process is involved in the persistence of hairs on woollen garments from that on non woollen
garments.

Chemical and drugs

Vincent et al., (2002), report on the optimization and validation of an analytical procedure for
the determination of oxidative hair dyes.

Goodpaster et al., (2003), report on preliminary research using on-line supercritical fluid
extraction/gas chromatography – mass spectrometry (SFE/GC-MS) to examine the natural and
artificial surface components of human scalp hair. Results from this study, and other related
studies (Benner et al., 2003), have shown that it is possible to differentiate between hairs from
different individuals based on the analysis of lipids. It is possible to work with as little as 1 mg
of a hair strand using the on-line approach described. The authors have also assessed how their
approach can be seen as complementary to mtDNA analysis.

It is beyond the scope of this review to examine in detail the use of hair as a biological matrix for
drug analysis. There continues to be many papers published in this area, including a number of
recent review papers.

Kintz (2003) reviews testing for anabolic steroids and he also reviews the value of hair analysis
in post mortem toxicology (2004). In both areas he concludes that hair analysis may be a useful
adjunct to conventional drug testing whilst recognising that there remain concerns and
unanswered questions which still limit its broader acceptance. Of particular relevance to the
latter is the review by Ruth and Stout (2004) of mechanisms of drug deposition in hair and issues
for hair testing. They conclude that melanin and various interactions with the hair pigment
melanin, appear to dominate the scheme of interactions which influence deposition and retention

152
of drugs in hair. They argue that understanding these factors is central to distinguishing internal
deposition from external contamination and hence the interpretation of endogenous levels.

Conclusions and future directions

Hairs, and in particular human hairs, will remain an important trace material for the future if for
no other reason than it is a physical reality in routine case work. As humans lose 100 or more
hairs each day, hairs will always be present as potential evidence.

Microscopic examination will remain a core technique but debate will continue regarding its
value and reliability. Initiatives reported here such as the NIJ funded work being carried out in
the USA, and research aimed at capturing microscopic information in a more objective way,
have the potential to go some way to answering critics of hair examination.

DNA analysis will continue to be a very important adjunct to hair examination. It appears
unlikely that nuDNA testing will become a routine technique for shed (resting) hairs. More
work is required to gain a fuller understanding of nuDNA testing of resting hairs, in particular to
determine whether or not the DNA extracted is endogenous.

mtDNA testing will continue to play an important role but will still need to be carefully targeted
and prioritised in case situations due to cost factors and, more fundamentally, availability of
mtDNA testing (capacity). It is unlikely that this situation will greatly improve in the next three
years.

What should change through DNA testing, particularly mtDNA, is that, where this is available,
the hair examiner should change thinking from exclusion to avoid a wrong inclusion, to
acceptance of more hairs for testing using mtDNA as the ultimate exclusion/inclusion tool. This
will require an understanding by users that the apparent ‘fail rate’ for microscopic examination
should increase.

Research will no doubt continue on a range of novel approaches aimed at contributing to the
pool of available techniques capable of discriminating hairs in either a general sense or for
specific situations.

REFERENCES:

1 Anon. Proceedings of 3rd European Academy of Forensic Sciences. Forensic Science

International, 136 (Supplement 1), 2003.
2 Barbaro, A., Falcone, G., Barbaro, A. DNA Typing From Hair Shaft. Progress. Forensic
Genetics, 8, 523-525, 2000.
3 Benner, B.A., Goodpaster, J.V., DeGrasse, J.A., Tully, L.A., and Levin, B.C.
Characterization of Surface Organic Components of Human Hair by On-Line
Supercritical Fluid Extraction – Gas Chromatography/Mass Spectrometry: A Feasibility
Study and Comparison with Human Identification Using Mitochondrial DNA Sequences.
Journal of Forensic Sciences, 48, 554-563, 2003.
4 Bisbing, R.E. The Forensic Identification and Association of Human Hair, in, Forensic
Science Handbook, 2nd Ed., Ed., Saferstein, R. Pub. Prentice Hall, New York. Volume
1, 389-428, 2002.
5 Brandstätter, A., Parson, W. Mitochondrial DNA Heteroplasmy or Artefacts - A Matter
of the Amplification Strategy? International Journal of Legal Medicine, 117(3), 180-184,
2003.

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6 Brooks, E., McNaught, I., and Robertson, J. Digital Imaging and Image Analysis in
Forensic Hair Examination. Presented at the 17th Australian and New Zealand Forensic
Science Society (ANZFSS) International Symposium on the Forensic Sciences,
Wellington, New Zealand, 2004.
7 Budowle, B., Allard, M. W., Wilson, M. R. Critique of Interpretation of High Levels of
Heteroplasmy in the Human Mitochondrial DNA Hypervariable Region I From Hair.
Forensic Science International, 126(1), 30-33, 2002.
8 Butler, J. M., Shen, Y., McCord, B. R. The Development of Reduced Size STR
Amplicons as Tools for Analysis of Degraded DNA. Journal of Forensic Science, 48(5),
1054-1064, 2003.
9 Dacks, J., McNaught, I. J., and Robertson, J. The Persistence of Human Scalp Hair on
Clothing Fabrics. Forensic Science International, 138, 27-36, 2003.
10 Deedrick, D.W, and Koch, S.L. Microscopy of Hair Part 1: A Practical Guide and
Manual for Human Hairs. Forensic Science Communications, 6, 2004.
11 Goodpaster, J.V., Drumheller, B.C., and Benner, B.A. Evaluation of Extraction
Techniques for the Forensic Analysis of Human Scalp Hair Using Gas
Chromatography/Mass Spectrometry (GC-MS). Journal of Forensic Sciences, 48, 299-
306, 2003.
12 Grubwieser, P., Mühlmann, R., Parson, W. New Sensitive Amplification Primers for the
STR Locus D2S1338 for Degraded Casework DNA. International Journal of Legal
Medicine, 117(3), 185-188, 2003.
13 Grzybowski, T. Extremely High Levels of Human Mitochondrial DNA Heteroplasmy in
Single Hair Roots. Electrophoresis, 21, 548-553, 2000.
14 Grzybowski, T., Malyarchuk, B. A., Czarny, J., Miscicka-Sliwka, D., Kotzbach, R. High
Levels of Mitochondrial DNA Heteroplasmy in Single Hair Roots: Reanalysis and
Revision. Electrophoresis, 24, 1159-1165, 2003.
15 Hellmann, A., Rohleder, V., Schmitter, H., and Wittig, M. STR Typing of Human
Teloge Hairs – A New Approach. Int J Legal Med, 114, 269-273, 2001.
16 Houck, M.M. Hair Bibliography for the Forensic Scientist. Forensic Science
Communications, 4, 2002.
17 Houck, M.M., and Budowle, B. Correlation of Microscopic and Mitochondrial DNA
Hair Comparisons. Journal of Forensic Sciences, 47, 1-4, 2002.
18 Kintz, P. Testing for Anabolic Steroids in Hair: A Review. Legal Medicine, 5, 529-533,
2003.
19 Kintz, P. Value of Hair Analysis in Postmortem Toxicology. Forensic Science
International, 42, 127-134, 2004.
20 Linch, C.A., and Prahlow, J.A. Postmortem Microscopic Changes Observed at the
Human Head Hair Proximal End. Journal of Forensic Sciences, 46, 15-20, 2001.
21 Linch, C.A., Smith, S.L., and Prahlow, J.A. Evaluation of the Human Hair Root for
DNA Typing Subsequent to Microscopic Comparison. Journal of Forensic Sciences, 43,
305-314, 1998.
22 Linch, C.A., Whiting, D.A., and Holland, M.M. Human Hair Histogenesis for the
Mitochondrial DNA Forensic Scientist. Journal of Forensic Sciences, 46, 844-853, 2001.
23 McNevin, D., Personal Communication – papers to be published in Forensic Science
International and Journal of Forensic Sciences, 2004.
24 Prieto, L., Montesino, M., Salas, A., Alonso, A., Albarrán, C., Álvarez, S., Crespillo, M.,
Di Lonardo, A., Doutremepuich, C., Fernández-Fernández, I., González de la Vega, A.,
Gusmão, L., López, C., López-Soto, M., Lorente, J., Malaghini, M., Martínez, C.,
Modesti, N., Palacio, A., Paredes, M., Pena, S., Pérez-Lezaun, A., Pestano, J., Puente, J.,
Sala, A., Vide, C., Whittle, M., Yunis, J. and Gómez, J. The 2000-2001 GEP-ISFG
Collaborative Exercise on mtDNA: Assessing the Cause of Unsuccessful mtDNA PCR
Amplification of Hair Shaft Samples. Forensic Science International, 134, 46-53, 2003.

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25 Rees, J.L., Genetics of Hair and Skin Colour. Annual Review of Genetics, 37, 67-90,
2003.
26 Rowe, W. F. Unusual Medulla Morphology in Human Hair. Microscope, 50, 155-157,
2002.
27 Ruth, J.A., and Stout, P.R. Mechanisms of Drug Deposition in Hair and Issues for Hair
Testing. Forensic Science Review, 16, 116-133, 2004.
28 Sato, H. Statistical Evaluation of Morphological Data of Japanese Head Hair and the
Screening of Evidential Hair Samples by Cluster Analysis. Legal Medicine, 4, 90-102,
2002.
29 Sato, H. Preliminary Study of Hair Form of Japanese Head Hairs Using Image Analysis.
Forensic Science International, 131, 202-208, 2003.
30 Sato, H. The Quantitative Classification of Hair Form and its Application to the Forensic
Comparison of Japanese Head Hair. 8(1), 59-73, 2003.
31 Takayangi, K., Asamura, H., Tsukada, K., Ota, M., Saito, S., and Fukushima, H.
Investigation of DNA Extraction from Hair Shafts. International Congress Series, 1239,
759-764, 2003.
32 Taupin, J.M. Forensic Hair Morphology Comparison – A Dying Art or Junk Science?
Science and Justice, 44, 95-100, 2004.
33 Verma, M., Pratt, L., Ganesh, C. and Medina, C. Hair-Map: A Prototype Automated
System for Forensic Hair Comparison and Analysis. Forensic Science International, 129,
168-186, 2002.
34 Vincent, U., Bordin, G. and Rodriguey, A. R. Optimization and Validation of an
Analytical Procedure for the Determination of Oxidative Hair Dyes in Commercial
Cosmetic Formulations. Journal of Cosmetic Science, 53, 101-119, 2002.
35 Bisbing, R. E., and Houck, M.M. Examination, Analysis, and Application of Hair in
Forensic Science – Human Hair. Forensic Science Review, in press.
36 Tridico, S. Examination, Analysis, and Application of Hair in Forensic Science – Animal
Hair. Forensic Science Review, in press.

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 QUESTIONED DOCUMENTS –
HANDWRITING

— A Review: 2001 to 2004 —

Rolf Berzell
Statens kriminaltekniska laboratorium/Swedish National Laboratory of Forensic Science
Dokumentenheten/Document Department
SE-581 94 Linkoping
Sweden

Phone: +46 13 241448

Fax +46 13 241822
Rolf.Berzell@skl.police.se

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CONTENTS;

Introduction

References

Handwriting Examination

General Handwriting Examination

Signature Examinations
Examination of Numerals
Writing Instruments
Examination of foreign handwriting
Computer assisted handwriting examinations

Miscellaneous

Quality Assurance

Networking

Actual Trends and a Look into the Future

List of acronyms used

References

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INTRODUCTION:

The first part of this review covers reported progress on forensic handwriting examination and
the second part advances in other forensic document matters. Thus the contents of the first eight
pages is strictly dealing with the forensic examination of handwriting and signatures with some
related areas.

The review is based on:

1. Articles published in the major forensic science journals as well as papers presented at
international forensic QD meetings during the period 2001-2003.

2. Results of a survey among INTERPOL member forensic science services and leading forensic
document laboratories, asking for relevant contributions as well as complementary information
on the quality assurance policies within the reporting services.

The following INTERPOL Member States provided information for this review:

Colombia, Czech Republic, Denmark, Estonia, Finland, France, Germany, Georgia, Hungary,
Israel, Japan, Latvia, Lithuania, Mexico, the Netherlands, Norway, Northern Ireland, Poland,
Scotland, Slovakia, Spain, Sweden, Switzerland (various services) and Turkey.

REFERENCES:

The most important sources of reference are to be found in some of the major international
forensic science journals e.g. Australian Journals of Forensic Science, FBI Law Enforcement
Bulletin, Forensic Science Review, Journal of Forensic Sciences, International Journal of
Forensic Document Examiners, The Canadian Society of Forensic Science Journal, Journal of
the American Society of Questioned Documents Examiners, International Criminal Police
Review, Science and Justice etc. Articles published in other languages than English are mostly to
be found in Mannheimer Hefte für Schriftvergleichung.

There are various national and international conferences and symposia on questioned document
issues but those with a special interest in handwriting examinations are the following:

The biennial meetings of ENFHEX (European Network of Forensic Handwriting Experts), the
Biennial international congresses of the GFS (Gesellschaft für Forensische Schriftuntersuchung),
the Annual meeting of ASQDE (American Society of Questioned Document Examiners). The
biennial international meeting of Scandinavian Handwriting Examiners (today enlarged with the
Baltic States) also gives interesting information from the handwriting field (127).

HANDWRITING EXAMINATION

The debate on the interpretation and the presentation of evidence in handwriting cases has to
some extent continued but the number of articles and essays dealing with these matters has
decreased even if there are ongoing discussions in several countries how to change their
reporting systems. The debate on different scales of conclusions continue and the future will
show if there is a possibility to create one joint scale in the handwriting field. The Daubert
challenge in USA doesn’t seem to be very well known in European courts but, still, there is a
readiness among European examiners to defend handwriting methodology, if and when it will be
questioned (56).

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Kelly (69) advocates that the positive impact of the Starzecpyzel case has been the handwriting
studies and research conducted since 1995 and that courts can now point to these studies as a
means by which the evidentiary reliability and validity of forensic document evidence is ensured.

General Handwriting Examination

The earlier so lively flow of articles on interpretation and presentation of handwriting evidence
based on the Bayesian approach seems to have decreased quite substantially. Stockton and Day
(109), however, have given their version on how Bayes Theorem can be applied to handwriting
cases and Riess (94) has given an important contribution to the theoretical discussion of how the
Bayesian approach could be of use in future statements. On the other hand opponents have also
given voice to their opinion such as Bodziak (10) advocating that the statistical background is
more or less confusing for many document examiners and he questions if it could ever be used in
the U.S. legal system.

The necessary research to avoid future mistakes in handwriting examination is outlined by

Hecker (56). According to him it will be necessary to further develop the FISH-system and the
main features will be the approximation of various questions such as the quantitative off-line
evaluation of handwriting dynamics, the development of a coefficient expressing the identifying
value of signatures and the implementation of quality assurance measures including – among
others - the harmonisation of expressing conclusions with respect to the Bayesian approach.
Hanlen et al (53) discuss how forensic handwriting examinations can be established as a science
rather than a technical skill by defining the properties of individuality, reliability, performance
testing and validity. Srihari (105) discusses how to develop quantitative measures for
handwriting comparison and to develop new computer algorithms for forensic document
examination.

Found and Rogers in Australia (28, 29,30) have made many contributions in the handwriting
field of which e.g. their Forensic Expertise Profiling Laboratory (FEPL) is of great interest by
providing research programs aiming at characterising the skill and expertise associated with
forensic practitioners’ perceptual and cognitive processes. To date they have collated more than
50 000 blind trial opinions from nine countries on handwriting and signature trials. These
investigations have among other things provided information on how document examiners assess
original versus photocopied writings and the relative writing speed.

A personal experience having taken part in one such validation trial as described above is given
by Stuebe (112 ) who discusses the learning curve associated with taking the trials, how the trials
are set up, the information presented on the certificate the examiner can opt to have after having
one year of trials and the benefits of participation in the trials.

One frequent theme over the years has been to study the influence of alcohol on handwriting and
in a study performed by Chen and Leung (18) there is a report on how Chinese writing is
disturbed. A group of 151 occasional to habitual drinkers took part and the results confirm earlier
studies that there is an increase in size, spacing and pressure in the writing. Almost the same
results are reported by Asicioglu and Turan (5) but they also found that even the lowest level of
alcohol in the blood impairs the writing which haven’t been that clear in earlier studies.

Several studies have been performed on persons with different diseases. Buch and Contreras-
Vidal (12) show that Parkinson’s disease impairs the visuomotor adaptation and Rogers et al (95)
show that Parkinson patients could at least for a certain time write better if using different means
of assistance, such as supporting lines. The effect of Parkinson’s disease has also been
investigated by Stelmach, Ketcham and Dounskaja (107), Van Gemmert , Adler and Stelmach

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(116) and Teulings (113). Several of the studies treat the correlation between time of writing and
the size of the text (79, 91). Other diseases are rather seldom studied in connection with
handwriting but Zywucka-Kozlowska (125) has performed research on how Graves-Basedov
Disease influences on the appearance of handwriting.

In a study performed at the Silesian University in Kraków Buczek (13) tried the hypothesis if
there are statistically significant differences in the pace of tracing for persons from different
groups according to sex, degree of writing proficiency and age. The result was that in most cases
the criterion of sex doesn’t have any influence on the rate of tracing of neither counterfeit
signatures nor signatures made in their own handwriting whereas the degree of writing
proficiency does.

A support for the rule that a photo-copy never should be used in a handwriting examination is
expressed by Ciocian (19). She warns that even if the modern office image printing machinery
offers chances for almost perfect reproductions they can not reproduce the intricate features of an
original signature or handwriting in a satisfactory way. On the other hand Found et al (32) have
shown in a trial with 260 original signatures (and photocopies of them) that examiners are able to
make comparison on a complex signature with almost the same accuracy and similar sensitivity
when using either originals or photocopies.

The effects of handwriting produced by a guided hand has been discussed by Widla and
Swiderek (120) and the results show slower speed, irregularity, changes in the slant, higher
pressure and tremor.

Signature Examinations

Kam et al (66) show in a study of signatures comparing the abilities of forensic handwriting
examiners and laypersons in terms of signature examination that the error rates of the
handwriting examiners were considerably lower than for the laypersons. Even if the laypersons
were promised to earn some extra money producing a good result they did not improve their
performance.

The danger of giving opinions based on comparisons of small amount of signatures are discussed
by Harris (54). He also gives the following advice:

• never emphasise on one particular feature in a signature

• small but persistent differences in slant, size, shading and letter forms must be seriously
considered
• it is of vital importance to examine the handwriting of all parties involved in a case.

The decreasing quality of writing efficiency of signatures and what to do in the future to replace
the old type of signature is discussed by Owoc (88). He proposes that the New Signature (which
is his working name of it) should contain the following three elements:

• a stamp containing descriptive information about the bearer

• a traditional handwritten signature
• a print of the epidermal ridges pattern (the simplest would be that of a finger).

Found and Rogers (28) have continued their reporting on statistical modelling of expert’s
perception of the ease of signature simulation which is a field within handwriting examination
that can cause some problems.

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The difficulty to examine ”self-counterfeited signatures” of elderly people is discussed by
Koziczak (73) who among other advice says that ”…signatures whose graphism may change due
to natural causes (e.g. the bearer’s old age or illness) should be examined especially carefully…”
In some countries, as e.g. in the Argentine, it seems to be usual with short, illegible and strongly
simplified signatures. The risk and difficulty to examine this kind of signature is discussed by
Pena (89).

Examination of Numerals

Li Chi-Keung et al (77) found in a study where they collected specimens of the Arabic numerals
0-9 from 187 persons that no two individuals showed the same set of characteristic codes. They
developed a classification system based on characteristic features such as slant, writing direction,
relative position of strokes, angularity of turnings etc. The hypothesis of unique handwriting was
thus supported.

Seaman Kelly (68) made a study in which 200 persons took part writing a four-page exemplar
where three pages consisted of naturally written numerals whilst the participants were asked to
disguise their writing on the fourth page. The study showed that of the 200 persons 37%
connected at least one set of numbers using a connecting stroke but also that a significant
number of writers use more than one form of a numeral.

Writing Instruments

When examining signatures and handwriting produced with gel pens Oleksow and Matranga
(86) advocate that it is very important to be cautious because the class characteristics of these
pens are very special and it is easy to reach an erroneous opinion.

In another report on gel pens Czermak (20) has found that as an examiner you have to take into
consideration the interaction between paper surface and the writing instrument especially
concerning the line quality.

Examination of foreign handwriting

Grube and Zscach (51) have made a thorough survey of the difficulties with examinations of
foreign handwriting in Germany. They discuss especially the problems with examination of
Cyrillic handwriting which has increased after the fall of the Iron Wall. To examine block letters
in Cyrillic writing is, just as in the Latin writing, more difficult than to examine signatures. The
most important factor is, however, that the examiner has access to copy-book writings from the
countries concerned, which can be achieved through the constant growing collection of copy-
book models that has been created at the Dutch Laboratory (130). The plans are moreover to
make this database available on the ENFSI/ENFHEX website provided that access to the system
is well protected.

Aloyoni (3) maintains the opinion that when it comes to examination of foreign writings such as
Arabic handwriting and signatures you should do a thorough research and study of the
characteristics and then treat the findings with extreme caution.

A useful tool for examining foreign handwritings as efficiently as possible has been described by
Purdy (92). The Write-On Software is a computer program which is an aid especially when it
comes to large amounts of text where the program searches for comparable combinations of
letters and numerals and also provides more objective data that supports handwriting
conclusions.

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Another computer based system for recognition of handwritten text has been presented by Al-
Ohali-Y et al (2). Their paper considers work that has been done with regard to the establishment
of Arabic cheque databases for research into the automated recognition of handwritten Arabic
cheques.

Kurgoniene (74) reports on the bilingual situation in Lithuania where within the last century
Russian has influenced both the manner of writing and the spoken language. Her report, which is
based on the study of 700 Lithuanian and 200 Russian texts, analyses the influence of the
Lithuanian (or Russian) alphabet and mother tongue in Russian and Lithuanian texts written by
bilingual writers.

Abulafia and Gerber (1) have made a study in which 170 persons wrote in Hebrew, Arabic and
English to try to see if it is possible at all to compare different alphabets and if the findings could
give basis for any conclusions. The answer is that in the majority of the cases it was impossible
to reach any conclusion but in a number of cases the examiners dared to use rather strong
conclusions. Their research in this field will continue.

Computer assisted handwriting examinations

The renewal of the old FISH system for computer assisted handwriting examination has been
reported by Philipp (130) and the general approach of the system is quoted in the following:

”The FISH-new is a modular programme library and graphical user interface for acquisition,
annotation and storage of digitized handwriting. The overall design philosophy contains the
following elements:

• User actions (e.g. measurements) are costly. Therefore, the system should aim at convenient
entry and modification of data items
• The user should be guided in order to reduce subjective influence on the measurement
process. Where possible, script features are computed automatically.
• The system must be standard and multi-platform, certainly at the user client side, preferably
also at the server side.
• Results must be reproducible, on the basis of the original scan. The number of files
representing intermediate processing stages is reduced.
• The system will be realized in such a way that new insights in the forensic writer
identification technology can be added using plug-in software.
• The final demonstrator should be considered as a proof of concept, not as a finished
product.”

The above mentioned FISH-new system has been worked out by Franke et al (34) and an oral
presentation of if was given at the 3rd EAFS Meeting in Istanbul. The system has also been
presented in the ENFHEX bulletin under the name of WANDA (130).

Other contributions to computer assisted experiments in the handwriting field have been reported
by Franke and Köppen (38), Franke, Schomaker and Penk (39) and Franke and Grube (37).

MISCELLANEOUS

Sadorf (97) has reported on an unusual case concerning graffiti from Bayern where a suspect
individual declared that the almost perfect match between questioned tags and specimens from
him could be explained by his ability to almost perfectly copy tags that he had seen elsewhere in
the town. To prove this he volunteered to try to imitate (from his memory) six different tags. The
162
result was, however, that the handwriting examiners could easily see the difference between the
questioned tags and specimens produced by the suspect,

Lines and Franck (78) presented a report on the writing of triplets compared to the writing of
their non-multiple-birth sibling. This is the first time such a study has been reported in the
literature and the findings support the concept of natural variation in handwriting and two of the
premises of handwriting identification, namely that no two individuals write exactly alike and
that nobody writes the same text exactly in the same way twice.

Changes of copy book models in Poland have been reported by Widla and Garcarczyk (121) who
assumes that the new pattern will give better legibility, ability to write and economy of
movement

The old question of graphology versus forensic handwriting examination has been discussed by
Tomaszewski and Gruza(114) and the debate will certainly go on even if it seems difficult to
claim any scientific value in graphology.

The difficult task of teaching trainees to become handwriting examiners is discussed by Carlson
(14) and she proposes the marriage of Art and Science. The training to become a forensic
document examiner can also be formalised like Glass informs about the Master of Forensic
Science Administration Degree Program at Oklahoma State University (46). In Australia Sita
(101 ) has performed studies that has given many interesting and previously undocumented
relationships between features of the writing and examiners’ opinions. Using these findings a
model was constructed that can give a useful analytical tool for future training of handwriting
examiners.

QUALITY ASSURANCE

Even if some answers to the questionnaires indicate that a couple of laboratories are on their way
to start QA works according to ISO standards it seems as if the accreditation preparations have
not advanced as fast as could be expected. The laboratories that belong to a quality-accredited
service are still few. The laboratories that are working with QA are dependant on the national
accreditation bodies and one of the problems for the handwriting field is to find auditors within
their own countries. Apart from the English speaking countries this is almost impossible so there
has to be an exchange of expert auditors between different countries (at least for the small
nations). Moreover there is a language problem because all the QA documents are written in a
native tongue and these documents have to be translated to give the auditor a solid background
for his assessment.

Most of the laboratories that have answered the questionnaire report, however, that they take part
in some form of QA testing. The American Collaborate Testing Service (CTS) remains the most
international system but there are also other systems, such as the Australian system (from La
Trobe University) which now has participants world-wide. The difference between the
Australian testing system and the other systems is that the aim of the former is to give a basis for
a certificate for the experts taking part, a certificate where the error rate is mentioned. In Europe
many countries take part in the proficiency tests or collaborative exercises organised by
ENFHEX (129). The intention of these tests is to use writing from different countries so the
examiners will have a chance to get used to other copy-book models.

163
NETWORKING

The major regional associations such as ASQDE and AAFS in North America, GFS and
ENFHEX in Europe and ANZFSS in Australiasia continue their work with different activities
within the handwriting field. Minor groups exist also e.g. the Nordic Handwriting Examiners
who have meetings every second year together with experts from the Baltic states. The German
speaking countries have their regular meetings and repeated in-country conferences are held in
the UK. An example of how the work can be done is shown in the strategic plan for 2003 given
by ENFHEX (129):

• create databases of ongoing research projects,

• create a literature database
• organise exchanges of expertise between handwriting labs
• produce a survey of methods and procedures
• create a database of handwriting samples and copy-book models
• organise proficiency tests and collaborative exercises for the handwriting working group
• regularly publish the ENFHEX News Bulletin
• create a website for communication within ENFSI
• prepare new projects for EU funding
• hold handwriting and document sessions at EAFS meetings
• hold working group committee and business meetings

ACTUAL TRENDS AND A LOOK INTO THE FUTURE

The reduction of the use of cheques for payment purposes has continued during this period and
one of the main reasons is of course that electronic systems of payment and cash withdrawal
have increased in number. In some countries there are almost no handwritten cheques submitted
for handwriting examination while other countries have almost the same caseload or even have
seen an increase of such cases (52). One could suspect that the number of credit card slips with
signatures would increase instead of cheques but there has been no reports saying that either. The
use of electronic signatures when paying e.g. bills via Internet has increased rapidly even if the
security is not as high as could be desired.

There has been discussions if e.g. the forensic laboratories in Europe could develop an all-
European standard of competence for forensic scientists (126) and also if there is any possibility
to agree on how to write a forensic handwriting report including the scale of conclusion used.
According to Strach (110) the ideal would be a universally accepted scale for all the forensic
sciences but that the day for reaching such an agreement seems to be a long way in the future.

A good guess is that, in some years, we can expect more developed systems with computer
assisted handwriting examinations such as the WANDA system. According to Franke (130) this
system will give “… a huge potential for research and development in the field of forensic
handwriting and signature analysis as well as writer identification.” - “Moreover, the distributed
client/server architecture allows for joining and sharing collected handwriting data, domain-
specific knowledge and implemented software routines.”

To raise the level of competence among the handwriting examiners in Europe ENFHEX have
performed several efforts and one of these is the exchange of experts between European
laboratories. It seems as if this is a way to continue as the reports from these exchanges (126,
127, 128) have shown that they can spread a great deal of knowledge both to guests and hosts.

164
LIST OF ACRONYMS USED

ANZFSS Australian and New Zealand Forensic Science Society

ASQDE American Society of Questioned Document Examiners
ENFHEX European Network of Forensic Handwriting Experts
ENFSI European Network of Forensic Science Institutes
GFS Gesellschaft für Forensische Schriftvergleichung
IGS International Graphonomics Society
ISU Institut für Schrift- und Urkundenuntersuchung

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120) Ueda K, OCR-aided Preparation of Handwriting Comparison Charts for the Forensic
Examination of Japanese Documents; poster at the 3rd European Academy of Forensic
Science Meeting, Istanbul 2003
121) Van Gemmert A W A, Adler C H, Stelmach G E, The Isochronic Size Range is Reduced
in Handwriting of Parkinsonian Patients; proceedings of the 10th Biennial Conference of
the International Graphonomics Society, 2001 Nijmegen
122) Vargas R, Do People Always Disguise Their Writing the Same?; proceedings of ASQDE
2003, Baltimore
123) Vastrick T, Handwriting Identification: Back to Reality; proceedings of ASQDE 2002,
San Diego
124) Welch J R, A Survey of ”t-h” Joins in the Definite Article and Other Wording;
proceedings of ASQDE 2003, Baltimore
125) Widla T, Swiderek B, Handwriting by a Guided Hand; Document Various Specifications
no 4/2002, p 7-20, Wroclaw
126) Widla T, Garcarczyk M, Forming of Writing Habits; Document Various Specifications
no 3/2002, Wroclaw, p 7-12
127) Vydhyanathan A, Chennai, I N, Nadu T, Dynamic Signature Verification Using
Biometrics; poster at the 3rd European Academy of Forensic Science Meeting, Istanbul
2003;
128) Zhang B, Fu M, Yan H, A Nonlinear Neural Network Model of Mixture of Local
Principal Component Analysis: Application to Handwritten Digits Recognition; Pattern
Recognition, 2001,v 34, p 203-214
129) Zlotnick J, Lin J R, Handwriting Evidence in Federal Courts – From Frye to Kumho;
Forensic Science Revue, 2001, v13, p 87-99
130) Zywucka-Kozlowska E, The Effect of Graves-Basedov Disease on the appearance of
Handwriting; Document Various Specifications nr 4/2002, p 73-79, Wroclaw
131) ENFHEX news no 1.01
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134) ENFHEX news no 1.03
135) ENFHEX news no 1.04

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 FORENSIC SPEECH
AND
AUDIO ANALYSIS
FORENSIC LINGUISTICS

— A Review: 2001 to 2004 —

A.P.A. Broeders MA PhD

Chief Scientist
Netherlands Forensic Institute
Ministry of Justice
P.O. Box 24044

2490 AA THE HAGUE

The Netherlands

Phone: +31 70 888 61 26

Fax:+31 70 888 65 50
E-mail: t.broeders@nfi.minjus.nl

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CONTENTS

Abstract

Introduction

Speaker Identification
Speaker identification by earwitnesses
The present
Speaker identification by experts
Some history
The present
Expressing Conclusions in Speaker Identification
Organisations

Audio Analysis
Intelligibility Enhancement
Integrity and Authenticity Examinations of Audio Recordings
Disputed Utterances
Organisations and Conferences

Linguistic Authorship Studies

Organisation

Conclusions
Speaker Identification
Integrity and Authenticity Examinations
Linguistic Authorship Attribution
Final Conclusion

References

The Survey
Scope of the Survey
Casework
Research
Databases
Education and Training
Quality Assurance
Publications
Forensic Speech and Audio Analysis - Publications
Forensic Speech and Audio Analysis - Papers
Forensic Linguistics - Publications

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ABSTRACT:

Although the development of state-of-the-art automatic speaker recognition systems continues to

show considerable progress, performance levels of these systems do not as yet seem to warrant
large-scale introduction in anything other than relatively low-risk, investigative applications.
Conditions typical of the forensic context such as transmission channel mismatch, the presence
of background noise and mismatch of linguistic or communicative context continue to pose a
major challenge. Consequently, the impact of automatic speaker recognition technology on the
forensic scene has been relatively modest and forensic speaker identification practice, certainly
when applied for evidential purposes, remains heavily dominated by the use of a wide variety of
largely subjective procedures.

While substantial progress in forensic speaker identification performance remains relatively

slow, recent developments in the interpretation of the evidential value of forensic evidence are
now clearly beginning to make themselves felt. Conclusions in the form of a binary yes/no-
decision or a qualified statement of the probability of the (prosecution) hypothesis rather than in
the form of a statement of the probability of the speech evidence given a set of hypotheses are
increasingly criticised for being logically flawed. Instead, conclusion formats that make it
possible for results to be expressed in terms of a likelihood ratio are increasingly propagated and
becoming more widely used. However, unlike automatic procedures, traditional methods in the
field of speaker identification do not readily lend themselves to these formats. Against this
background, the need to put alternative validation procedures in place for traditional types of
forensic speaker identification is becoming more widely accepted.

Although speaker identification by earwitnesses differs in some important respects from the
much more widely studied field of eyewitness identification, there are sufficient parallels
between the two for speaker identification by earwitnesses to benefit greatly from a close study
of the guidelines that have been proposed for the administration of line-ups in the visual domain.
Some of the central notions are briefly discussed.

Rapid technical developments in the world of telecommunications in which speech and data are
increasingly transmitted through the same communication channels pose new threats for the
analysis of speech and audio interception as an investigative and evidential tool. The shift from
analogue to digital recording media and the increasingly widespread availability of digital sound
processing equipment as well as its ease of operation make certain types of manipulation of
audio recordings comparatively easy to perform. If done competently, such manipulation may
leave no traces and may therefore be impossible to detect. However, new methods for the
authentication of audio recordings utilizing mains frequency fluctuation and the visualization of
the magnetic patterns by exploiting the Faraday effect show considerable promise.

Authorship attribution is another forensic area that has had a relatively chequered history. The
rapid increase in the use of electronic writing media including e-mail, sms, and the use of ink jet
printers at the expense of typewritten and to a lesser extent hand-written texts reduces the
opportunities of authorship attribution by means of traditional document examination techniques
and may create a greater demand for linguistic expertise in this area.

A survey is provided of ongoing work in the area, based on reactions to a questionnaire sent out
in June 2004.

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INTRODUCTION:

The field of forensic speech and audio analysis comprises a wide range of activities of which the
most spectacular is no doubt speaker identification. Other activities in the field include
intelligibility enhancement of recorded speech samples, the analysis of disputed utterances, and
the examination of the authenticity of audio recordings. A related though in many ways very
different activity is linguistic authorship identification, the linguistic analysis of a spoken or
written text undertaken with a view to establishing the identity of the author of that text.

SPEAKER IDENTIFICATION

In spite of the regular appearance of high-tech speaker identification equipment in contemporary

fiction and the film industry, forensic speaker identification at the beginning of the 21st century
is an extremely challenging field, in which the promise held by technological advance remains
largely unfulfilled. This applies most obviously to large-scale forensic applications, which are as
yet virtually non-existent. Outside the forensic arena, the introduction of automatic speaker
identification technology in real-world applications has also fallen far short of what might be
expected on the basis of its popular appeal and the promise the technology initially seemed to
hold. So far it has mainly been limited to relatively low-risk applications, frequently involving
communication by telephone. According to Boves [1], one of the more successful applications
appears to be home incarceration surveillance.

Technically, a distinction is often made between speaker recognition - which is used as a cover
term for the wide variety of situations in which people are identified, or strictly speaking
individualised, on the basis of the sound of their voices - and the terms speaker identification and
speaker verification. Identification systems are those which compare a test speaker against all the
voices in a particular database to determine his or her identity; verification systems compare the
test sample with a reference sample of the speaker who is claimed to have produced the test
sample. In this sense, the forensic application typically amounts to a verification task, in that the
question that needs to be answered tends to be whether the recorded voice is that of a particular
speaker (i.e., the suspect). Occasionally, the term authentication is used for the process of
establishing the identity of a speaker, but this term is generally more appropriately used to
describe the examination of audio recordings with a view to establishing their authenticity (see
3.2 below).

The first and oldest form of speaker identification is of course speaker identification by ear-
witnesses. The second major category comprises all forms of speaker identification by experts.
At present, experts working in the field of forensic speaker identification use one of three
approaches: (i) a phonetic-acoustic approach, (ii) a (semi-)automatic, analytical acoustic
approach frequently combined with an auditory phonetic analysis, and (iii) a global automatic
approach. Also methods are employed in which elements of the three types are combined in
various ways.

SPEAKER IDENTIFICATION BY EARWITNESSES

The present

Today, procedures in speaker identification by witnesses for evidential purposes typically

involve the use of line-ups, following existing practice in the related domain of visual
identification of persons by witnesses [2, 3, 4, 5]. It is worth stressing that the use of single
person identification procedures, while producing positive identification scores in controlled
experiments that are comparable to those obtained for (multi-person) line-ups, is generally

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rejected except to confirm an earlier identification, or as an investigative rather than an evidential
tool. The reason is that line-ups, unlike identification procedures involving a single speaker only
(i.e., the suspect), make it possible to detect the vast majority of false identifications. Detection is
possible because in a properly designed line-up all members should have an equal probability of
false identification, which reduces the risk of a false identification going undetected to 1/N in an
N-person line-up, where 1/N is the likelihood of a false identification involving an innocent
suspect. By contrast, there is of course no way in which false-positive identifications can be
distinguished from correct identifications if only a single speaker is presented to the witness:
both correct and incorrect identifications amount to selection of the suspect.

Compared with the rich literature on eyewitness identification, which has created sufficient
consensus in the scientific community for a set of common guidelines to be formulated [6, 7, 8,
9], empirical studies of earwitness identification are few and far between, with the notable
exception of the work of Yarmey [10, 11]. The last decades have seen various attempts to
formulate guidelines for speaker identification by witnesses [2, 3, 4]. As in the visual domain,
the main purpose of these guidelines is to control variables that might unduly affect the result of
an identification test, rendering its meaning essentially null and void. In order to prevent such
undesirable effects from occurring, procedures should be carefully thought out and strictly
enforced. It is only when a positive identification cannot be argued to be due to other factors than
an observed correspondence between the memory trace of the perpetrator's voice in the witness's
memory and the sound of the suspect's voice that it can meaningfully contribute to the resolution
of an identity question. A set of guidelines based on those developed by Broeders & Van
Amelsvoort [3] was officially adopted by the ENFSI Expert Working Group for Forensic Speech
and Audio Analysis during the European Academy of Forensic Science Meeting held in Istanbul,
Turkey, in October 2003.

In addition to the 'formalised type' of speaker identification by witnesses that is used as evidence
for or against an individual's involvement in a crime, there is of course a very much greater
volume of speaker identification work carried out by members of police forces and interpreters
involved in the processing of the vast quantities of telephone interceptions undertaken within the
legal framework of various countries. However, speaker attributions in these calls are rarely
made on the basis of the speaker's voice quality and speech patterns alone. Frequently,
information about the line or number being intercepted and prior knowledge about the
whereabouts of callers as well as information from earlier calls will play a major role in
attributing a certain call to a certain speaker. In view of the vast amounts of telephone calls that
are intercepted in some countries it is remarkable that relatively few challenges of these
attributions are made and that an even smaller number of these challenges is successful.

A brief and concise review of the present state of the field of voice identification by witnesses is
provided by Bull & Clifford [12]. There remains a great deal of research to be done to increase
our insight in the effect of so-called estimator variables on speaker identification performance by
earwitnesses. These estimator variables include the nature of the speech and of the voice quality
of the speaker, the amount of speech heard by the witness, the delay between exposure to the
voice of the unknown speaker and that of the suspect, the effect of telephone quality speech, of
differences in age, gender and ethnicity between speaker and witness and of differences in
communicative context. But also in the area of the so-called system variables, which are
essentially under the experimenter's or forensic examiner's control, there is a need for additional
empirical research. A more fundamental problem is that of the questionable relevance of
laboratory experiments to actual forensic casework. Casual observers in a non-threatening
environment may well behave very differently from witnesses or victims who are paying close
attention to the person they are confronted with. However, it is clear that ethical considerations
frequently stand in the way of attempts to accurately recreate real-world situations in a controlled

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experiment. Meanwhile, we would do well to heed the repeated warnings by Bull & Clifford
[12], Yarmey [10,11], Ormerod [66] and others to treat speaker identification based on
earwitness evidence with considerable caution.

Speaker identification by experts

Some history

The second and probably most frequently practised form in the forensic context is speaker
identification by experts. One of the early approaches based on the use of the spectrograph
initially showed considerable promise and came to be known as the voiceprint technique. This
method was actually developed during the Second World War and essentially amounts to a
visual comparison of spectrograms of linguistically identical utterances to determine whether
they originate from a single speaker. In the second half of the last century the limitations of this
approach were demonstrated to be so severe that its status soon became extremely controversial.
While highly suggestive, the parallel with the fingerprint that the term voiceprint invokes, was
shown to be utterly misleading. Unlike, fingerprints, or friction ridge patterns, spectrographic
representations of speech are not invariant over time but highly variable within speakers,
reflecting the inherent within-speaker variability that is characteristic of speech. Yet, in spite of
the publication of a critical review of the use of the sound spectrograph for the purposes of
forensic speaker identification carried out by a National Research Council committee of the
American National Academy of Sciences [13], testimony based on modified forms of the
voiceprint technique as practised by members of the VIAAS (Voice Identification and Acoustic
Analysis Subcommittee) of the IAI (International Association for Identification) and others
continues to be admitted as evidence in US courts of law. Saks [14] reports that by his last count
it is admissible in six states, excluded in eight, admissible in four federal courts and excluded in
one. Brief surveys of the history of forensic speaker identification can be found in Braun &
Künzel [15], Meuwly [16], Hollien [17] and Rose [18] and, with special reference to the legal
situation in the United States, in Solan & Tiersma [19]. Ormerod [20] discusses the legal position
in England and Wales. He contrasts the preference expressed for a combination of auditory and
acoustic analysis of voice samples by the Court of Appeal for Northern Ireland in O’Doherty1
with the qualified approval given to an analysis largely based on auditory analysis only by the
English Court of Appeal in Robb.1

The present

There are probably few forensic disciplines that are characterised by such a diversity of methods
and procedures as the field of forensic speaker identification by experts. Basically, practitioners
can be divided in three groups. The first group consists of trained phoneticians. They rely
primarily on a combination of auditory phonetic analysis and a variety of acoustic
measurements, and will generally only consider themselves competent to analyse speech samples
in their own native language. Experts working within this phonetic-acoustic tradition, which was
pioneered by the German BKA in Wiesbaden, are found in several government forensic
laboratories including those of Germany, Austria, Sweden, the Netherlands and Spain, and in
private practice in countries like the United Kingdom and Germany. Perhaps the main criticism
of this type of approach is that it has a strong subjective element and does not easily lend itself to
validation [15].

The second group consists of those who use a set of semi-automatic measurements of a variety
of acoustic speech parameters such as vowel formants, articulation rate and the like, sometimes
combined with the results of a detailed, largely auditory phonetic analysis by a human expert.
Examples of this type of approach are the methods used in Italy (RCIS), the Dialect system used

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in Russia (FSC) and Belarus, the SIVE system used in Lithuania, and the type of method that is
frequently referred to as phonoscopy and is used in several Eastern-European countries.

The third, most recent approach differs form the first two in that it is both automatic and global.
It is automatic in the sense that any subjective analysis or evaluation of the speech material is
reduced to a minimum; it is global in the sense that it does not address specific acoustic speech
parameters but treats the signal as a physical phenomenon, more specifically as a continuously
varying complex vibration. Most automatic speaker identification systems today use a form of
Gaussian mixture modelling to characterise or 'model' the speech of the known, target speaker
(i.e., frequently the suspect in a forensic application) and that of the unknown speaker (i.e., the
perpetrator). In addition to this, a relevant speaker population is defined and a probability-density
function of the speech variance of this set is calculated. What the method essentially sets out to
do is determine how likely a degree of similarity or difference as found between speech samples
of the target speaker (say the suspect) and an unknown speaker (say the perpetrator) is to occur
within the relevant population.

There are two main problems with this approach. One is general and applies equally to other
types of speaker identification; the other is specific to a forensic-type application. The first is the
problem of within- and between-speaker variation. In the context of automatic speaker
verification this means that speaker models may overlap because they may occupy similar spaces
in the mode of representation utilised by the automatic technique. As a result, speakers may not
always be reliably distinguished, and the system will produce a certain proportion of false-
positives. As this is precisely the type of error that the criminal justice system should always take
great pains to avoid, the solution would seem to lie in adopting a more conservative decision
criterion. However, as in all biometric identification techniques and in decision procedures in
general, there is a trade-off between false-positives and false rejections, which means that a
system that is biased towards reducing false-positives will tend to produce unacceptable levels of
false rejections and/or report unrealistically low probability scores for matches.

The second problem is related to the extreme sensitivity to transmission channel effects of
automatic procedures, including the effects of different handsets, telephone lines, GSM-coding
and perception-based compression techniques as used in Minidisk players and compression
formats like MPEG. Research by Schmidt Nielsen & Crystal [21] suggests that, while human
listeners showed considerable individual variability in performance, on average they tended to
slightly outperform then current speaker verification systems. More importantly, they found that
it is especially when conditions deteriorate as a result of differences in transmission channels, the
presence of background noise and the like that human listeners are superior to automatic speaker
verification algorithms, with EERs of about 15 % for humans versus 25 % for machines. It is
precisely these conditions that tend to prevail in the forensic context. However, since the
publication of this research in 1998 the performance of automatic speaker recognition systems
has improved, if not spectacularly.

Many observers of the scene, including Schmidt-Nielsen & Crystal [21], believe that in order for
the performance of automatic speaker recognition techniques to improve significantly, a better
understanding of the speaker-specific, linguistic element in the speech signal will be necessary
[1, 22, 23]. However, such relatively long term ‘high-level’ features are difficult to extract
automatically. In a recent study [24] an attempt was made to analyze, characterize, extract, and
apply high-level information and combine this with short term low-level information in the
speaker recognition task. The goals were to develop new features and classifiers exploiting high-
level information, show performance improvements relative to baselines on an established
evaluation data and task, and demonstrate that new features and classifiers provide
complementary information. Results show that these novel features and classifiers indeed

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provide complementary information reducing equal error rates of systems employing a purely
acoustic approach from 0.7% to 0.2% when combined with high-level features. However, these
improvements were obtained for non-forensic material, using considerably longer training
material than is normally used in performance testing.

Fully automatic systems are gradually being introduced in forensic casework albeit on a
relatively small scale. They are currently used in France [25], Switzerland [16, 26] and Spain
[27], and are being tested in the United States of America [28]. The Dutch NFI, in collaboration
with TNO, recently finished a project which explored the possibilities of deploying state-of-the-
art automatic speaker identification procedures in police investigations, with a view to enabling
detectives to make better inferences as to the identity of foreign language speakers on intercepted
telephone lines. First results show that performance of state-of-the-art automatic identification
systems on real-world forensic speech data is not far below that for non-forensic material,
thereby making deployment for investigative purposes a realistic option [29]. It is worth noting
that the results were obtained in a text (and thus language) independent mode, with systems
performing equally well on test material in languages other than that used in the training session.

Expressing Conclusions in Speaker Identification

As in many other forensic identification disciplines, the formulation of the conclusions has been
receiving considerable attention in the literature in the last few years [30,31]. Traditionally,
forensic speech experts, like their colleagues in other forensic disciplines, have been expressing
their conclusions in terms of the probability that the questioned (trace) material originated from a
given source, usually the suspect. In recent years, partly accelerated by the advent of DNA
evidence, this type of conclusion has been challenged as logically flawed [32, 33]. Rather than
reporting the probability of the questioned (speech) material originating from the suspect, the
expert should report the probability of the evidence under two rival assumptions. One is the
prosecution hypothesis: the assumption that the material originates from the suspect. The other
hypothesis will generally be that the trace material originates from some other member of a
potential suspect population, like the adult male population of a town or a particular region. The
ratio between these two probabilities is called the 'likelihood ratio' and takes the form of a
number, which in the case of DNA evidence - where known distribution frequencies of what are
taken to be independent characteristics are multiplied - frequently assumes astronomical
proportions. Yet, even these high numbers do not indicate how likely the trace material is to have
originated from the suspect. This question may only be answered by the decision-making judge
or jury, who are in possession of all known facts of the case, and is an - ultimate - issue that is
considered outside the province of the expert. What the likelihood ratio does express is the
relative strength of the evidence, i.e., the extent to which it serves to make the prosecution case
stronger or weaker. Because of the conceptual problems posed by the (large) numbers involved
in the expression of the likelihood ratio, advocates of this approach, frequently known as
Bayesians, have suggested the use of verbal scales [34]. It is worth stressing that these verbal
terms express the relative strength of the evidence in favour of one proposition versus another
and do not address the probability of the actual proposition. Interestingly, methods involving
automatic speaker identification algorithms such as those pioneered by Marescal [25], González-
Rodriguez [27], Meuwly & Drygajlo [35] and Boves & Koolwaaij [36] readily lend themselves
to the Bayesian approach and typically employ the likelihood ratio format to express their
conclusions. A good illustration of the Bayesian approach is found in Rose [37].

It has been argued that, in spite of the semblance of qualified opinion that the phrasing of their
conclusions conveys, experts using traditional probability scales are effectively giving
categorical judgements [38], without necessarily always being aware of this. However this may
be, the claim provoked a prompt response by Champod & Evett [39], arguing the superiority of

178
the Bayesian approach to evidence interpretation. What is clear is that experts working in many
forensic identification disciplines are generally unable to quantify their findings to the extent that
the calculation of likelihood ratios becomes a realistic scenario. However, even if quantification
of parameter values is not possible or possible only to a limited extent, the Bayesian framework
may still serve as a useful conceptual framework, which separates the responsibilities of the
expert and the trier of fact. As in many other forensic identification disciplines, validation of the
methods and of the resulting opinions is often lacking in forensic speaker identification [14] and
is generally difficult to undertake.

Organisations

In addition to VIAAS (the Voice Identification and Acoustic Analysis Subcommittee of the IAI),
whose membership is predominantly American and is open only to those who are certified IAI
members, there are currently two more international organisations whose members are in one
way or another involved in forensic speaker identification. One is IAFPA, the International
Association for Forensic Phonetics and Acoustics (www.iafpa.net), which was formally
established in 1991 with the aim of providing a forum for those working in the field of forensic
phonetics as well as ensuring professional standards and good practice in this area. Its
membership is predominantly European. Until 2003 membership was open only to established
phoneticians. It now welcomes as members all those working in forensic speech and audio
analysis.

The second is the Expert Working Group for Forensic Speech and Audio Analysis. It had its
inaugural meeting in Voorburg, the Netherlands in July 1998 and has since met in Madrid,
Cracow, Paris, Moscow, Istanbul and in Toledo, earlier this year. It forms part of ENFSI, the
European Network of Forensic Science Institutes, which was set up in 1991, currently has 50
member laboratories in 32 countries and has been the driving force behind the establishment of
Expert Working Groups for the various forensic disciplines. The Forensic Speech and Audio
Analysis Working Group’s membership includes experts from 17 European countries, as well as
Turkey. One of the first priorities the Working Group has set itself is to collect information about
the various procedures that are used in the member laboratories.

In Spain, interest in forensic speaker identification and forensic acoustics is such that a national
society, SEAF (Sociedad Española de Acústica Forense), was formally established in 2000. It
brings together leading experts from such diverse fields as linguistics, electrical engineering,
acoustics and forensic phonetics, with a view to improving methods and techniques in speaker
identification and acoustic phonetics.

In response to a highly publicised court case in France, the AFCP (Association Francophone de
la Communication Parlée) initiated by the GFCP (Groupe Francophone de la Communication
Parlée) of the Société Française d’Acoustique (SFA), a group of predominantly French
acousticians who are active in the field of speech technology, circulated a petition on the internet
demanding that voice expertise be no longer used by the legal system until such time as it is
scientifically validated [40]. The group earlier suggested that it is unethical for anyone to be
active in the field of forensic speaker identification without first demonstrating his or her
competence in the field [41].

Both Braun & Künzel [15] and earlier Broeders [42] have argued that while there is a real
concern that voice evidence is presented in an irresponsible and incompetent manner, the charge
of unethical conduct is unfounded and the call for speech experts to dissociate themselves from
forensic examinations will ultimately only result in an increased danger that phonetically
uninformed testimony will go unchallenged. What is of the essence is that those who are

179
involved in deciding issues of guilt, i.e., judges and juries, are made aware of the limitations of
the methodology employed.

In a recent article by Bonastre, Bimbot and Boé, all members of the French AFCP and earlier
signatories of the French petition, and Campbell, Reynolds and Magrin-Chagnolleau, members
of the SpLC-SIG, the Speaker and Language Characterization special interest group of ISCA, the
International Speech Communication Association, the authors conclude that ‘at the present time,
there is no scientific process that enables one to uniquely characterize a person’s voice or to
identify with absolute certainty an individual from his or her voice.’ [43, p. 33] While
presumably wishing to emphasize that the discriminatory power and validity of forensic speaker
identification methods must be rated very considerably below that of forensic DNA analysis or
dactyloscopy, the authors seem unaware that, as it stands, their statement is valid for all forensic
individualization procedures. After all, all evidence is probabilistic and DNA evidence is
explicitly so. Absolute certainty, as traditionally delivered by fingerprint experts under the so-
called ‘positivity doctrine’, is not scientifically attainable [40b]. Somewhat in the same vein, the
authors argue that ‘[c]aution and judgment must be exercised when applying speaker recognition
techniques, whether human or automatic, to account for […] uncontrolled factors. Under more
constrained or calibrated situations, or as an aid for investigative purposes, judicious application
of these techniques may be suitable, provided they are not considered as infallible’ [43, p. 35].
Again, the problem is not that forensic speaker identification is not infallible but that there is
insufficient information about its validity. In a recent, critical appraisal it is factors like these,
i.e., the lack of validity and the non-scientific nature of many of the methods used, that Ormerod
[20] sees as the most serious shortcomings of the discipline. However, his suggestion that
instrumental phonetic analysis is inherently more valid and reliable for forensic purposes than
auditory phonetic analysis is met with considerable scepticism by Byrne & Foulkes [44], who
observe that ‘[o]ur data serve to remind us that blind reliance on instrumental data is potentially
dangerous.’ They found that ‘[f]ormant measurements, just like auditory data, may present
empirical difficulties, opportunities for different interpretations, and thus varying degrees of
forensic value.’

AUDIO ANALYSIS

Intelligibility Enhancement

Although the use of dedicated filtering hard- and software is widespread in this type of work, the
net effect of the use of this equipment in terms of getting additional words down on paper is not
always impressive. In fact, a large proportion of the work carried out under this heading is
probably primarily of a cosmetic nature; in judiciaries with a jury system in particular it is often
necessary for all relevant speech recordings to be played in court. Removing unpleasant noises
may facilitate listening for uninitiated listeners like members of the jury; it may also reduce
fatigue and thereby increase productivity in those who have to transcribe large quantities of
speech recorded under forensic real-world conditions.

The enhancement of clandestine or covert recordings, other than those made by private citizens,
is not a core activity for many forensic laboratories for the simple reason that covert recordings
made by police or other investigative forces will not normally be ruled admissible by a criminal
court of law. Information obtained from such recordings cannot therefore be used for evidential
purposes. The extent to which information obtained from enhanced audio recordings may play a
role as an investigative tool and the efficacy of covert recording is hard to assess because by
definition these matters do not lend themselves to public scrutiny. The public image of this type
of activity is strongly shaped by publications like Spycatcher [41] and the Francis Ford Coppola

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film The Conversation (1974), in which Gene Hackman plays an audio surveillance expert who
is slowly caving in under the psychological pressure of his job.

To achieve the best results in transcribing questioned utterances in low to extremely low quality
recordings the use of highly competent and educated native speakers of the language variety in
question is strongly recommended. A thorough familiarity with the accent and dialect of the
speakers in the recording, as well as familiarity with the details of the case and the voices of the
speakers, will often enable the analyst to compensate for the loss of redundancy of linguistic
cues that is characteristic of poor quality recordings.

Integrity and Authenticity Examinations of Audio Recordings

An interesting development in the field of authenticity and integrity examinations of audio

recordings in the analogue domain is the use of Faraday crystals as pioneered by a number of
Russian scientists. This has proved to be a valuable addition to the existing array of techniques in
this field [42]. Traditionally, these include visual inspection of the tape and its housing, auditory
analysis of the recording, magnetic development of the magnetisation patterns on the tape track,
narrow band spectrum analysis of the recorded signal, and, last but not least, high resolution
waveform analysis of the signal [43]. The analysis of replay transients, as Dean [44] calls them,
plays a central role in these examinations. The new, non-destructive method to inspect the
magnetic layer of a tape employs the Faraday effect. i.e., the ability of certain transparent
materials to rotate the polarisation plane of the light passing through it in the presence of a
magnetic field. The technique is rapidly gaining popularity among forensic experts working on
tape authenticity investigations. More specifically, a technique that uses ferri-magnetic garnet
films makes it possible to take pictures showing the magnetic flux distribution on a tape in such
detail that it enables the investigator to answer questions that could not be addressed reliably
before. The new method replaces the time-consuming and potentially destructive magnetic
development of the tape using ferrofluids with a non-destructive procedure that takes only
seconds to perform and makes it possible for multi-channel recordings to be easily discriminated
from single-channel recordings, which was sometimes impossible using traditional techniques.
More importantly, the new visualisation techniques are capable of revealing characteristics with
the degree of detail that is required to improve the discriminatory power to the extent where it
may be possible to trace a particular recording to a particular source recorder rather than merely
to a particular brand and type.

A second development which holds considerable promise was recently introduced by Grigoras
[45]. His method seeks to resolve authenticity questions for – longer - audio recordings by
comparing the fluctuations of the 50Hz frequency of the electric power network observed in the
questioned recording with the variations present in the reference registration of the fluctuations
as they occurred at the time when the recording was alleged to have been made. In some
European countries including Switzerland, records of these network fluctuations have been kept
for years. Since large parts of Europe are essentially linked to a single power grid which shows
the same fluctuations throughout its sphere of operation, these records are potentially relevant to
recordings made in all countries within this grid.

In spite of these new developments, there are serious limitations to the results of a tape
authenticity investigation. The increasingly widespread availability of relatively inexpensive
digital sound processing equipment and its ease of operation make certain types of manipulation
comparatively easy to perform. If done competently, such manipulation may leave no traces and
might therefore be impossible to detect from an engineering point of view. Failure to find
positive evidence of copying and/or manipulation does not therefore imply that the recording
under investigation must be a complete and uninterrupted magnetic registration of the acoustic

181
events it is supposed to represent. Faced with recordings of extremely incriminating telephone
conversations which were only available as copies, defence experts have been known to turn this
argument round: if the recording is a copy it cannot be authenticated and must therefore be
viewed with a high degree of suspicion regarding its authenticity. Not unnaturally, defence
lawyers will pick this up and argue that this means that any recording that is not claimed to be an
original recording but a copy should be ruled inadmissible as evidence because there is no way
in which its integrity can be established. However, the mere fact that a recording is a copy does
not ipso facto make it likely to have been tampered with.

The reservations made with respect to the authentication of analogue audio recordings apply
even more strongly to digital audio recordings. A brief discussion of the problems can be found
in Cain & Chial [46]. These are becoming more numerous as digital dictation machines are
becoming more and more common. As part of the chain-of-custody process, audio recordings,
like all digital data, are increasingly required to be authenticated by means of checksums, hash
codes or other methods to ensure their integrity.

Disputed Utterances

There are relatively few reports of either casework or research undertaken in this area. French
[47] provides an illustration of some of the procedures that may be helpful here.

A related issue is the growing demand for speech recognition systems to meet the need to
transcribe enormous quantities of forensic speech recordings. At present, the vast quantities of
recorded speech generated by telephone interception systems are transcribed by relatively highly
paid and trained human listeners. Most commercially available speech-to-text systems require
extensive learning sessions, a (single) co-operative speaker and relatively high quality recordings
to meet acceptable performance standards and are therefore unsuitable for forensic use.
Interestingly, the Lithuanian Institute of Forensic Examination in Vilnius reports a system called
Transcriber, produced by the Speech Technologies Centre, Russia, which it claims to be using
for the automatic conversion of speech to text.

Organisations and Conferences

The Working Group on Forensic Audio (SC-03-12) of the Audio Engineering Society (AES) is
currently revising its standard procedures for forensic audio. The first, AES27, was published in
1996 and provides recommended practice for managing recorded audio materials intended for
examination [46]. The revised version should be available by 2007. AES43, which was first
published in 2000 and lays down criteria for the authentication of analogue audio tape
recordings, should be revised by 2005 [47]. Two new standards planned for release in 2004 have
been downgraded to the status of Information Documents. They are AES-X10 (Guidelines for
Forensic Audio Analysis: Study of Requirements for Identification and Enhancement of
Recorded Audio Information) and AES-X135 (Forensic Audio – Recorded Audio Evidence
Collection FARAEC). AES is planning an International Conference on Forensic Audio in June
2005. More information can be found on its website www.aes.org. The FBI has developed its
own standards for forensic audio as part of its FAVIAU (Forensic Audio, Video and Image
Analysis Unit) standards.

Both IAFP - renamed IAFPA in 2003 to reflect the change of membership eligibility introduced
to include non-phoneticians - and the ENFSI Expert Working Group for Speech and Audio
Analysis organise annual conferences, frequently held back-to-back in the same venue or partly
as a joint event. A combined meeting took place in Moscow, Russia in 2002. In 2003 the ENFSI
Expert Working Group met in Turkey, as part of the triennial EAFS meeting held in Istanbul.

182
IAFPA met at Vienna in 2003 and in Helsinki in 2004. A special session devoted to Forensic
Speaker Recognition was held at Eurospeech 2003 in Geneva. A follow-up meeting to the
Martigny (1994), Avignon (1998) and Crete (2001) Speaker Recognition Tutorial and Research
Workshops was held in Toledo, Spain in 2004, back-to-back with the 7th Meeting of the ENFSI
Expert Working Group for Speech and Audio Analysis.

The Forensic Speech and Audio Departments of the German Bundeskriminalamt (BKA) and the
Netherlands Forensic Institute (NFI) obtained funding from the European Commission’s OISIN
II program for a three day seminar for European Specialists in automatic speaker
recognition/verification, which was held in 2003. The purpose of the seminar was to provide an
opportunity for forensic experts who use non-automatic methodologies to gain an insight in the
methods used, the limitations imposed by real-world conditions and the perspectives of
development of state-of-the-art automatic speaker recognition/verification systems. The focus
was on in-depth system demonstrations using forensically realistic data and on discussions of
decision criteria pertaining to the selection of the audio material and conclusions.

EESAG (the Electronic Evidence Specialist Advisory Group), Australia was successful in its
application to have laboratory accreditation. EESAG represents specialists involved in speech
enhancement, audio and video recording analysis, image and video enhancement, and the
application of digital imaging to forensic science. Its aims include the preparation of guidelines
for digital image processing and for the management of recordings for the purpose of forensic
examination.

Linguistic Authorship Studies

As seems to be the case for works of art in general, the authorship of literary texts is an issue that
has been known to generate prolonged and sometimes downright acrimonious debate. Heated
arguments have arisen over the authorship of diverse Classical Greek and Latin texts, as well as
over the attribution of seventeenth-century poems and plays to authors like Shakespeare,
Marlowe and Bacon [50]. In some cases of course, handwriting analysis can go a long way
towards answering these questions. An example from the non-forensic domain is the study of the
diary of Anne Frank [51]. However, if machine or handwriting analysis is not possible, a
linguistic analysis may be the sole type of evidence that may shed light on the authorship
question, short of the presence of clues in the contents of the text itself. Perhaps the first and
probably still one of the few truly scientific and quantitative approaches to the study of
authorship, sometimes also known as stylometry, was undertaken by Mosteller & Wallace [52]
in their authorship study of The Federalist Papers.

In the last decade of the last century, a method developed by the classical scholars Morton and
Michaelson called the Cusum technique enjoyed a short-lived popularity in Britain. Although the
method was not officially published until 1997 [53], results of this type of analysis were readily
accepted by courts in England and Australia. However, the method came in for scathing criticism
in several reviews including [54,55,56,57] and now seems to have vanished from the forensic
scene. Also in the last decade, the importance of the availability of large databases to quantify
the frequency of potentially author distinctive linguistic features came to be recognised. Two
very different examples are the KISTE-collection of forensic texts of the BKA [58] and the
Habeas Corpus of the University of Birmingham [59].

A basic controversy that has long divided the authorship identification community is that about
the distinctive character of common as opposed to less common words. While the Cusum
method claimed to base its discriminatory power on differences in the frequency of very frequent
phenomena like three- or four-letter words or the proportion of words starting with a vowel or a

183
consonant, others have worked on the assumption that it is rare words that are most characteristic
of a person's style. More generally, the idea is to establish author distinctive features. Most
recently, attempts have been undertaken to use neural networks to detect systematic differences
between authors. One major drawback for the forensic context is that meaningful results tend to
presuppose a fairly large amount of language. Unfortunately, in many cases, forensic texts tend
to be extremely short [59]. A useful survey of the type of information that may be relevant in
linguistic authorship identification is provided by McMenamin [60]. Woolls [61] describes the
use of a series of computer programmes specially developed to deal with forensic material in
questions of disputed authorship, including suspected plagiarism. An interesting development is
the availability of a variety of plagiarism tests, developed not primarily for forensic purposes but
in response to the need to determine the originality or otherwise of student essays. On the
internet, a plagiarism list can be found at http://lists.leeds.ac.uk/mailman/listinfo/plagiarism.
Chaski [62] describes the results of an attempt to provide empirical tests for author identification
following recent court decisions in the US on the admissibility of language-based authorship
identification. A thorough treatment of some of the theoretical problems in authorship
identification is given in [63]. On the internet, a forensic linguistics list can be found at
www.jiscmail.ac.uk/lists/forensic-linguistics.html.

Organisations

The International Association of Forensic Linguistics (IAFL) was founded in 1991. In addition
to authorship attribution, forensic linguistics includes the study of courtroom discourse,
courtroom interpreting and translation, comprehensibility of legal documents and texts, including
the police caution issued to suspects, and the use of linguistic evidence in court. IAFL organises
annual conferences, maintains a website (www.iafl.org) and publishes the journal The
International Journal of Speech, Language and the Law: Forensic Linguistics with its sister
organisation IAFPA.

Conclusions

Speaker Identification

Although the performance levels obtained by state-of-the-art speaker recognition technology are
now comparable to those of other major biometric identification methods [64], prevailing
conditions in the forensic context have so far stood in the way of large-scale introduction of
automatic methods [65]. Variations in recording and transmission conditions, the presence of
background noise and of variation due to differences in communicative context are responsible
for performance degradations of such severity that automatic methods either cannot be applied or
their results are difficult to interpret. Meanwhile, forensic speaker identification practice
continues to be heavily dominated by the use of a wide variety of largely subjective procedures
of which many have a strong phonetic or acoustic basis. The need to validate these methods is
increasingly acknowledged within organisations like IAFPA and the ENFSI Expert Working
Group for Forensic Speech and Audio Analysis. Recent developments in the interpretation of the
evidential value of forensic evidence are also beginning to make themselves felt in the forensic
speaker identification community.

Within the ENFSI Expert Working Group guidelines based on those by Broeders & Van
Amelsvoort [3] have been accepted for the conduct of earwitness identification tests. They are
similar in purpose and scope to those advocated for the more widely studied field of visual
identification by witnesses.

184
Integrity and Authenticity Examinations

A promising development in the field of authenticity and integrity examinations of audio

recordings in the analogue domain is the use of Faraday crystals as pioneered by a number of
Russian scientists. Comparison of mains network frequency fluctuations may help resolve
authenticity questions for longer recordings. These potential gains are offset by the widespread
availability of relatively inexpensive digital sound processing equipment. Its ease of operation
makes certain types of manipulation comparatively easy to perform. If done competently, such
manipulation may leave no traces. As part of the chain-of-custody process, audio recordings, like
all digital data, are therefore increasingly required to be authenticated by means of checksums
and hash codes or other methods to ensure their integrity. A first proficiency test on analogue
tape authentication organised by NFI for the ENFSI Expert Working Group on forensic speech
and audio analysis may help to improve standards for the field of forensic tape authenticity
investigations.

Linguistic Authorship Attribution

Authorship attribution is probably the oldest application of forensic linguistics. Nevertheless, the
discriminatory power of the methods used so far remains relatively weak, if it has not been
shown to be totally lacking. In countries like the United States of America and Australia, other
applications of forensic linguistics, not concerned with authorship identification, are becoming
increasingly prominent, as witness publications in journals like The International Journal of
Language and the Law: Forensic Linguistics.

Final Conclusion

On the basis of the findings of the survey, it would appear that the volume of work undertaken in
forensic speech and audio analysis has clearly increased over the last years. There are signs that
recent developments in the interpretation of the evidential value of forensic evidence are also
beginning to make themselves felt in the forensic speaker identification community. More
importantly, there are also clear indications of a growing awareness among those working in the
field of forensic speech and audio analysis of the need to view validation of the methods used as
an integral part of their discipline. In a field that was - and some would argue still is - somewhat
controversial, these developments may be long overdue but that does not make them any less
welcome.

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 Forensic Imaging

— A Review: 2001 to 2004 —

Jurrien Bijhold(1), Zeno Geradts(1), Lena Klasen(2)

1 Netherlands Forensic Institute (NFI)
2 Swedish Defense Research Agency (FOI)

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ABSTRACT
The rapid development of digital imaging technology and widespread use of camera's and video
re-cording systems for private and public applications has had a big impact on the development
of forensic image analysis. Four mainstreams of activities can now be distinguished in forensic
image analysis:
Imaging technology.
Capturing images and video from analog and digital media, filtering and sorting large amounts
of images and video, coding and decoding data, detection of manipulation, image authentication,
identification of camera's and systems as tools used for production of e.g. child porn movies. In
this field of expertise a lot of cooperation is needed with experts in audio technology, digital
evidence and information technology in order to keep up with all new developments.
Crime scene photography, laser scanning, photogrammetry and 3d-modeling.
Crime scene recording using combinations of wide view and close up photography and laser
scanning, panorama views, 3d-modeling of crime scenes, 3d-models as tools for interpretation of
questioned video recordings of e.g. shooting incidents, car accidents or explosions, scenario
testing using 3d-models of the crime scene, human bodies with wound channels, virtual stringing
of bloodstain pat-terns, etc. In this field of expertise many new forensic applications are being
explored.
Biometric identification .
The international concern for terrorist attacks has led to large investments in projects for testing
and introducing biometric systems based on finger scans, facial photographs and iris scans. The
demand for extremely large databases of finger scans and new insights from the development of
DNA evidence has led to a new interest for the process of fingerprint capturing and
identification.
While guidelines and procedures have been developed for forensic comparison of facial
photographs and estimation of body heights from surveillance video, it also has become apparent
that these methods for identification have to be used extremely carefully. New developments can
be expected from facial 3d-scans and 3d-data extraction from video.
Pattern recognition and forensic image databases.
A number of systems have been developed and demonstrated for storage and retrieval of images
captured from evidence such as shoeprints, cartridges, tablets and tool marks. Improvements of
automated retrieval are expected from more strict standards for the capturing procedures and
using 3d-scans instead of images. New developments are not pushed strongly now, because
investments in DNA-technology get higher priorities.
The development of forensic image analysis has also been pushed by the consolidation of a
number of relatively new international working groups: the European group ENFSIDIWG
(methods and techniques), the US groups SWGIT (guidelines and best practice manuals) and
LEVA (training on video processing), and the Australian group EESAG (proficiency tests for
video and audio processing).
A survey is provided of ongoing work in the area, based on information from direct
communications with these working groups and an extensive literature search.

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INTRODUCTION

The rapid development of digital imaging technology and widespread use of camera’s and video
recording systems for private and public applications has had a big impact on the development of
forensic image analysis. In 2000 and before, there was still debate going on about the admittance
and quality of digital photography and the main applications of digital image processing were in
the fields of document analysis and enhancement of fingerprint images and surveillance video
images. Nowadays, quality and admittance seems to be not so much disputed anymore, and
digital photography and video have been introduced in almost every forensic discipline. The aim
of digital image processing is gradually shifting from image enhancement to image
interpretation. The availability of large amounts of digital images has led to the development of
image databases that can be searched using pattern recognition technology. The latest
developments concern the introduction of scanning technologies that give 3-dimensional
information about a crime scene or the surface of e.g. a tool mark.

This review is based on information from an extensive search in literature databases (Inspec,
Compendex and several others), participation in meetings organized by the AAFS, ENFSI and
SPIE, and contacts with the working groups SWGIT, LEVA, EESAG and ENFSIDIWG. This
review is certainly not complete for two reasons: most of the information used is obtained from
American and European sources and the scope of the review is limited to the fields of expertise
that the authors have been working in or with. A questionnaire with the abstract of this paper was
sent by email to members of these working groups and contacts of the authors in some institutes
in Japan and China. However, the number of responses was so low that it appeared to be not
possible to base any general statement about the state of forensic image analysis from them

In this review, we describe the most important developments in separate chapters for each of the
following fields of expertise: (1) imaging and video technology, (2) photogrammetry and
computer modeling, (3) biometric identification and (4) pattern recognition in forensic image
databases. Then, we focus briefly on a number of forensic activities that do no fit well in the
previous chapters like medical imaging, document analysis and face reconstruction. The last
chapter deals with relevant organizations and their work in forensic image analysis. Each chapter
starts with a list of keywords to help the reader finding topics of interest. Literature references
are given at the end of each chapter.

IMAGING AND VIDEO TECHNOLOGY

Keywords: Capturing images and video from analog and digital media, image processing,
filtering and sorting large amounts of images and video, coding and decoding data, detection of
manipulation, image authentication, identification of camera’s and systems as tools used for
production of e.g. child porn movies, damaged media, Multimedia analysis

Video surveillance systems are still the most important source of questioned images for forensic
investigation. Numerous companies have developed systems for capturing and analyzing
analogue video in ways that minimize the damage to the tape by replaying and result in almost
perfect digital copies without loss of quality due to e.g. data compression. Applications of real
time video processing that help dealing with analogue video are: de-multiplexing (sorting images
from different cameras) and automated detection of changes in a scene. Many surveillance
systems are now being replaced by digital systems. Although degradation of image quality due
to wear of the magnetic tape is no longer a problem, the image quality of digital systems is now
often worse than of analogue systems due to the data compression applied. The acquisition of
images from these systems often gives problems that can only be solved with help of computer

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technicians that are trained in the field of digital evidence (11). At the moment, the quality of
surveillance video images almost never allows for identification of depicted people.

In many countries, the widespread use of private and public surveillance systems with 32 or
more camera’s allow for new applications such as tracking cars and people (12,13) by focusing
on features like color, shape and size. Errors in the process of tracking people in a typical
multiplex time lapse recording (recording of 4 images per second and switching between
different cameras) are easily introduced by wrong interpretation. During the time that no images
are recorded, or the recording switches between camera’s, different look-alike people or cars can
move in or out the scene. In a digital capture of analogue video (10), images can be easily missed
due to bad quality of the video signal.

Timing of surveillance video also deserves some attention. The frame rate of analogue time-
lapse video varies for short time intervals, and the time and date that is printed in the images is
not equal to the correct time and date.

Surveillance cameras are usually mounted at a fixed position and orientation. This is an
advantage for forensic applications such as photogrammetry and image comparison, because the
results of an analysis can be rather easily verified or validated. Video-overlay techniques can be
used now to detect changes in the camera mounting and zoom and can also help to restore them
for the purpose of recording reference images.

Private, TV or police observation video recordings made with a camera that is held in a hand
or on a shoulder are being offered now for forensic analysis in large numbers. If something
happens that attracts the attention of the public (2,3), like an accident (7), a disaster, a shooting
incident, a riot or a demonstration, it is almost certain that video recordings have been made by
witnesses. Taps of emergency phone calls can give extra audio information for the reconstruction
of what happened actually. Image quality is generally better that surveillance video. Typical
problems are shaking and fast unpredictable movement of the camera, and uncertainties in the
camera position, direction and zoom of the lens.

Numerous methods have been developed to compensate for small camera movements and
rotations, simulating a more stabile viewpoint in the video images. Some of these methods go
further and try to take advantage of small camera movements. The idea, referred to as super-
resolution, is to combine a sequence of video images into a high resolution image by estimation
the displacements of an object in each image of the sequence with a precision that is better than
one pixel size. A license plate might be unreadable in each images of a sequence. The
information content in each image needed for the reconstruction of the license plate can be
different if the car or the camera had moved between two image recordings. Super-resolution
(4,8) aims at a smart combination of images in a sequence of images to get a new image with
more information content. So far, the authors have not been presented examples of successful
application in actual case investigations.

Multimedia analysis might be a new keyword for referring to reconstructions of accidents,

shooting incidents or disasters, based on multiple video-recordings, audio-taps, photographs,
infrared-photography, satellite images, seismic sensors etc. In order to get more information
from the combination of these sources, all these recordings have to be synchronized and
corresponding objects and persons have to be identified in all images. Methods are needed now
for smart storage and retrieval of large amounts of unstructured multimedia data. A special
application has been identified in the forensic analysis of child pornography. The idea is to
compare every image or video-stream that is found on a suspect’s computer with a multimedia
database in order to find images that show corresponding children or backgrounds. This

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information is used to detect new, unknown children that are victims, and relations between
different cases. So far, only results have been reported in automated detection of copies of
known images.

Formats and Codec’s are standard methods and/or pieces of software for coding images, video
and audio into digital data-files or streams. Especially, the choice of a codec and the software
that codes or decodes can have a big influence on the quality of images and audio signals.
Codecs are used for data compression. Most of them work by analyzing the information content
in the data and removing data that is considered less important. The authors expect that this loss
of information might be a cause of debate in forensic investigations of the near future.
Knowledge of the implementation of the JPEG-codec has proven to be useful for the restoration
of digital images. For presentation in court of video files with different software and hardware,
the quality of the video might differ from the quality that has been seen in the laboratory

Image integrity and authenticity are often questioned in cases of child pornography, snuff-
movies, and TV-documentaries or news programs that show video footage as evidence. Many
methods have been reported for detection of manipulation by checking file header information,
transitions in the images that cannot be explained for, and changes in the background noise
pattern. However, it is generally accepted that it can not be proven that an image has not been
manipulated, unless the original image is known and recognized.
For the purpose of crime scene photography camera’s are being used that can encode the image
in such a way that any alterations of the image can be detected by the viewing software that
comes with the camera. It is also possible to encode identification numbers for the camera and
the photographer. A study is being done by the Bundeskriminalamt in Germany for further
improvement of these methods. Also the number of steganography software packages for hiding
information in images is expanding. The software is available for free from the Internet. There
have been several test methods reported (1).

Camera identification is an investigation that aims at proof that a questioned digital image or a
video-stream has been recorded by a camera that was found in the neighborhood of a suspect.
One of the best methods available at the moment is the analysis of image defects (5,9) that are
caused by defects in the CCD-chip of the camera. Other indications such as camera-
identification numbers in the data, defects or pollution in the lens system that affect the images
visibly have not been seen in actual case work yet. It is expected that camera identification might
be virtually impossible in the near future due to data processing in the camera or the computer on
which the data is stored and viewed.

CRIME SCENE PHOTOGRAPHY, LASER SCANNING, PHOTOGRAMMETRY AND

3D-MODELING

Keywords: wide view and close up photography, photogrammetry, laser scanning, panoramic
views, 3d-modeling of crime scenes, 3d-models as tools for interpretation of questioned video
recordings, shooting incidents, car accidents or explosions, scenario testing, visualization of
wound patterns and channels, virtual stringing of bloodstain patterns, etc. , 3d-from video

Crime scene photography and computer modeling. The introduction of computer modeling
techniques has led to new interest in approaches to crime scene registration. One of the first and
most simple applications of computer modeling has been introduced in a number of software
packages for the reconstruction of car traffic accidents. A 2-dimensional model of the road with
traces like tire marks can be constructed from photographs, if sufficient reference points are
available at the scene. Firstly, distances between these points are measured with measure tape or
a geodimeter. Then, points and lines have to be marked in the photographs that will be used as

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input for calculations and simulations of the accident. Finally, top view images and graphs of the
road with all the marks are computed using these distances as reference information. The top
view images are actually warped copies of the photographs. The result is a 2-dimensional model
that exists of lines and points and top view images that than can be pasted into this model.
Many organizations (16,17,18,19,20,21,22) are now using or testing general application
modeling software packages for constructing 3-dimensional line models of crime scenes from
photographs. These packages can also be used for computing top view images of walls, floors
and traces on e.g. a table. This kind of work requires a good organization of crime scene
photography. Sufficient markers have to be placed at the scene in order to get a geometrically
accurate model of all the walls, objects and traces that are marked in the overview and close up
photographs.

Panorama photographs and interactive visualization of a crime scene. A 3-dimensional

computer model of the scene can be used for numerous applications, but the construction
requires a lot of skills and a substantial amount of time. However, for the purpose of giving an
overview of the situation at the crime scene to colleagues, other investigators and the court, new
methods of photography are available that do not require a lot of extra skills and time and that
yield an interactive view from one viewpoint in the crime scene in a webpage. The viewer can
look around in the scene by intuitively moving the mouse. Other viewpoints or other crime scene
documentation can be found by clicking hotspots in the view.

Laser scanning. Recently, scanners are available that produce images with range data. These
scanners are usually mounted on a tripod and have a rotating head and a laser beam. If this light
is reflected from an object, the scanner registers the distance to this reflecting point, the rotation
angles of the scanner head and finally the color of the reflecting point. The result is a point cloud
that can be interactively viewed. Since the result is a cloud of unconnected points, interpretation
can be difficult, especially if no reference points can be recognized in the cloud. An advantage is
that accurate measurements can be done directly in this data. Constructing a computer model of
the crime scene from this point cloud is not a straight forward process and requires a lot of skill
and time.

Video recording of a scene and computer modeling. Another simple method for getting and
presenting an overview of the situation at a crime, or an accident, scene is a video recording.
Future developments concern the storage and retrieval of this kind of recordings in crime scene
knowledge databases and the construction of 3-dimensional computer models of the scene, or
parts of it.

Testing and animations of scenarios. Once a computer model of a scene is available it is

possible to put models of people and objects in the virtual scene. The model (22) can be viewed
from the viewpoint of an eyewitness to test a number of possible configurations of the people
and the objects in the scene. In software packages for producing animations it is possible to
visualize different scenarios for movements of people and objects in the scene. This activity has
been referred to as scenario testing. So far, not many results have been reported yet. However,
animations of scenarios for crimes and accidents are often shown on TV and in court. Since an
animation gives a very strong suggestion of truth, that is certainly not desirable in investigative
court systems, new methods for visualizing scenarios have to be developed. These visualizations
should give information about accuracy of the geometry and the time intervals, the completeness
of the model (can it show all traces?) and the distinction between facts and assumptions.

So far, visualizations of bullet trajectories in models of a scene have been reported (19), as well
as wound channels in models of humans and the results from bloodstain analysis. The last
activity is referred to as virtual stringing.

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Projection of 3d-models on photographs and video has proven to be very useful as a tool for
image interpretation. The idea is to place a virtual camera in the computer model (12, 14), that
corresponds to the position, orientation and zoom of the camera that was used for the acquisition
of the questioned image. If a corresponding virtual camera is placed in the model, its view of the
points and lines in the model can be fit as an overlay onto the image. Most software packages
can place this virtual camera automatically after the user has marked reference points in the
model and in the image. This process is referred to as camera matching. Projection of a model on
an image can help to identify objects in an image or to find points that correspond in images
from different cameras. Measurements can be done by placing virtual rulers in the model.
However, the accuracy of the camera match will have a big impact on the accuracy of the
measurement and it is strongly recommended to do appropriate validation (20,21,22,26).

BIOMETRIC IDENTIFICATION

Keywords: Facial image comparison, height estimation, biometric systems, fingerprint

processing, Bayesian approach, likelihood ratio’s, ear prints, gait

Height estimation and gait. Because surveillance video images almost never show clear details
of a face, one of the most frequently asked questions is if it is possible to measure the body
length of a person depicted in the video. Since most video images show a person walking,
wearing shoes and hats or caps, most investigators prefer to do an estimation of the height. The
height is defined as the distance between a point on the floor between the feet and the top of the
head including hair, a hat or a cap. The marking of these points in a video image is not accurate,
and prone to errors in the interpretation of the image, especially in views from cameras that are
mounted at a ceiling. Further, one study (30) has shown that the top the head goes up and down
in a walking cycle over distances up to 8 cm. In a video image it is not always clear at which
point in a walking cycle a person is depicted. Because of these uncertainties, height estimations
can only be used as very weak indications for identifying a suspect. Cases have been reported
that suspects could be excluded by height estimation. A number of methods and guidelines have
been published (24,30) for doing height estimations. In all cases, it is strongly recommended to
make reference recordings with known persons, and preferably also the suspect, with the same
video surveillance system at the same location under similar lighting conditions. In this
approach, systematic errors in the photogrammetry applied and the interpretation of the video
images can be more easily detected.

Another frequently asked question is if persons can be recognized in video by analyzing their
gate. One study has been reported that shows that parameters of the gait (42) are not very
distinctive and can not be measured accurately in time-lapse video.

Facial image comparison. People doing facial image comparison can be found in three different
kinds of professions: forensic photographers , forensic anthropologists (33) and video
investigators. A lot of literature (31,32,35,38,41) exists on comparison of good quality
conventional chemical photographs in which many facial details can be seen. A number of
methods have been published in the past for the acquisition of reference photographs that show
the face of a suspect in a comparable pose and from a comparable distance. Knowledge of
anatomy and physiology of the face is needed to get a better interpretation of differences and
similarities in facial features. In the comparison of facial video images, or the low quality digital
photographs in passports conform to ICAO (International Civil Aviation Organization)
standards, it appears that small details are almost never visible. Obvious similarities or
differences in such images can often be explained by differences in the imaging conditions.
Therefore, it is strongly recommended to acquire reference images of the suspect and a number

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of other people with the same video camera in the same situation under similar lighting
conditions. A small facial detail is mostly depicted as distorted due to noise, pixel sampling and
compression. In a sequence of reference images, it can be checked if this distortion does not
change for small changes in pose and position of the suspect.

Statistical data that can be used to estimate the uniqueness of a facial feature are hard to find. A
number of studies are being carried out now in which data is collected from 3-dimensional facial
scans.

Biometric systems. The international concern for terrorist attacks has led to large investments in
projects for testing and introducing biometric systems based on finger scans, facial photographs
and iris scans. Future forensic investigations might be assessing the evidential value of
recognition by such a system or, finding out how a system could have been misled (43).

Automatic face recognition. In the forensic community is a widespread concern about the
public expectations from face recognition. The quantities of questioned images from surveillance
systems, web-cams, phone-cams, biometric systems are growing while the quality of the images
is getting worse. The quality of digital photographs in passports is already far worse than from
conventional chemical photography.

Fingerprint capturing and processing. The demand for extremely large databases with finger
scans for border control has led to a new interest for the process of fingerprint capturing,
processing and identification. Debate is still going on if digital image processing (28) of
fingerprint images is admissible in court. The reproducibility of a finger scan or a fingerprint and
the feature extraction are being studied now. One study is being carried out, that aims at
estimation of likelihood ratio’s for fingerprint identification using data from conventional AFIS-
systems and estimations of variations in the process of fingerprint capture, processing and
feature extraction. The idea of estimating likelihood ratios is generally referred to as the
Bayesian approach.

Earprints. The European ECG funded project FearID (45) is an in-depth study of the evidential
value of latent ear-prints that can be found at a scene of crime. Methods are being developed for
capturing the prints, processing and feature extraction, for database storage and retrieval. The
development of ears and their anatomical changes in a life time are studied. The project aims at
an assessment of the uniqueness of ear-prints. Publication of results is expected in 2005.

PATTERN RECOGNITION AND FORENSIC IMAGE DATABASES

Keywords: Cartridges, shoeprints, toolmarks, tablets, surface scanning

A number of systems have been developed and demonstrated for storage, comparison and
retrieval of images captured from evidence such as shoeprints (61, 62), cartridges
(46,47,48,49,50,51,52), tablets (60, 59) and tool marks ( 53,54,55,56,57,58,59). Improvements of
automated retrieval are expected from more strict standards for the capturing procedures and
using 3d-scans instead of images. New developments are not pushed strongly now, because
investments in DNA-technology get higher priorities. One paper describes the use of 3d-surface
scanning for the investigation of plastic bags (63),

Since the authors have stopped working in this field and activity in the field of databases is very
low in the forensic community, this review is limited to a list of publications.

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RELATED FIELDS OF EXPERTISE

Keywords: document analysis, face reconstruction, medical imaging

Document analysis, including handwriting has always been posing interesting problems for
forensic image analysis. Some problems like the judgment of crossing ink lines (65),
enhancement and analysis of latent images of handwriting, classification of the paper, and the
printer or the copier used, might be solved by a multidisciplinary approach that includes forensic
image analysis and pattern recognition. Handwriting analysis is a forensic discipline in itself and
new methods for image analysis and pattern recognition are still being implemented. One
special application of pattern recognition that should be mentioned in this review is the
reconstruction of ripped-up documents (66,67).

Face reconstruction from skulls or dead bodies is done by forensic anthropologists for the
purpose of finding people that might be able to able to help identifying a dead person. The first
international meeting on the reconstruction of soft tissues in Potsdam 2003 aimed at forming a
network of anthropologists, artists, computer imaging scientists and specialists in forensic facial
identification. Many techniques appeared to be based on the availability of statistical data for the
thickness of tissues. Statistical data of facial features, and their change in a life time, are also
important for the discipline of facial image comparison. Apart form the proceedings of this
conference, the following publications have been found: (69,70,71,72).

Medical imaging for forensic applications is a discipline with a very small number of active
institutes. The ideas that were found in the publications give a hint of how the future might
change for forensic pathologists and anthropologists (73,74,75,76,77,78,).

WORKING GROUPS AND ORGANIZATIONS

Keywords: guidelines, proficiency tests, collaborative exercises, quality assurance

The development of forensic image analysis has strongly been pushed by the consolidation of a
number of relatively new international working groups:
• ENFSIDIWG : a European group that is primary focused on methods and techniques.
(http://www.forensic.to/webhome/enfsidiwg)
• SWGIT: an American group that has produces a lot of guidelines and best practice
manuals. (http://www.theiai.org/swgit/)
• LEVA : an American group focused on video processing and training
(http://www.leva.org)
• EESAG: an Australian-New Zealand group that proficiency tests for video and audio
processing)
• SPIE working group for Investigative Image Processing has contributed to several
publications in this field.
(http://spie.org/Membership/index.cfm?fuseaction=TG_InvestigativeImage)
• A working group that is especially focused on facial image comparison was found in
Germany: http://www.foto-identifikation.de/ .
• An active web-based working group working on forensic applications of computer
modeling can be found on: http://groups.yahoo.com/group/forensic3d/

The following SWGIT-documents can be found on:

http://www.fbi.gov/hq/lab/fsc/current/backissu.htm (86)

ENFSIDIWG documents and presentations have been published on two CD-roms: the
ENFSIDIWG meeting in Zurich 2002 and the ENFSIDIWG meeting in Prague 2004. that

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have been made available to all members of ENFSIDIWG, SWGIT and EESAG.

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42. Use of gait parameters of persons in video surveillance systems , Geradts Z, Merlijn
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43. Extracting forensic evidence from biometric devices, Geradts Z, Ruifrok A. Proc.
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46. Line-scan imaging for the positive identification of ballistics specimens., Smith, C.L.
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47. Development of a 3D-based automated firearms evidence comparison systern,

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48. An intelligent imaging approach to the identification of forensic ballistics specimens.

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49. Image matching algorithms for breech face marks and firing pins in a database of
spent cartridge cases of firearms, Geradts Zeno J.; Bijhold Jurrien; Hermsen Rob;
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50. Reference ballistic imaging database performance, J de Kinder, F Tullener and H

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51. Three dimensional visualization and comparison of impressions on fired bullets,

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53. Model-based analysis of striation patterns in forensic science. Heizmann, M.; Puente
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54. Pilot investigation of automatic comparison of striation marks with structured light.,
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55. Imaging and analysis of forensic striation marks., Heizmann, M. (Inst. fur Mess und
Regelungstechnik, Univ. Karlsruhe, Germany); Leon, F.P., Optical Engineering (Dec.
2003) vol.42, no.12, p.3423-32 Published by: SPIE

56. Pattern recognition for optical PSI images of surface topography using wavelets.
Xiangqian Jiang (Sch. of Eng., Univ. of Huddersfield, UK); Shaojun Xiao; Blunt, L.,
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57. Automated comparison of striation marks with the system GE/2., Heizmann, M. (Inst.
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USA, 4 April 2002

58. Strategies for the automated recognition of marks in forensic science, Investigative
image processing II : Orlando FL, 4 April 2002, HEIZMANN M., SPIE proceedings
series, (2002), 4709, 68-79, Conference: 2 Investigative image processing.
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59. Evaluation of contents based image retrieval methods for a database of logos on drug
tablets., Geradts, Z.J.; Hardy, H.; Poortman, A.; Bijhold, J. (Netherlands Forensic
Inst., Rijswijk, Netherlands), Proceedings of the SPIE - The International Society for
Optical Engineering (2001) vol.4232, p.553-62. Published by: SPIE-Int. Soc. Opt.
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MA, USA, 5-8 Nov 2000

60. 3D capture, representation and manipulation of cuneiform tablets., Woolley, S.I.;

Flowers, N.J.; Arvanitis, T.N.; Livingstone, A.; Davis, T.R. (Birmingham Univ., UK);
Ellison, J., Proceedings of the SPIE - The International Society for Optical
Engineering (2001) vol.4298, p.103-10.,Published by: SPIE-Int. Soc. Opt. Eng,
Conference: Three-Dimensional Image Capture and Applications IV. San Jose, CA,
USA, 24-25 Jan 2001

61. New Developments in Forensic Image Processing and Pattern Recognition.

(Proceedings of the Forensic Science Society Meeting 'European Connections", April
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(Forensic Science Soc., Harrogate, UK), 8 pp.

62. Data mining in Forensic Image Databases, Investigative image processing II : Orlando
FL, 4 April 2002, Geradts Zeno; Bijhold Jurrien , SPIE proceedings series, (2002),
4709, 92-101, Conference: 2 Investigative image processing. Conference, Orlando FL
(United States), 4 Apr 2002

63. 3D measurements on extrusion marks in plastic bags, Berx V (Reprint); De Kinder J,

JOURNAL OF FORENSIC SCIENCES, (SEP 2002) Vol. 47, No. 5, pp. 976-985.

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65. A 3D view on the 'crossing lines' problem in document investigation, Investigative

image processing II : Orlando FL, 4 April 2002, BERX Veerle; De Kinder Jan, SPIE
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66. Tracing the source of a shredded document., Brassil, J. (Hewlett Packard Labs., Palo
Alto, CA, USA), Information Hiding. 5th International Workshop, IH 2002. Revised
Papers (Lecture Notes in Computer Science Vol.2578), Editor(s): Petitcolas, F.A.P.,
Berlin, Germany: Springer Verlag, 2002. p.387-99 of vi+426 pp. Conference:
Noordwijkerhout, Netherlands, 7-9 Oct 2002

67. Computer vision techniques for semi-automatic reconstruction of ripped-up

documents, De Smet, P.; Johan De Bock; Corluy, E. (Dep. TELIN/TWO7, Ghent
Univ., Belgium), Proceedings of the SPIE - The International Society for Optical
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Conference: Visual Information Processing XII. Orlando, FL, USA, 21 April 2003

68. A computer-based system to support forensic studies on handwritten documents.,

Franke, K.; Koppen, P. (Dept. of Pattern Recognition, Fraunhofer Inst. for Production
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69. Proceedings of the first international meeting on the Reconstruction of soft tissues in
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70. Facial 3d reconstruction, Eliasova H (Reprint); Dvooak D; Prochazka O, FORENSIC

SCIENCE INTERNATIONAL, (SEP 2003) Vol. 136, Supp. [1], pp. 177-178.

71. The application of anthropometric indices in forensic photography: Three case studies.
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72. From the skull to the face: inverse 3D-simulation in archaeology and forensic
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Simulation Symposium 2000. ESS'2000, Editor(s): Moller, D.P.F. San Diego, CA,
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Sept 2000

73. Improved vision in forensic documentation: forensic, 3D/CAD-supported

photogrammetry of bodily injury external surfaces, combined with volumetric
radiologic scanning of bodily injury internal structures, provides more investigative
leads and stronger forensic evidence., Thali, M.J; Braun, M.; Kneubuehl, B.P.;
Brueschweiler, W.; Vock, P.; Dirnhofer, R., Proceedings of the SPIE - The
International Society for Optical Engineering (2000) vol.3905, p.213-21. Conference:
28th AIPR Workshop: 3D Visualization for Data Exploration and Decision Making.
Washington, DC, USA, 13-15 Oct 1999

204
74. Bite mark documentation and analysis: the forensic 3D/CAD supported
photogrammetry approach, Thali M. J.; Braun M.; Markwalder Th. H.;
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science international, (2003), 135(2), 115-121

75. Estimation of age from human renal tissues by image processing. Furutani A; Tatsumi
S; Sugiyama S, Acta Med Kinki Univ, (2001) vol. 26, no. 1, pp. 7-17.

76. Optical 3D surface digitizing in forensic medicine: 3D documentation of skin and

bone injuries, Thali Michael J.; Braun Marcel; Dirnhofer Richard, Forensic science
international, (2003), 137(2-3), 203-208

77. Development of a prototype automated system for forensic hair comparison and
analysis using neural networks, Verma M S (Reprint); Pratt L; Ganesh C; Medina C,
FORENSIC SCIENCE INTERNATIONAL, (SEP 2003) Vol. 136, Supp. [1], pp. 116-
117.

78. Background correction in forensic photography I. Photography of blood under

conditions of non-uniform illumination or variable substrate color - Theoretical
aspects and proof of concept, Wagner J H; Miskelly G M (Reprint), JOURNAL OF
FORENSIC SCIENCES, (MAY 2003) Vol. 48, No. 3, pp. 593-603.

79. Definitions and Guidelines for the Use of Imaging Technologies in the Criminal
Justice System" (General Overview of Imaging in Law Enforcement) or revised draft
at "Guidelines for Field Applications of Imaging Technologies" (includes info on Film
vs. Digital Cameras)

80. "Recommendations and Guidelines for the Use of Digital Image Processing in the
Criminal Justice System"

81. "Considerations for Managers" (High level advice for labs considering moving to
digital imaging systems)

82. "General Guidelines for Capturing Latent Impressions Using a Digital Camera"

83. "Guidelines and Recommendations for Training in Imaging Technologies in the

Criminal Justice System"

84. "Definitions, Recommendations, and Guidelines for the Use of Forensic Video
Processing in the Criminal Justice System"

85. "General Guidelines for Photographing Footwear Impressions"

86. "General Guidelines for Photographing Tire Impressions"

205
CHEMICAL and MATERIAL
ANALYSIS

206
Research On Drug Evidence

— A Review: 2001 to 2004 —

Presented by: Robert F.X. Klein

Prepared by: Melanie E. Domagala, Robert F.X. Klein,

and Patrick A. Hays

U.S. Department of Justice

Drug Enforcement Administration
Office of Forensic Sciences
2401 Jefferson Davis Highway
Alexandria, Virginia 22301 USA
(Coordinating Office)

and

Special Testing and Research Laboratory

22624 Dulles Summit Court
Dulles, Virginia 20151 USA
(Coordinating Laboratory)

207
CONTENTS

General Overview (Talking Paper)

Routine and Improved Analyses of Abused Substances

Synthesis and/or Cultivation of Controlled Substances, their Precursors, and

Essential Chemicals

Clandestine Laboratories - Appraisals and Safety Issues

Reference Drug Standards and Total Syntheses

Source Determination of Drugs (Impurity Profiling), and Comparative Analyses

Analysis of Non-Controlled Pharmaceuticals, Pseudo-Drugs, Adulterants, Diluents,

and Precursors

New and/or Improved Analytical Techniques

Portable Detection and Analytical Instrumentation

Surveys and Miscellaneous Topics

Notes:
1. All categories are subdivided by topic or category, then alphabetically by the first
author’s name.
2. Where appropriate, a short explanatory note is added to the citation to provide additional
detail concerning the reference.
3. Note that the following references are law enforcement restricted, and not available to
the general public: Microgram and Microgram Bulletin prior to 2003, and the Journal of
the Clandestine Laboratory Investigating Chemists Association (all years).

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GENERAL OVERVIEW:

As the Symposium Delegates are well aware, production, trafficking, and use of illicit drugs are
not static situations, but rather are undergoing continuous change. Indeed, the worldwide
situation is significantly different since the last Symposium. The most noteworthy changes have
occurred with hallucinogenic compounds, the methylenedioxyamphetamines, methamphetamine
and related amphetamine type stimulants, heroin, cocaine, and the Internet.

The most dramatic changes have occurred with hallucinogenic compounds. Until recently, LSD
was the principal hallucinogen being used throughout the world. However, the arrests in the
United States of a number of individuals who were involved in the large-scale manufacture of
LSD, have apparently had a significant, negative impact on the production, availability, and use
of LSD, worldwide. Of all the reporting nations, only the United Kingdom reports significant
continuing use of LSD. In the United States and elsewhere, the seizures and reported use of
LSD have been in dramatic decline. The lack of supply has had several consequences in North
America and Europe: First, there have been increased seizures of small-scale, “amateur” LSD
laboratories, some of which included attempts to cultivate ergot fungi. More importantly, there
have been significant increases in the production, trafficking, and use of alternative
hallucinogens, including "designer" tryptamines, "designer" dimethoxylated phenethylamines,
psilocybin mushrooms, and unusual plants such as salvia divinorum, ayahuasca, and various
species of mescaline-containing cacti. Over the past five years, more than two dozen designer
tryptamines and dimethoxylated phenethylamines have appeared in the drug markets. In
addition, many of the tryptamines and dimethoxylated phenethylamines that are not specifically
controlled have been openly produced and marketed by various commercial chemical firms.
Most of these compounds are featured in Alexander Shulgin’s textbooks, PIHKAL and
TIHKAL. Although recent enforcement efforts in the United States have closed down some of
the commercial operations producing these compounds, a number of firms outside the United
States are still marketing these compounds, and clandestine production of some of the more
popular drugs is being encountered in the United States and Europe. Mushroom spore kits and
cultivation instructions are available from multiple sources, both on the Internet and in
publications catering to drug users. As a result, psilocybin mushroom cultivation, trafficking,
and use have dramatically increased. Preparations of finely chopped or powdered psilocybin
mushrooms in chocolate have become popular in North America. Salvia divinorum, a
hallucinogenic plant native to Mexico and nearby areas that was relatively unknown just three
years ago, has become a significant abuse problem in the United States - but remains
uncontrolled. Preparations of marijuana and marijuana extracts in various candy-like and other
commercial products have greatly increased. Law enforcement and forensic laboratories are still
reacting to the rapid rise of these alternative hallucinogens, and these challenges are expected to
continue to increase in the near future.

Another drug category that has seen significant changes since the last Symposium is the
methylenedioxyamphetamines, generically known as Ecstasy. First, there has been a diaspora of
production laboratories worldwide. Although it is felt that most manufacture continues to be
based in northern Europe, major laboratories are now being seized in North America (United
States and Canada), and there have been reports of seizures of large laboratories elsewhere,
including Southeast Asia, South America, and South Africa. Second, there have been dramatic
increases in adulterated Ecstasy tablets and in Ecstasy tablet “mimics” over the past three years.
Primary adulterants/substitutes include methamphetamine, ketamine and phencyclidine,
amphetamine, various hallucinogenic dimethoxylated phenethylamines (2-CT-7, 2C-I, etc.),
piperazines (BZP and TFMPP), substituted amphetamines (PMA, PMMA, and 4-
methylthioamphetamine), GHB salts, etc. Reports of “Ecstasy” tablets that do not contain either
MDA or MDMA are now routine. Many of these tablets contain mixtures of two, three, or more

209
drugs. As an unexpected consequence of these adulterations and/or substitutions, law
enforcement agencies in North America reports sharp changes in behavior of arrestees at “Rave”
parties and similar events. Whereas previously the arrestees were often friendly and cooperative
under the influence of MDA or MDMA, they are now often paranoid and combative. Similarly,
emergency room personnel often have difficulty treating drug overdose victims because they are
under the influence of multiple, unknown drugs, and/or are psychotic and violent. There has
been a concurrent increase in “Ecstasy” overdose deaths (notably from PMA/PMMA, but also
others). This problem continues to worsen.

Another drug area in flux is methamphetamine and related amphetamine type stimulants
(ATS’s). In the United States, the synthesis of methamphetamine via active metal reductions
(lithium in anhydrous ammonia) has become a major method, but remains a “cottage industry”
at this time. The theft of anhydrous ammonia from farming and refrigeration supplies has
become epidemic in North America. Of serious concern, there have been a number of major
spills of anhydrous ammonia resulting from thefts or attempted thefts, but to date there have
been no Bhopal-like disasters. Efforts to adulterate anhydrous ammonia to make it unusable for
production of methamphetamine are ongoing. Iodine/phosphorous type laboratories are
somewhat in decline, but are still the primary method used by the so-called methamphetamine
“Superlabs”. Efforts to restrict the sale of over-the-counter ephedrine and pseudoephedrine
containing products are having some effect on both large-scale and small-scale laboratory
production within the U.S., and there are recent indications that the "Superlabs" in the American
Southwest are shifting back into Mexico/Central America. Production and use of "Ice"
methamphetamine (high purity d-methamphetamine hydrochloride in large crystal form) is
slowly increasing in the United States and around the Pacific Rim, including Australia.
Unusually, production of l-methamphetamine (the much less potent isomer of
methamphetamine) has appeared and is growing, both along the Pacific Rim and in the
American West. l-Methamphetamine has appeared both in large crystal form resembling "Ice"
methamphetamine, and also in methamphetamine and Ecstasy tablets. It is unclear if this
production is intentional or the result of chemically unsophisticated clandestine chemists
unknowingly purchasing and using d-ephedrine and l-pseudoephedrine. Production of so-called
"Thai Tabs" (small methamphetamine tablets that are produced primarily in Myanmar)
continues to increase in Southeast Asia, and increasing numbers of Thai Tabs are now being
encountered in the United States. Despite the fact that Thai Tabs are significantly smaller than
typical Ecstasy tablets and are intended for smoking purposes, unsophisticated users in North
America often ingest Thai Tabs as Ecstasy. Smuggling of freshly harvested khat from the
eastern Horn of Africa into Europe and North America continues to increase, and dried khat has
been encountered in the United States (drying apparently prevents decomposition of cathinone,
the active component). Finally, and very unusually, illicit production and use of methcathinone
has become a significant problem in South Africa.

The worldwide production, trafficking, and use of opium and heroin continues to increase.
After a brief hiatus, illicit opium production in Southwest Asia and South America are now at
all-time record levels. Most Southwest Asian heroin is sent to Europe, while most South
American heroin is sent to the United States. Southeast Asian opium is being increasingly
encountered in North America, where it is being consumed primarily in expatriate Asian
communities. However, Southeast Asian heroin is now mainly consumed in the Far East,
Australia, and Russia, and is not commonly encountered in North America. Of possible
concern, in 2003 the Australian authorities made a seizure of 75 kilograms of heroin from a
cargo vessel that signature analysis indicated to be of unknown origin. This suggests the
possibility of a new heroin production technique.

210
The production, trafficking, and use of cocaine are in flux. After nearly a decade of significant
declines, coca cultivation in Bolivia and Peru is slightly increasing. Colombia remains the
world's top producer of coca, with dramatic expansions of coca production throughout the
country over the past five years. Illicit production of cocaine continues to be continuously
modified in response to law enforcement initiatives to restrict essential production chemicals.
Use of pharmaceuticals to adulterate cocaine at the production stage is increasing. Production of
“crack” cocaine in South America for export is also increasing. Use of cocaine in the United
States has somewhat declined; however, cocaine use is increasing elsewhere, especially in
Europe. Use of "crack" cocaine is increasing in England and South Africa.

Although the discussed variations in drug production, trafficking and use have been significant,
the most important change is the involvement of the Internet in virtually all aspects of illicit
drugs. The Internet is now firmly entrenched as THE source for information on all aspects of
illicit drugs - production, use, concealment, smuggling techniques, methods to evade law
enforcement, methods to evade drug testing, and more. Several well established websites,
notably erowid, rhodium, and lycaeum, act as historical repositories and archives for a large
volume of drug related information, while a large number of "chat-rooms" and bulletin boards
provide constant updates and feedback from active users on current trends, new drugs,
problems, etc. As a result, previously sensitive information is now easily accessed, common
knowledge. Of particular concern is the issue of so-called "rogue pharmacies", which sell huge
volumes of subscription medications over the Internet with minimal or no medical evaluations
of the subscribers. The products include a wide variety of controlled substances such as
Oxycontin, Vicodin, Xanax, etc. Rogue pharmacies are also the source of a large percentage of
so-called "spam" email messages, where unsolicited advertisements are sent to tens of millions
of email accounts every day. Pharmaceutical abuse is the fastest growing drug problem in the
world. In addition, precursors, essential chemicals, and laboratory equipment are often sold on
Internet auction sites such as ebay and ubid, or on industrial surplus auction sites. It is unclear
how the free exchange of information via the Internet can be reconciled with legitimate social
concerns such as drug use. At present, it appears that imposed restrictions are ineffective, and
this problem will likely continue to grow as an increasing percentage of the World’s population
becomes conversant with the Internet.

From a forensic point of view, there are two fields that have experienced significant advances
over the past three years: Instrumentation and Signature Profiling. Over the past ten years,
Capillary Electrophoresis (CE) has evolved from a research instrument to a mainstream
technique. Over the past three years, benchtop CE instruments have started replacing High
Performance Liquid Chromatographs (HPLCs) in many forensic laboratories. Tandem
technique instruments - notably CE-Mass Spectrometers - have also become available. An older
technique that is slowly evolving into a potentially useful field tool is Raman Spectroscopy.
Raman has the potential to identify compounds through many types of plastic and glass
containers, thereby allowing rapid identifications of contents, without exposure. Other "Field
Instruments" include improved Ion Mobility Spectrometers (including IMS-Mass
Spectrometers), and miniaturized Gas Chromatograph-Mass Spectrometers. Improvements in
trace analysis, notably Isotope Ratio Mass Spectrometry (IRMS) and Inductively Coupled
Plasma Mass Spectrometry (ICP/MS) have greatly enhanced drug profiling, especially for
geographical sourcing of cocaine and to a lesser extent heroin, and for synthetic route
determination of the amphetamine type stimulants and the methylenedioxyamphetamines.
These efforts have significantly enhanced the abilities of law enforcement to monitor and track
developing trends in production and trafficking of controlled substances. Finally, DNA analysis
has been applied for profiling of cannabis; however, it is unclear what impact these analyses will
have on geo-sourcing of cannabis.

211
ROUTINE AND IMPROVED ANALYSIS OF ABUSED SUBSTANCES

Issue:

Improved methods of analysis, i.e., faster, more discriminatory, more sensitive, less costly, etc.,
are needed for all abused substances. Additionally, standard analytical data are required for
previously unknown or rarely encountered substances and/or new homolog or analog (i.e.,
"designer"-type) drugs.

Solution:

Drug seizures and clandestine laboratory operations are continuously monitored to provide a
comprehensive overview of new developments. Ongoing research in the forensic community,
as well as in the general field of analytical chemistry, provide new and/or improved methods of
analysis for both routine and specialized analyses of seized drugs. Reports providing standard
analytical data for new drugs of abuse and/or improved analytical protocols for known drugs of
abuse are generated for the forensic and enforcement communities.

SYNTHESIS AND/OR CULTIVATION OF ABUSED SUBSTANCES, THEIR

PRECURSORS, AND ESSENTIAL CHEMICALS

Issue:

Forensic chemists must maintain familiarity with existing and new clandestine syntheses of
abused substances, their precursors, and essential chemicals, and with the cultivation of abused
natural products, in order to assist enforcement activities, to ensure safety and effectiveness
during enforcement operations, and to provide expert testimony in legal proceedings.

Solution:

Illicit drug seizures, clandestine laboratory operations, and illicit grow operations, are
continuously monitored to maintain a comprehensive overview of the field. In cases where new
drugs are synthesized, or new methodologies are utilized, case reports are generated for the
forensic and enforcement communities.

CLANDESTINE LABORATORIES - APPRAISALS AND SAFETY

Issue:

Forensic chemists must maintain familiarity with clandestine laboratory procedures, setups, and
techniques in order to assist enforcement activities, to ensure safety and effectiveness during
enforcement operations, and in order to provide expert testimony in court proceedings.

Solution:

Clandestine laboratory operations are continuously reviewed to provide a comprehensive

overview of the field. In cases where new methodologies are noted, or unusual safety concerns
are salient, reports are generated for the forensic and enforcement communities.

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REFERENCE DRUG STANDARDS AND TOTAL SYNTHESES

Issue:

Many reference drug standards or structurally related internal standards are either commercially
unavailable, or if available are extremely expensive.

Solution:

Controlled substances and their structural or isotopically labelled analogs are synthesized as
needed. Internal standards are also prepared as needed. Case reports are published for new or
unusual standards or improved synthetic approaches.

SOURCE DETERMINATION OF DRUGS (IMPURITY PROFILING) AND

COMPARATIVE ANALYSES

Issues:

Impurity profiling of drugs is important for comparative analysis protocols, geo-sourcing, and
synthetic route determinations. However, although certain drugs have been well characterized
with respect to their impurity profiles, most have not been properly investigated.

Comparative analysis (i.e., the systematic application of impurity profiling for determination of
commonality of origin) is complicated due to both the high complexity of the data and the large
numbers of exhibits. Improved analytical and data handling techniques are needed.

Solution:

High sensitivity analytical techniques (primarily chromatographic) provide detailed profiles of

trace-level impurities, ions, trace metals, and stable isotopes. Identification of individual
impurities enhance origin identification and comparative analyses and also aid in development
of internal standards for improved accuracy and precision of analysis.

In-depth analysis via improved instrumental methodologies help identify discriminatory

components in impurity profiles. Computer databases, sorting programs, and pattern
recognition/neural networks provide enhanced data handling and analysis, enabling and
improving comparative analyses.

Case reports are generated for the forensic and enforcement communities.

ANALYSIS OF NON-CONTROLLED PHARMACEUTICALS, PSEUDO-DRUGS,

ADULTERANTS, DILUENTS, AND PRECURSORS

Issue:

Most "street-level" drugs are "cut" with various adulterants and diluents. Many of these cutting
agents are pharmaceutical products or precursors. Others are “carry-through” compounds
present in precursors (especially in cold remedy products). Separation and identification of
these extraneous materials can be tedious, especially in exhibits which contain many
components. In addition, new or unusual adulterants and/or diluents are occasionally identified
in drug exhibits, and standard analytical data are required for these substances. Finally,

213
improved methods of analysis, i.e., faster, more discriminatory, less costly, etc., are needed for
all cutting agents.

NEW AND/OR IMPROVED INSTRUMENTAL TECHNIQUES

Issue:

Forensic Chemists must maintain familiarity with updates in current instrumental techniques and
become versant in new, improved methods of analysis.

Solution:

Improved/existing and new technologies are reviewed and applied to both routine and
specialized analyses of drugs. In cases where improved performance is observed, case reports
are generated for the forensic community.

PORTABLE DETECTION AND ANALYTICAL INSTRUMENTATION

Issue:

“Free Trade” agreements and the easing of formally restrictive national and international
borders have resulted in dramatic increases in cargo transshipments and personal travel, thereby
complicating drug inspection and interdiction efforts at POEs. Discovery and confirmational
analysis of suspected drugs in cargo or on individuals is severely hampered by the lack of on-
site detection and/or analytical equipment.

Solution:

Development of portable and highly sensitive detectors for drug detection and analyses allows
law enforcement personnel and/or forensic chemists to perform screening type analyses on-site.
In those cases where new methodologies have proven effective, case reports are generated for
the forensic and enforcement communities.

REFERENCES

Routine and improved analysis of abused substances

Reviews:

1) Brettell TA, Rudin N, Saferstein R. Forensic science. Analytical Chemistry

2003;75(12):2877. [A two year review of the forensic science literature.]

2) Christian DR Jr. Analysis of controlled substances. Forensic Science 2003:375. [A

review of the title topic (forensic emphasis). This is a CRC Press publication.]

3) Cole MD, Linacre AMT. The identification of controlled plant drugs using
phytochemistry and DNA. Current Topics in Phytochemistry 2002;5:129. [A minor
review of the title topic, focusing on marijuana, catha edulis, papaver somniferum, and
erythroxylum.]

4) Dal Cason TA, Franzosa ES. Occurrences and forms of the hallucinogens. Hallucinoge

214
5) ns 2003:37. [A review, including LSD and its analogs, indoalkylamines, hallucinogenic
phenethylamines, PCP and its analogs, ketamine, and beta-carbolines.]

6) Hugel J, Meyers J, Lankin D. Analysis of the hallucinogens. Hallucinogens 2003:191.

[A review of the forensic analysis of hallucinogens.]

7) Klein RFX, Hays PA. Detection and analysis of drugs of forensic interest, 1992 - 2001;
A literature review. Microgram Journal 2003;1(1-2):55. [A ten year review of the
forensic science literature.]

Scientific Working Group for Forensic Analysis of Illicit Drugs:

8) Bono JP. Report of the Scientific Working Group for the Analysis of Seized Drugs
(SWGDRUG) Conference. Microgram Journal 2003;1(3-4):208. [A summary of the
Conference’s findings and recommendations.]

9) Bono JP, Janovsky TJ. Scientific Working Group for the Analysis of Seized Drugs
(SWGDRUG) – Update. Proceedings of the American Academy of Forensic Sciences
2004;10:67. [An update of the accomplishments and objectives of the SWGDRUG.]

10) Janovsky TJ, Bono JP. Scientific Working Group for the Analysis of Forensic Drug
Samples (SWGDRUG) – Update 2002. Proceedings of the American Academy of
Forensic Sciences 2002;8:30. [An update of the accomplishments and objectives of the
SWGDRUG.]

Amphetamine, Methamphetamine, and Dimethylamphetamine (see also Substituted

Amphetamines, Phenethylamines, and Methylenedioxyamphetamines):

11) Brown H, Kirkbride KP, Pigou PE, Walker GS. New developments in SPME, Part 1:
The use of vapor-phase deprotonation and on-fiber derivatization with
alkylchloroformates in the analysis of preparations containing amphetamines. Journal of
Forensic Sciences 2003;48(6):1231. [Presents a method for conversion of solid drug
salts to their free bases, capture via SPME, and analysis by GC/MS. The technique can
be used for noninvasive recovery from consumer items such as banknotes and garments.
Use of on-fiber derivatization with alkylchloroformates improves chromatography and
also allows for enantiomer determinations.]

12) Chan KB, Chong YK, Nazarudin M. The identification of N,N-dimethyl-amphetamine

(DMA) in an exhibit in Malaysia. Microgram Journal 2003;1(3-4):162. [Presents the
title analysis, using color tests, GC/MS, FTIR, HPLC, melting point, and optical
rotation.]

13) Faulds K, Smith WE, Graham D, Lacey RJ. Assessment of silver and gold substrates for
the detection of amphetamine sulfate by surface enhanced Raman Scattering (SERS).
Analyst 2002;127(2):282.

14) Herraez-Hernandez R, Campins-Falco P, Verdu-Andres J. Strategies for the

enantiomeric determination of amphetamine and related compounds by liquid
chromatography. Journal of Biochemical and Biophysical Methods 2002;54(1-3):147.
[Presents a review of recent advances in the title field, with an emphasis on biological
samples.]

215
15) Liau AS, Liu JT, Lin LC, Chiu YC, Shu YR, Tsai CC, Lin CH. Optimisation [sic] of a
simple method for the chiral separation of methylamphetamine and related compounds in
clandestine tablets and urine samples by beta-cyclodextrin modified capillary
electrophoresis: A complementary method to GC-MS. Forensic Science International
2003;134(1):17. [Compounds include methamphetamine, methcathinone, ephedrine, and
pseudoephedrine. The focus is toxicological.]

16) Lua AC, Chou TY. Preparation of immunoaffinity columns for direct enantiomeric
separation of amphetamine and/or methamphetamine. Journal of Chromatography A
2002;967(2):191. [For direct enantiomeric determination of amphetamine and
methamphetamine in urine.]

17) Matsushima K, Nagai T, Nihei H, Kikuchi F, Tokudome S. Analysis of a new type of

tablet containing l-(-)-methylamphetamine. Japanese Journal of Science and Technology
for Identification. 2003;8(1):99. [Presents the analysis of the referenced tablet (which
also included ketamine and caffeine).]

18) Wang S-M, Liu RH. Solid-phase microextraction based approach for enantiomeric
analysis of amphetamines. Proceedings of the American Academy of Forensic Sciences
2004;10:72. [Diastereomers were created via derivatization with S-(-)-N-trifluoroacetyl-
prolyl chloride, followed by isolation with SPME, followed by analysis.]

para-Substituted Amphetamines:

19) Dal Cason TA. A re-examination of the mono-methoxy positional ring isomers of
amphetamine, methamphetamine, and phenyl-2-propanone. Forensic Science
International 2001;119(2):168.

20) Mortier KA, Dams R, Lambert WE, De Letter EA, Van Calenbergh S, De Leenheer AP.
Determination of para-methoxyamphetamine and other amphetamine-related designer
drugs by liquid chromatography/sonic spray ionization mass spectrometry. Rapid
Communications in Mass Spectrometry 2002 16(9):865. [For analysis of tablets,
powders, or aqueous solutions.]

Barbiturates:

21) Bartzatt R. Determination of barbituric acid, utilizing a rapid and simple colorimetric
assay. Journal of Pharmaceutical and Biomedical Analysis 2002;29(5):909. [Presents
three assay methods, which can be utilized on either aqueous or solid samples.]

22) Chang W-T, Smith J, Liu RH. Isotopic analogs as internal standards for quantitative
GC/MS analysis - Molecular abundance and retention time differences as interference
factors. Journal of Forensic Sciences 2002;47(4):873. [Isotopic analogues of five
barbiturates were evaluated as internal standards for GC/MS analyses.]

23) Forgacs E, Cserhati T, Miksik I, Echardt A, Deyl Z. Simultaneous effect of organic

modifier and physicochemical parameters of barbiturates on their retention on a narrow-
bore PGC column. Journal of Chromatography B - Analytical Technologies in the
Biomedical and Life Sciences 2004;800(1-2):259. [Presents the analysis of 22
barbiturates on a narrow-bore porous graphitized carbon column using water-dioxane
mobile phases.]

216
24) Jones, JJ, Kidwell H, Games DE. Application of atmospheric pressure chemical
ionisation [sic] mass spectrometry in the analysis of barbiturates by high speed analytical
countercurrent chromatography. Rapid Communications in Mass Spectrometry
2003;17(14):1565. [Presents the analysis of four barbiturates (barbital, allobarbital,
phenobarbital, and butalbital) using the title technique.]

25) Kepczynska E, Bojarski J, Pyka A. Lipophilicity of barbiturates determined by TLC.

Journal of Liquid Chromatography and Related Technologies 2003;26(19):3277.
[Thirteen 5,5-disubstituted derivatives of barbituric acid were analyzed by RP-TLC.]

Benzodiazepines:

26) Aebi B, Sturny-Jungo R, Bernhard W, Blanke R, Hirsch R. Quantitation using GC-TOF-

MS: Example of bromazepam. Forensic Science International 2002;128(1-2):84.
[Various methods are used to validate the use of GC-TOF-MS for analysis of
bromazepam; diazepam and nordazepam were also studied, but to a lesser extent.]

27) Bakavoli M, Kaykhaii M. Quantitative determination of diazepam, nitrazepam and

flunitrazepam in tablets using thin-layer chromatography - densitometry technique.
Journal of Pharmaceutical and Biomedical Analysis 2003;31(6):1185. [Also includes
and contrasts HPLC analyses; UV (254 nm) detection was used for both techniques.]

28) Benson A, Rose S, Hsu Y, Furton KG, Sabucedo A. LC/MS analysis of flunitrazepam
(Rohypnol) solid dosage tablets. Proceedings of the American Academy of Forensic
Sciences 2004;10:78.

29) Cahours X, Cherkaoui S, Rozing G, Veuthey JL. Microemulsion electrokinetic

chromatography versus capillary electrochromatography-UV-mass spectrometry for the
analysis of flunitrazepam and its major metabolites. Electrophoresis 2002;23(14):2320.
[Flunitrazepam and its three major metabolites (in biological fluids) were separated by
the title technique.]

30) Ferreyra CF, Ortiz CS. Simultaneous spectrophotometric determination of

phenylpropanolamine HCl, caffeine and diazepam in tablets. Journal of Pharmaceutical
and Biomedical Analysis 2002;29(5):811. [UV spectrophotometry and LC methods
were used.]

31) Kamande MW, Kapnissi CP, Zhu XF, Akbay C, Warner IM. Open-tubular capillary
electrochromatography using a polymeric surfactant coating. Electrophoresis
2003;24(6):945. [The title technique was applied to the analysis of benzodiazepines (not
specified in the abstract).]

32) Pirnay S, Ricordel I, Libong D, Bouchonnet S. Sensitive method for the detection of 22
benzodiazepines by gas chromatography - ion trap tandem mass spectrometry. Journal of
ChromatographyA 2002;954:235. [The title technique method was applied to biological
samples.]

33) Saelzer R, Gody G, Vega M, De Diego M, Godoy R, Rios G. Instrumental planar

chromatographic determination of benzodiazepines: Comparison with liquid
chromatography and gas chromatography. JAOAC International 2001;84(4):1287.

217
34) Suzuki Y, Arakawa H, Maeda M. The capillary electrophoresis separation of
benzodiazepine drugs using dextran sulfate and SDS as running buffer. Biomedical
Chromatography 2004;18(3):150. [Presents the EKC analysis of 10 benzodiazepines
(not specified in abstract). The authors claim that the presented method may also be used
for many other pharmaceuticals.]

Dimethoxyphenethylamines:

35) Cole MD, Lea C, Oxley N. 4-Bromo-2,5-dimethoxyphenethylamine (2C-B): A review

of the public domain literature. Science Justice 2002;42(4):223. [An overview of the
title compound, including a minor review of the available literature.]

36) Curtis B, Kemp P, Harty L, Choi C, Christensen D. Postmortem identification and

quantitation of 2,5-dimethoxy-4-n-propylthiophenethylamine using GC-MSD and GC-
NPD. Journal of Analytical Toxicology 2003;27(7):493. [Primary focus is analysis of
biological fluids and tissue samples; however, includes a small scale mass spectra (from
GC/MS) of the title compound (i.e., 2C-T-7).]

Chlordiazepoxide:

37) EHefnawey GB, ElHallag IS, Ghoneim EM, Ghoneim MM. Voltammetric behavior and
quantification of the sedative-hypnotic drug chlordiazepoxide in bulk form,
pharmaceutical formulation, and human serum at a mercury electrode. Journal of
Pharmaceutical and Biomedical Analysis 2004;34(1):75. [Includes comparisons against
existing methods.]

Clenbuterol:

38) Chankvetadze B, Lomsadze K, Bergenthal D, Breitkreutz J, Bergander K, Blaschke G.

Mechanistic study on the opposite migration order of clenbuterol enantiomers in capillary
electrophoresis with beta-cyclodextrin and single isomer heptakis(2,3-diacetyl-6-sulfo)-
beta-cyclodextrin. Electrophoresis 2001;22(15):3178.

39) Garcia-Ruiz C, Marina ML. Fast enantiomeric separation of basic drugs by electrokinetic
chromatography. Application to the quantitation of terbutaline in a pharmaceutical
preparation. Electrophoresis 2001;22(15):3191. [Includes clenbuterol.]

40) Ozkan Y, Ozkan SA, AboulEnein HY. Determination of clenbuterol HCl in human
serum, pharmaceuticals, and in drug dissolution studies by RP-HPLC. Journal of Liquid
Chromatography and Related Technologies 2001;24(5):679.

Cocaine:

41) Cabovska B, Norman AB, Stalcup AM. Separation of cocaine stereoisomers by capillary
electrophoresis using sulfated cyclodextrins. Analytical and Bioanalytical Chemistry
2003;376(1):134.

42) Koulis CV, Reffner JA, Bibby AM. Comparison of transmission and internal reflection
spectra of cocaine. Journal of Forensic Science 2001;46(4):822. [Study is on cocaine
hydrochloride; includes cautionary notes on the use of ATR.]

218
43) Rofael HZ, AbdelRahman MS. Development and validation of a high-performance
liquid chromatography method for the determination of cocaine, its metabolites and
ketamine. Journal of Applied Toxicology 2002;22(2):123.

44) Swiatko J, De Forest PR, Zedeck MS. Further studies on spot tests and microcrystal tests
for identification of cocaine. Journal of Forensic Sciences 2003;48(3):581. [Presents a
study of the Wagner, Marquis, and cobalt thiocyanate spot tests, and the gold chloride
and platinic chloride microcrystal tests, for the identification of cocaine.]

Ergot Alkaloids (see also LSD):

45) Stahl M, Jakob A, von Brocke A, Nicholson G, Bayer R. Comparison of different setups
for one- and two-dimensional capillary high-performance liquid chromatography and
pressurized capillary electrochromatography coupled on-line with mass spectrometry.
Electrophoresis 2002;23(17):2949. [Presents a comparison of different separation
methods (HPLC, capillary HPLC, and pressurized capillary electrochromatography
(pCEC)) coupled on-line with mass spectrometry (MS)) for the separation of a crude
extract of ergot fungus (secalis cornuti).]

Fentanyl(s):

46) DeBoer D, Goemans WPJ, Ghezavat VR, vanOoijen RD, Maes RAA. Seizure of illicitly
produced para-fluorofentanyl: Quantitative analysis of the content of capsules and
tablets. Journal of Pharmaceutical and Biomedical Analysis 2003;31(3):557. [Presents a
GC/MS methodology for the title analysis; HPLC/UV was also used to quantify caffeine
being used as an adulterant. The samples derived from an illicit laboratory in the
Netherlands.]

47) Jimeno ML, Alkorta I, Cano C, Jagerovic N, Goya P, Elguero J, FocesFoces C. Fentanyl
and its analogue N-(1-phenylpyrazol-3-yl)-N-[2-phenylethyl-4-piperidyl]propanamide:
H-1 and C-13 NMR spectroscopy, X-ray crystallography, and theoretical calculations.
Chemical and Pharmaceutical Bulletin 2003;51(8):929. [The oxalate salts and free bases
of the title compounds were analyzed by the title techniques.]

48) Van Nimmen NFJ, Veulemans HAF. Development and validation of a highly sensitive
gas chromatographic - mass spectrometric screening method for the simultaneous
determination of nanogram levels of fentanyl, sufentanil, and alfentanil in air and surface
contamination wipes. Journal of Chromatography A 2004;1035(2):249. [Focus is on
sampling for industrial occupational exposure. The technique uses SIM.]

Flos Daturae:

49) Ye NS, Zhu RH, Gu XX, Zou H. Determination of scopolamine, atropine and
anisodamine in Flos daturae by capillary electrophoresis. Biomedical Chromatography
2001;15(8):509.

Fluoxetine (Prozac):

50) Olsen BA, Borer MW, Perry FM, Forbes RA. Screening for counterfeit drugs using near-
infrared spectroscopy. Pharmaceutical Technology North America 2002;26(6):62.
[Uses NIR to screen and differentiate Prozac vs. many generic formulations.]

219
Heroin:

51) Dongre VG, Kamble VW. HPTLC detection and identification of heroin
(diacetylmorphine) in forensic samples. Part III. Journal of Planar Chromatography -
Modern TLC 2003;16(6):458. [Presents a new spray reagent for detection of heroin and
similar opium alkaloids after TLC elution.]

52) Fitsev IM, Budnikov GK, Blokhin VK, Teslenko PG. Gas chromatographic
determination of diacetylmorphine with mass spectrometric detection. Journal of
Analytical Chemistry (English translation of Zhurnal Analiticheskoi Khimii) 2003;47(9-
12):423. [Appears to be a GC/MS method for analysis of heroin in fluids (not clear in
abstract).]

53) Kulikowska J, Celinski R, Soja A, Sybirska H. Investigations on the quality of home-

made poppy straw products (“Compote”) at the forensic medicine department in
Katowice. Proceedings, 39th Annual TIAFT Meeting, Prague, 2001. [Illicit production of
morphine and heroin in Poland (from poppy straw) is reviewed, and the techniques used
for analysis of these products are discussed.]

54) Lurie IS, Hays PA, Garcia AE, Panicker S. Use of dynamically coated capillaries for the
determination of heroin, basic impurities, and adulterants with capillary electrophoresis.
Journal of Chromatography A 2004;1034(1-2):227.

55) Macchia M, Manetto G, Mori C, Papi C, Di Pietro N, Salotti V, Bortolotti F, Tagliarro F.

Use of beta-cyclodextrin in the capillary zone electrophoretic separation of the
components of clandestine heroin preparations. Journal of Chromatography A
2001;924(1):499.

gamma-Hydroxybutyric Acid (GHB), gamma-butyrolactone (GBL) and 1,4-butanediol (BD):

56) Alston WC, Ng K. Rapid colorimetric screening test for gamma-hydroxybutyric acid
(Liquid X) in human urine. Forensic Science International 2002;126(2):114. [Based on
the ferric hydroxamate test for ester detection; takes 5 minutes and has a detection limit
0.1 mg/mL for 1 mL samples.]

57) Bishop SC, McCord BR, Svec F. Analysis of GHB and its analogs by capillary
electrochromatography. Proceedings of the American Academy of Forensic Sciences
2002;8:268. [Includes analysis of GHB, GBL. BD, and gamma-aminobutyric acid
(GABA).]

58) Bravo DT, Harris DO, Parsons SM. Reliable, sensitive, rapid, and quantitative enzyme-
based assay for gamma-hydroxybutyric acid (GHB). Journal of Forensic Sciences
2004;49(2):379. [Several assays are presented for detection of GHB in beverages and
urine.]

59) Chappell JS. The non-equilibrium aqueous solution chemistry of gamma-hydroxybutyric

acid. Journal of the Clandestine Laboratory Investigating Chemists Association
2002;12(4):20. [Presents a study of the chemistry of GHB in aqueous solutions.]

220
60) Chappell JS, Meyn AW, Ngim KK. The extraction and infrared identification of gamma-
hydroxybutyric acid (GHB) from aqueous solutions. Journal of Forensic Sciences
2004;49(1):52. [Presents a liquid-liquid extraction technique for isolating GHB free acid,
with analysis by IR.]

61) Chew SL, Meyers JA. Identification and quantitation of gamma-hydroxybutyrate

(NaGHB) by nuclear magnetic resonance spectroscopy. Journal of Forensic Sciences
2003;48(2):292. [Presents an NMR technique for identification and quantitation of GHB;
the identification of GBL by NMR is also presented.]

62) Ciolino LA, Mesmer MZ, Satzger RD, Machal AC, McCauley HA, Mohrhaus AS. The
chemical interconversion of GHB and GBL: Forensic issues and implications. Journal of
Forensic Sciences 2001;46(6):1315.

63) Dahlen J, Vriesman T. Simultaneous analysis of gamma-hydroxybutyric acid, gamma-

butyrolactone, and 1,4-butanediol by micellar electrokinetic chromatography. Forensic
Science International 2002;125(2-3):113.

64) DeFrancesco JV. An NMR study of the stability of gamma-butyrolactone (GBL) in

water. Proceedings of the American Academy of Forensic Sciences 2003;9:32.
[Presents a study of the conversion of GBL to GHB over time, starting with different
concentrations of GBL.]

65) Duer WC, Byers KL, Martin JV. Application of a convenient extraction procedure to
analyze gamma-hydroxybutyric acid in fatalities involving gamma-hydroxybutyric acid,
gamma-butyrolactone, and 1,4-butanediol. Journal of Analytical Toxicology
2001;25(7):576.

66) Garcia AD, Catterton AJ. 1,4-Butanediol (BD) - Forensic profile. Microgram Journal
2003;1(1-2):44.

67) Meyers JE, Garcia AD, Almirall JR. The analysis of gamma-hydroxybutyric acid (GHB)
and gamma-butyrolactone (GBL) in forensic samples using GC/MS and H1-NMR.
Proceedings of the American Academy of Forensic Sciences 2003;9:30. [Presents the
referenced analyses, and also discusses the interconversion between the two substrates.
SPME was utilized to recover the substrates for analysis.]

68) Meyers JE, Almirall JR. The analysis of gamma-hydroxybutyric acid (GHB) and
gamma-butyrolactone (GBL) in forensic samples using gas chromatography/mass
spectrometry (GC/MS) and proton nuclear magnetic resonance (H1-NMR). Proceedings
of the American Academy of Forensic Sciences 2004;10:57. [Further investigates the
interconversion between GHB and GBL, and presents a procedure for avoiding
interconversion prior to analysis.]

69) Negrusz A, Cooper FJ, LeBeau MA, Marinetti LJ, Borgen LA, Zvosek DL, Smith SW.
GHB: Old substance, new problem. Proceedings of the American Academy of Forensic
Sciences 2002;8:10. [A workshop presenting a comprehensive overview of the title
compound.]

221
70) Parsons SM, Harris DO, Bravo DT. Methods, compositions and apparatuses for detection
of gamma-hydroxybutyric acid (GHB). U.S. Pat. Appl. Publ. US 2003 175,846 (Cl. 435-
25; C12Q1/26), 18 Sep 2003, Appl. 98,811, 14 Mar 2002. [Presents a method for
detecting GHB using a biochemical reaction.]

71) Smith JV. Method for detection of 4-hydroxybutyric acid and its precursor(s) in fluids.
U.S. US 6,617,123 (Cl. 435-19; C12Q1/44), 9 Sep 2003, Appl 607,026, 29 Jun 2000.
[Appears to be a detection method for adulterated beverages (not biological fluids).]

72) Sabucedo AJ, Furton KG. Extractionless GC/MS analysis of gamma-hydroxybutyrate

and gamma-butyrolactone with trifluoroacetic anhydride and heptafluoro-1-butanol from
aqueous samples. Proceedings of the American Academy of Forensic Sciences
2004;10:109. [GHB can be derivatized directly in water solutions, without organic
solvent extraction needed. GABA, diethylene glycol, BD, and GBL were analyzed under
the same conditions (GBL gave a small response from conversion to GHB).]

73) Tanaka E, Terada M, Shinozuka T, Honda K. gamma-Hydroxybutyric acid (GHB); its

pharmacology and toxicology. Japanese Journal of Forensic Toxicology 2003;21(3):210.
[An overview and brief review.]

74) Vose J, Tighe T, Schwartz M, Buel E. Detection of gamma-butyrolactone (GBL) as a

natural component in wine. Journal of Forensic Sciences 2001;46(5):1164.

75) Witkowski MR, Ciolino LA, DeFrancesco JV. GHB free acid: More on issues of
interconversion with isolation and spectroscopic characterization of forensic analysis.
Proceedings of the American Academy of Forensic Sciences 2003;9:30. [A forensic
profile of the free acid (versus the more commonly encountered base form) is presented
and discussed.]

76) Witkowski MR, Ciolino LA. Infrared (IR) spectroscopic identification of GHB free acid,
GHB salts, and GBL. Proceedings of the American Academy of Forensic Sciences
2003;9:31. [Includes an in-depth discussion.]

Ketamine:

77) Standifer SR, Kercheval JC. Special K and the K-hole. Analysis of ketamine. Mid-
Atlantic Association of Forensic Scientists Newsletter 2001;29(2):6.

Khat:

78) Kite GC, Ismail M, Simmonds MSJ, Houghton PJ. Use of doubly protonated molecules
in the analysis of cathedulins in crude extracts of khat (Catha edulis) by liquid
chromatography/serial mass spectrometry. Rapid Communications in Mass Spectrometry
2003;17(14):1553. [Analysis of fresh khat by LC/MS revealed 62 cathedulins.]

LSD:
79) Fang C, Liu JT, Lin CH. Optimization of the separation of lysergic acid diethylamide in
urine by a sweeping technique using micellar electrokinetic chromatography. Journal of
Chromatography B - Analytical Technologies in the Biomedical and Life Sciences
2002;775(1):37. [Presents the separation and analysis of LSD, iso-LSD, and LAMPA by
capillary electrophoresis - fluorescence spectroscopy using sodium dodecyl sulfate (SDS)
as an anionic surfactant.]

222
80) Fang C, Liu JT, Lin CH. On-line identification of lysergic acid diethylamide (LSD) in
tablets using a combination of a sweeping technique and micellar electrokinetic
chromatography/77 K fluorescence spectroscopy. Electrophoresis 2003;24(6):1025.
[Presents and contrasts the title analysis with standard GC/MS methods.]

81) Libong D, Bouchonnet S. Collision-induced dissociations of trimethylsilylated lysergic

acid diethylamide (LSD) in ion trap multiple stage mass spectrometry. International
Journal of Mass Spectrometry 2002;219(3):615. [Presents a highly sensitive GC/MS-MS
method for detection of LSD.]

Marijuana and Related Cannabinoids:

82) Alghanim HJ, Almirall JR. Development of microsatellite markers in Cannabis sativa
for DNA typing and genetic relatedness analyses. Analytical and Bioanalytical
Chemistry 2003;376(8):1225.

83) Coyle HM, Palmbach T, Juliano N, Ladd C, Lee HC. An overview of DNA methods for
the identification and individualization of marijuana. Microgram Journal 2003;1(3-
4):196. [Presents the title overview and review. Note that this article is a reprint from the
Croatian Medical Journal 2003;44(3):315.]

84) Fucci N. Growing cannabis with naphthalene in Rome. Forensic Science International
2003;138(1-3):91. [Presents the analysis of marijuana that was treated with naphthalene
as a pesticide in a moderate sized home grow operation (80 plants); naphthalene was
found in high concentration in the marijuana.]

85) Galand N, Emouf D, Montigny F, Dollet J, Pothier J. Separation and identification of

cannabis components by different planar chromatography techniques (TLC, AMD,
OPLC). Journal of Chromatographic Science 2004;42(3):130.

86) Gambaro V, Dell’Acqua L, Fare F, Froldi R, Saligari E, Tassoni G. Determination of

primary active constituents in cannabis preparations by high-resolution gas
chromatography/flame ionization detection and high-performance liquid
chromatography/UV detection. Analytica Chimica Acta 2002;468(2):245. [Presents a
comparative study between the two title techniques for the complete, quantitative analysis
of all the active constituents in cannabis. Validation studies were carried out on hashish.]

87) Gilmore S, Peakall R. Isolation of microsatellite markers in Cannabis sativa L.

(marijuana). Molecular Ecology Notes 2003;3(1):105. [Fifteen markers were identified
that can characterize genetic diversity in cultivated and natural marijuana populations.]

88) Gilmore S, Peakall R, Robertson J. Short tandem repeat (STR) DNA markers are
hypervariable and informative in Cannabis sativa: Implications for forensic
investigations. Forensic Science International 2003;131(1):65. [Presents a profiling
study of 93 individual cannabis plants of widespread origin, using 5 STR markers. The
authors claim that source determination is possible using the presented methods.]

89) Hsieh, H-M, Hou R-J, Tsai L-C, Wei C-S, Liu S-W, Huang L-H, Kuo Y-C, Linacre A,
Lee JC-I. A highly polymorphic STR locus in Cannabis sativa. Forensic Science
International 2003;131(1):53. [Reports the isolation of a short tandem repeat locus from
Cannabis sativa.]

223
90) Miller Coyle H, Shutler G, Abrams S, Hanniman J, Neylon S, Ladd C, Palmbach T, Lee
HC. A simple DNA extraction method for marijuana samples used in amplified fragment
length polymorphism (AFLP) analysis. Journal of Forensic Sciences 2002;48(2):343.
[Presents an AFLP technique for creating a DNA profile for different plant varieties.]

91) Szabady B, Hidvegi E, Nyiredy S. Determination of neutral cannabinoids in hemp

samples by overpressured-layer chromatography. Chromatographia 2002;56(Suppl.
S):S165. [The overpressured-layer chromatographic separation of neutral cannabinoids
(delta(9)-tetrahydrocannabinol, cannabidiol, cannabinol, cannabigerol and
cannabichromene) was achieved on amino HPTLC plates, using dichloromethane as the
mobile phase.]

92) Wojtasik E, Anyzewska M, Arent I. The optimization of the separation conditions for
cannabinoids from Cannabis sativa L. var. Indica and application of the method to
determine the content of delta(9)-tetrahydrocannabinol in plant material. Journal of
Liquid Chromatography and Related Technologies 2002;25(6):949.

Mescaline/Peyote:

93) Maloney DC. Extraction of mescaline from peyote. Microgram 2001;34(8):205.

Methadone:

94) Kelly T, Doble P, Dawson M. Chiral separation of methadone, 2-ethylidene-1,5-

dimethyl-3,3-diphenylpyrrolidine (EDDP) and 2-ethyl-5-methyl-3,3-diphenyl-1-pyrroline
(EMDP) by capillary electrophoresis using cyclodextrin derivatives. Electrophoresis
2003;24(12-13):2106. [Presents a stereoselective method for the simultaneous
determination of methadone and its two principal metabolites.]

Methylenedioxyamphetamines and Related Compounds:

95) Aalberg L, DeRuiter J, Noggle FT, Sippola E, Clark CR. Chromatographic and
spectroscopic methods of identification for the side-chain regioisomers of
3,4-methylenedioxyphenethylamines related to MDEA, MDMMA, and MBDB. Journal
of Chromatographic Science 2003;41(5):227. [Presents the synthesis and GC and
GC/MS analyses of ten closely related 3,4-methylenedioxyphenethyl-amines all having a
molecular weight of 207.]

96) Chan KB. A normal phase HPLC method for the quantitation of MDMA in illicit ecstasy
tablets. Microgram 2001;34(9):237.

97) Fang C, Chung Y-L, Liu J-T, Lin C-H. Rapid analysis of 3,4-methylenedioxy-
methamphetamine: A comparison of non-aqueous capillary electrophoresis/ fluorescence
detection with GC/MS. Forensic Science International 2002;125(2-3):142.

98) Huang YS, Liu JT, Lin LC, Lin CH. Chiral separation of 3,4-methylenedioxy-
methamphetamine and related compounds in clandestine tablets and urine by capillary
electrophoresis/fluorescence spectroscopy. Electrophoresis 2003;24(6):1097. [MDA
was also analyzed. Contrasts the title analysis with standard GC/MS methods.]

224
99) Kulikowska J, Celinski R, Soja A, Sybirska H. Identification study of tablets of unknown
composition originating from illicit drug sale. Z-Zagadnien-Nauk-Sadowych
2002;49:99. [A study of Ecstasy tablets by TLC, UV, HPLC-DAD, and MS.]

100) Piette V, Parmentier F. Analysis of illicit amphetamine seizures by capillary zone

electrophoresis. Journal of Chromatography A 2002;979:345. [Presents a CZE
methodology for analysis of typical drugs found in Ecstasy tablets]

101) Pizarro N, Liebaria A, Cano S, Joglar J, Farre M, Segura J, de la Torre R. Stereochemical

analysis of 3,4-methylenedioxymethamphetamine and its main metabolites by gas
chromatography/mass spectrometry. Rapid Communications in Mass Spectrometry
2003;17:330. [Presents a derivatization procedure, followed by GC/MS analysis. The
focus is for analysis of biological fluids].

102) Sagmuller B, Schwarze B, Brehm G, Schneider S. Application of SERS spectroscopy to

the identification of (3,4-methylenedioxy)amphetamine in forensic samples utilizing
matrix stabilized silver halides. Analyst 2001;126(11):2066.

103) Schneider RC, Kovar KA. Analysis of ecstasy with a monolithic reverse-phase column.
Chromatographia 2003;57(5-6):287. [Presents an HPLC method that analyzes for
amphetamine, MDMA, MDEA, and N-methyl-1-(3,4-methylene-dioxyphenyl)-2-
butanamine in suspected ecstasy tablets.]

104) Schneider RC, Kovar K-A. Analysis of ecstasy tablets: Comparison of reflectance and
transmittance near infrared spectroscopy. Forensic Science International 2003;134(2-
3):187. [Presents analyses of mixed composition tablets by the title techniques;
transmittance mode was found to be better than reflectance mode.]

Methylphenidate:

105) Denk OA, Watson DG, Skellern GG. Chiral analysis of methylphenidate and
dextromoramide by capillary electrophoresis. Journal of Chromatography B - Analytical
Technologies in the Biomedical and Life Sciences 2001;761(1):61.

106) Schneiderman E, Gratz SR, Stalcup AM. Optimization of preparative electrophoretic

chiral separation of Ritalin enantiomers. Journal of Pharmaceutical and Biomedical
Analysis 2002;27(3-4):639.

Morphine, Codeine, and Related Opium Alkaloids:

107) Baeyens WRG, VanderWeken G, Smet E, GarciaCampana AM, Remon JP. Comparison
of morphine and hydromorphone analysis on reversed phase columns with different
diameters. Journal of Pharmaceutical and Biomedical Analysis 2003;32(4-5):913.
[Presents the analysis of the title compounds by HPLC on 2, 3, and 4 mm i.d. RP columns
with UV detection.]

108) Barnett NW, Hindson BJ, Lewis SW, Jones P, Worsfold PJ. Soluble manganese(IV); A
new chemiluminescence reagent. Analyst 2001;126(10):1636. [Includes application for
trace detection of morphine and codeine.]

225
109) Dams R, Benijts T, Lambert WE, DeLeenheer AP. Simultaneous determination of in
total 17 opium alkaloids and opioids in blood and urine by fast liquid chromatography -
diode-array detection - fluorescence detection, after solid-phase extraction. Journal of
Chromatography B - Analytical Technologies in the Biomedical and Life Sciences
2002;773(1):53.

110) Degim T, Akay C, Buyukafsar K, Cevheroglu S. Simultaneous determination of codeine

and ethyl morphine HCl in tablet formulations using LC. Journal of Pharmaceutical and
Biomedical Analysis 2001;26(1):15.

111) Dinc E, Baleanu D, Onur F. Simultaneous spectrophotometric analysis of codeine

phosphate, acetylsalicylic acid, and caffeine in tablets by inverse least-squares and
principal component regression techniques. Analytical Letters 2002;35(3):545.

112) Garrido JMPJ, Delerue-Matos C, Borges F, Macedo TRA, Olivera-Brett AM.

Electroanalytical determination of codeine in pharmaceutical preparations. Analytical
Letters 2002;35(15):2487. [Presents a square wave voltametric (SWV) method and a
flow injection analysis system with electrochemical detection (FIA-EC) for determination
of codeine in various pharmaceutical preparations. Limitations with certain co-
ingredients (e.g., acetaminophen) are discussed.]

113) Hosztafi S, Noszal B. Determination of morphine and its derivatives, by means of

luminescence analysis. Acta Pharmaceutica Hungarica 2002;72(3):191. [A minor
review of the title topic.]

114) Hood DJ, Cheung HY. A chromatographic method for rapid and simultaneous analysis
of codeine phosphate, ephedrine HCl, and chlorpheniramine maleate in cough-cold syrup
formulation. Journal of Pharmaceutical and Biomedical Analysis 2003;30(5):1595.
[Presents a reversed phase HPLC with UV detection method for analysis of a cough-cold
syrup product.]

115) Kartal M. LC method for the analysis of paracetamol, caffeine and codeine
phosphate in pharmaceutical preparations. Journal of Pharmaceutical and Biomedical
Analysis 2001;26(5-6):857.

116) Martos NR, Diaz AM, Navalon A, Capitan-Vallvey LF. Spectrofluororimetric

determination of acetylsalicylic acid and codeine mixtures in pharmaceuticals. Analytical
Letters 2001;34(4):579.

117) Molina-Diaz A, Ramos-Martos N, Navalon A, Capitan-Vallvey LF. Simultaneous

determination of codeine and pyridoxine in pharmaceutical preparations by first
derivative spectrofluorimetry. JAOAC International 2002;85(4):861.

118) Ramos-Martos N, Aguirre-Gomez F, Molina-Diaz A, Capitan-Vallvey LF. Application

of liquid chromatography to the simultaneous determination of acetylsalicylic acid,
caffeine, codeine, paracetamol, pyridoxine, and thiamine in pharmaceutical preparations.
JAOAC International 2001;84(3):676.

119) Stubberud K, Forsberg A, Callmer K, Westerlund D. Partial filling micellar

electrokinetic chromatography optimization studies of ibuprofen, codeine and
degradation products, and coupling to mass spectrometry. Electrophoresis
2002;23(4):572.

226
120) Stubberud K, Callmer K, Westerlund D. Partial filling - micellar electrokinetic
chromatography optimization studies of ibuprofen, codeine and degradation products, and
coupling to mass spectrometry: Part II. Electrophoresis 2003;24(6):1008. [For analysis
of pharmaceutical preparations.]

121) Sun GX, Wang Y, Sun YQ. The quantitative determinations of glycyrrhizic acid,
glycyrrhetinic acid, morphine, and sodium benzoate in compound liquorice tablets by
HPCE. Journal of Liquid Chromatography and Related Technologies 2003;26(1):43.
[Presents a CZE/UV method to perform the title analysis.]

122) Zakaria P, Macka M, Haddad PR. Separation of opiate alkaloids by electrokinetic

chromatography with sulfated cyclodextrin as a pseudo-stationary phase. Journal of
Chromatography A 2003;985(1-2):493. [Presents an EKC method for separation of
morphine, thebaine, 10-hydroxythebaine, codeine, oripavine, and laudanine.]

Opiate Alkaloids:

123) Kuznetsov PE, Aparkin AM, Zlobin VA, Nazarov GV, Kosterin PV, Lyubun’ EV,
Shcherbakov AA. Analysis of opiates by spin-lattice relaxation techniques.
Pharmaceutical Chemistry Journal (English translation of Khimiko-Farmatsevticheskii
Zhurnal) 2002;36(6):331. [Presents the use of the title technique to detect opiates in
plasma.]

124) Pennanen K, Kotiaho T, Huikko K, Kostiainen R. Identification of ozone-oxidation

products of oxycodone by electrospray ion trap spectrometry. Journal of Mass
Spectrometry 2001;36(7):791.

Opium (and Opium Poppies):

125) Lurie IS, Panicker S, Hays PA, Garcia AD, Geer BL. Use of dynamically coated
capillaries with added cyclodextrins for the analysis of opium using capillary
electrophoresis. Journal of Chromatography A 2003;984(1):109. [Presents a rapid,
precise, accurate, and robust method for analysis of the major opium alkaloids in either
opium gum or latex. The same conditions may be utilized to analyze LSD exhibits.]

126) Reddy MM, Suresh V, Jayashanker G, Rao BS, Sarin RK. Application of capillary zone
electrophoresis in the separation and determination of the principal gum opium alkaloids.
Electrophoresis 2003;24(9):1437. [The presented method does not require sample
purification or derivatization.]

127) Szucs Z, Szabady B, Szatmary M, Cimpan G, Nyiredy S. High-throughput analytical

strategy with combined planar and column liquid chromatography for improvement of the
poppy (Papaver somniferum L.) with a high alkaloid content. Chromatographia
2002;56(Suppl. S):S49. [Four different liquid chromatographic methods (multi-layer
overpressured-layer chromatography (MLOPLC), normal-phase high-performance thin-
layer chromatography (NPHPTLC), rapid reversed-phase high-performance liquid
chromatography (RPHPLC), and a second, different RPHPLC method, were used for
determination of alkaloid content of over 15,000 poppy capsule samples.]

227
Overview/Polydrug:

128) Peinhardt G. Identification of illegal drugs in pharmacy laboratories: Combination of

thin layer chromatography and immunochemical quick tests.
PZ Prisma 2002;9(2):99. [A combination of isolation and analytical methods are
presented for detection and determination of cannabis, opiates, heroin, cocaine,
amphetamines, designer drugs, and LSD.]

Pethidine:

129) Quaglia MG, Farina A, Donati E, Cotechini V, Bossu E. Determination of MPTP, a toxic
impurity of pethidine. Journal of Pharmaceutical and Biomedical Analysis 2003;33(1):1.
[Presents the use of CE, MECK, and RP-HPLC to analyze for pethidine and MPTP.]

Phenethylamines (including mixtures of Amphetamines, Methylenedioxy-amphetamines, and

Related Compounds):

130) CampinsFalco P, VerduAndres J, HerraezHernandez R. Separation of the enantiomers of

primary and secondary amphetamines by liquid chromatography after derivatization with
(-)-1-(9-fluorenyl)ethyl chloroformate. Chromatographia 2003;57(5-6):309. [Analysis
of amphetamine, methamphetamine, ephedrine, pseudoephedrine, MDA, MDMA, and
MDE are reported. A variety of sample types (not specified in the abstract) were
analyzed.]

131) Cheng W-C, Lee W-M, Chan —F, Phil M, Tsui P, Dao K-L. Enantiomeric separation of
methamphetamine and related analogs by capillary zone electrophoresis: Intelligence
study in routine methamphetamine seizures. Journal of Forensic Sciences
2002;47(6):1248. [The simultaneous separation of ephedrine, pseudoephedrine, and
methamphetamine using CZE with beta-cyclodextrin as a chiral selector is presented.
Application to the analysis of seized drugs is discussed.]

132) Iwata YT, Garcia A, Kanamori T, Inoue H, Kishi T, Lurie IS. The use of a highly
sulfated cyclodextrin for the simultaneous chiral separation of amphetamine-type
stimulants by capillary electrophoresis. Electrophoresis 2002;23(9):1328.

133) Iwata YT, Kanamori T, Ohmae Y, Tsujikawa K, Inoue H, Kishi T. Chiral analysis of
amphetamine-type stimulants using reversed-polarity capillary electrophoresis/positive
ion electrospray ionization tandem mass spectrometry. Electrophoresis
2003;24(11):1770. [Presents the specialized CE/MS-MS analyses of a variety of ATS’s,
ranging from precursor ephedrines to methylenedioxy- substituted drugs.]

134) Kato N, Ogamo A. A TLC visualization reagent for dimethylamphetamine and other
abused tertiary amines. Science Justice 2001;41(4):239.

135) Lurie IS Bethea MJ, McKibben TD, Hays PA, Pellegrini P, Sahai R, Garcia AD,
Weinberger R. Use of dynamically coated capillaries for the routine analysis of
methamphetamine, amphetamine, MDA, MDMA, MDEA, and cocaine using capillary
electrophoresis. Journal of Forensic Sciences 2001;46(5):1025.

228
Piperazines:

136) de Boer D, Bosman IJ, Hidvegi E, Manzoni C, Benko AA, dos Reys LJAL, Maes RAA.
Piperazine-like compounds: A new group of designer drugs-of-abuse on the European
market. Forensic Science International 2001;121(1-2):47.

137) Kercheval JC. GC/MS analysis of BZP and TFMPP. Mid-Atlantic Association of
Forensic Sciences Newsletter 2004;32(2) (no page numbers). [Presents the GC/MS
analyses of 1-benzylpiperazine and 1-(3-trifluoromethylphenyl)-piperazine.]

138) Wikstroem M, Holmgren P, Ahlner J. N+Benzylpiperazine - A new drug of abuse in

Sweden. Journal of Analytical Toxicology 2004;28(1):67. [A brief overview reporting
the occurrence of BZP in Sweden, also reporting a law enforcement network which
enabled rapid identification of BZP cases.]

Polydrug:

139) Bazylak G, Nagels LJ. Simultaneous high-throughput determination of clenbuterol,

ambroxol and bromhexine in pharmaceutical formulations by HPLC with potentiometric
detection. Journal of Pharmaceutical and Biomedical Analysis 2003;32(4-5):887. [The
title analysis was performed using six different isocratic systems.]

140) Benson AJ, Sabucedo A, Furton KG. Detection and identification of date rape drugs
gamma-hydroxybutyrate (GHB), flunitrazepam (Rohypnol), lysergic acid diethylamide
(LSD), scopolamine, diphenhydramine, and ketamine by refocused solid phase
microextraction high performance liquid chromatography (SPME/HPLC) and solid phase
microextraction high performance liquid chromatography mass spectrometry
(SPME/HPLC/MS). Proceedings of the American Academy of Forensic Sciences
2003;9:29. [Presents a study of the SPME followed by HPLC and HPLC/MS for analysis
of the referenced drugs.]

141) Bishop SC, Lerch MA, McCord BR. A micellar electrokinetic screening for common
sexual assault drugs. Proceedings of the American Academy of Forensic Sciences
2004;10:70. [For detection of eight (unspecified) benzodiazepines, GHB, and GBL.]

142) Bishop SC, Lerch M, McCord BR. Micellar electrokinetic chromatographic screening
method for common sexual assault drugs administered in beverages. Forensic Science
International 2004;141 (1):7. [The title analysis was applied for detection of GHB, GBL,
and eight benzodiazepines (unspecified in abstract) in spiked beverages.]

143) Blanco M, Valverde I. Application of micellar electrokinetic chromatography to the

quality control of a pharmaceutical preparation containing three bronchodilators.
Electrophoresis 2002;23(4):578.

144) Cherkaoui S, Rudaz S, Varesio E, Veuthey JL. On-line capillary electrophoresis-

electrospray mass spectrometry for the stereoselective analysis of drugs and metabolites.
Electrophoresis 2001;22(15):3308. [Includes analyses of amphetamines, methadone, and
tropane alkaloids.]

229
145) Cherkaoui S, Veuthey JL. Use of negatively charged cyclodextrins for the simultaneous
enantioseparation of selected anesthetic drugs by capillary electrophoresis-mass
spectrometry. Journal of Pharmaceutical and Biomedical Analysis 2002; 27(3-4):615.
[Presents the enantioseparation of bupivacaine, mepivacaine, ketamine, and prilocaine.]

146) Geraghty E, Wu C, McGann W. Effective screening for “Club Drugs” with dual mode
ion trap mobility spectrometry. International Journal for Ion Mobility Spectrometry
2002;5(3):41. [Presents a study on the analysis of various “Rave” drugs by dual mode
ITMS, including: Ketamine, GHB, ephedrine, flunitrazepam, methamphetamine, MDA,
amphetamine, and MDMA.]

147) Ishii A, Watanabe-Suzuki K, Seno H, Suzuki O, Katsumata Y. Application of gas

chromatography-surface ionization organic mass spectrometry to forensic toxicology.
Journal of Chromatography B - Analytical Technologies in the Biomedical and Life
Sciences 2002;776(1):3. [The title technique detects phencyclidine (PCP), pethidine,
pentazocine, and MPTP and its derivatives in human body fluids, with high sensitivity
and selectivity.]

148) Katagi M, Tsutsumi H, Miki A, Nakajima K, Tsuchihashi H. Analyses of clandestine

tablets of amphetamines and their designer drugs encountered in recent Japan [sic].
Japanese Journal of Forensic Toxicology 2002;20(3):303. [Presents analyses of various
tablets recently seized in Osaka (including tablets containing MDMA, PMA, 2C-T-7, and
various tryptamines).]

149) Klingmann A, Skopp G, Aderjan R. Analysis of cocaine, benzoylecgonine, ecgonine

methyl ester, and ecgonine by high pressure liquid chromatography-API mass
spectrometry and application to a short-term degradation study of cocaine in plasma.
Journal of Analytical Toxicology 2001;25(6):425.

150) Lurie IS. Capillary electrophoresis analysis of a wide variety of seized drugs on the same
dynamically coated capillary. Proceedings of the American Academy of Forensic
Sciences 2004;10:107. [Drug types include phenethylamines, cocaine, heroin,
oxycodone, morphine, LSD, psilocybin, opium, and GHB/GBL; both qualitative and
quantitative results are achieved.]

151) Madej K, Wozniakiewicz M. Application of capillary electrophoresis to analysis of

tricyclic psychotropic drugs. Z Zagadnien Nauk Sadowych 2002;52:52. [Presents the
use of CZE and MECC for analysis of both blood and pharmaceutical preparations of
phenothiazines and tricyclic psychotropic drugs.]

152) Morehead RA. Optimizing HPLC separation of antidepressant drugs through stationary
phase selection. Proceedings of the American Academy of Forensic Sciences
2003;9:304. [Includes a discussion of the primary separation mechanisms for 14 drugs;
the referenced drugs were not identified.]

153) Pihlainen K, Kostiainen R. Effect of the eluant on enantiomer separation of controlled

drugs by liquid chromatography - ultraviolet absorbance detection - electrospray
ionisation tandem mass spectrometry using vancomycin and native beta-cyclodextrin
chiral stationary phases. Journal of Chromatography A 2004;1033(1):91. [Presents the
title study on nine amphetamine derivatives (not specified in abstract), methorphan, and
propoxyphene. 14 seized drug samples (not specified in abstract) were analyzed using
the optimized methodologies.]

230
Propoxyphene:

154) Magoon T, Ota K, Jakubowski J, Nerozzi M, Werner TC. The use of neutral
cyclodextrins as additives in capillary electrophoresis for the separation and identification
of propoxyphene enantiomers. Analytical and Bioanalytical Chemistry 2002;373(7):628.
[Baseline separation was achieved in approximately 6 minutes.]

Psilocybin Mushrooms, Psilocybin, and Psilocin:

155) Linacre A, Cole M, Chun-I Lee J. Identifying the presence of “magic mushrooms” by
DNA profiling. Science and Justice 2002;42(1):50. [Presents a minor review of DNA-
based analyses of psilocybe and panaeolus mushrooms. The techniques are especially
valuable for cases of dry, powdered material where microscopic characterization is
impossible.]

156) Mahler, H, Daldrup T. Quick detection of psilocin in mushroom culture substrates.

GTFCh-Symposium: Toxikologische Aspekte der Sterbehilfe - Neue Drogen:
Chemische, Analytische und Toxikologische Aspekte, Beitraege zum Symposium der
Gesellschaft fuer Toxikologische und Forensische Chemie, 12th, Mosbach, Germany,
Apr. 26 - 28, 2001 2001;(Pub 2001):242. [Psilocin was isolated and identified from
mushroom culture substrates with HPLC/UV and GC/MS.]

157) Nugent KG, Saville BJ. Forensic analysis of hallucinogenic fungi: A DNA-based
approach. Forensic Science International 2004;140(2-3):147. [Presents the title study.]

158) Sarwar M, McDonald JL. A rapid extraction and GC/MS methodology for the
identification of psilocyn in mushroom/chocolate concoctions. Microgram Journal
2003;1(3-4):177.

159) Tsujikawa K, Kanamori T, Iwata Y, Ohmae Y, Sugita R, Inoue H, Kishi T.

Morphological and chemical analysis of magic mushrooms in Japan. Forensic Science
International 2003;138(1-3):85. [Analyses included the complementary use of a
scanning electron microscope (SEM), along with standard microscopy and HPLC/UV.
Listed substrates included Psilocybe cubensis and Copelandia.]

Psychotria Viridis:

160) Blackledge RD, Taylor CM. Psychotria viridis – A botanical source of

dimethyltryptamine (DMT). Microgram Journal 2003;1(1-2):18. [Presents both forensic
and botanical profiles for the title substance.]

Salvia Divinorum

161) Blaszczyk P, Hernik H, Ehrmann R. Salvinorin A (Salvinoryna A). Problemy

Kryminalistyk 2002;237:48. [Presents a GC/MS method for analysis of Salvia
divinorum.]

231
Steroids:

162) Catlin DH, Ahrens BD, Kucherova Y. Detection of norbolethone, an anabolic steroid
never marketed, in athlete’s urine. Rapid Communications in Mass Spectrometry
2002;16(13):1273. [Presents analysis by GC/MS. The authors note that the title
compound has never been commercially marketed, and suggest that a clandestine source
may therefore be in operation.]

163) Hussain AA, Al-Bayatti AA, Dakkuri A, Okochi K, Hussain MA. Testosterone-17(beta)-
N,N-dimethylglycinate hydrochloride: A prodrug with a potential for nasal delivery of
testosterone. Journal of Pharmaceutical Sciences 2002;91(3):785.

164) Leinonen A, Kuuranne T, Kostiainen R. Liquid chromatography/mass spectrometry in

anabolic steroid analysis-optimization and comparison of three ionization techniques:
Electrospray ionization, atmospheric pressure chemical ionization and atmospheric
pressure photoionization. Journal of Mass Spectrometry 2002;37(7):693. [The
presented LC/MS/MS technique exhibited high sensitivity and specificity for the
detection of various steroids, and may be a suitable technique for screening for the abuse
of anabolic steroids.]

165) Lommen A, Schilt R, Weseman J, Roos AH, vanVelde JW, Nielen MWF. Application of
1D H-1 NMR for fast non-targeted screening and compositional analysis of steroid
cocktails and veterinary drug formulations administered to livestock. Journal of
Pharmaceutical and Biomedical Analysis 2002;28(1):87.

166) Nozaki O. Steroid Analysis for medical diagnosis. Journal of Chromatography A

2001;935(1-2):267. [Includes analysis of anabolic steroids; focus is on analysis of
biological matrices.]

(Designer) Tryptamines (see also Psilocybin):

167) Ausili PT, Negrusz A, Dal Cason TA, Larsen AK, Schlemmer RF, Tella SR.
Tryptamines and other psychotropic (mind altering) substances: Analysis, toxicology,
and pharmacology. Proceedings of the American Academy of Forensic Sciences
2004;10:13. [A comprehensive overview of the recent increase in psychotropics,
including evaluation and control issues.]

168) Meatherall R, Sharma P. Foxy, a designer tryptamine hallucinogen. Journal of

Analytical Toxicology 2003;27(5):313. [Primary focus is analysis of biological fluids;
however, includes a small scale mass spectra (from GC/MS) of “Foxy” (5-methoxy-N,N-
diisopropyltryptamine).]

169) Zimmerman MM. The identification of 5-methoxy-alpha-methyltryptamine. Microgram

Journal 2003;1(3-4):158. [Uses color tests and GC/MS).]

Zaleplon:

170) Tang B, Wang X, Jia BX, Niu JY, Wei Y, Chen ZZ, Wang Y. Simple, rapid, and
sensitive spectrofluorimetric determination of Zaleplon in micellar medium. Analytical
Letters 2003;36(14):2985.

232
Zolpidem

171) ElZeany BA, Moustafa AA, Farid NF. Determination of zolpidem hemitartrate by
quantitative HPTLC and LC. Journal of Pharmaceutical and Biomedical Analysis
2003;33(3):393. [Presents the analyses of zolpidem in the presence of its degradation
product by TLC-UV densitometry and by HPLC with UV detection.]

Zopiclone:

172) Meng Z-Y. Properties of a newly produced hypnotic “Imovane” and its determination.
Guangpu Shiyanshi 2003;20(3):471. [Presents HPLC and GC-MS data for the title
compound (principal component is Zopiclone).]

Miscellaneous:

173) Bartlett V. HPLC analysis of narcotic/acetaminophen admixtures. What to do if a

compendium method doesn’t work. The Restek Advantage 2002;3:6. [Discusses
modifications to established methods for separating admixtures of compounds with
similar structures.]

Synthesis and/or cultivation of abused substances, their precursors, and essential

chemicals

Production of Abused Substances and/or their Precursors and Essential Chemicals:

174) Courtney M, Ekis TR. O, dem bones. Systematic analysis of remnants from “Nazi”
methamphetamine laboratories. Journal of the Clandestine Laboratory Investigating
Chemists Association 2003;13(1):17. [Presents a systematic approach to analyzing the
reaction dregs recovered from Birch reduction laboratories, for the purpose of identifying
the original reactants, extraction solvents, and products.]

175) Crow BM. Production of anhydrous ammonia used to produce methamphetamine via the
Birch reduction method. Journal of the Clandestine Laboratory Investigating Chemists
Association 2004;14(1):18.

176) Dimitroff D. Psilocybin mushroom cultivation. Journal of the Clandestine Laboratory

Investigating Chemists Association. 2004;14(2):11. [An overview of the title topic.]

177) Hough M, Warburton H, Few B, May T, Man LH, Witton J, Turnbull PJ. A growing
market. The domestic cultivation of cannabis. Report Joseph Rowntree Foundation
2003; pp. 1 - 45. [Presents an overview of domestic cultivation of cannabis in England
and Wales.]

178) Laing R, Hugel J. Methods of illicit manufacture. Hallucinogens 2003:139. [A review

of the common illicit syntheses of a variety of hallucinogens.]

179) Person EC, Knops LA. Clandestine Ammonia Generation. Journal of the Clandestine
Laboratory Investigating Chemists Association 2004;14(1):20.

180) Person EC, Knops LA, Northrop DM, Sheridan SP. “One-pot” methamphetamine
manufacture. Journal of the Clandestine Laboratory Investigating Chemists Association.
2004;14(2):14. [Editor’s Notes: Presents an evaluation of an Internet recipe.]

233
181) Potter GR. The growth of Cannabis growing: A study of urban Cannabis growers in the
north of England. Report Sheffield University 2002; No. 00189486; pp. 1 - 20.
[Presents an overview of the title topic.]

Clandestine Laboratory Appraisals and Safety:

182) Bakouri E, Van Rijn A. Dismantling of [a] clandestine laboratory in Greece. Science
Justice 2001;41(3):213.

183) Borngasser J. Lab supplies go to the highest bidder: A brief analysis of clandestine
methamphetamine laboratory supplies and methamphetamine precursors being sold on
ebay®. Journal of the Clandestine Laboratory Investigating Chemists Association
2004;14(2):8.

184) De Haan JD, Angelos SA. Bubble, bubble, boom! Fires and explosions in clandestine
drug laboratories. Proceedings of the American Academy of Forensic Sciences
2004;10:18. [A comprehensive overview of the title subject, for both arson investigators
and forensic chemists.]

185) Hugel J, Pearson M, Evoy T. Drug Yield Calculator Version 3.2 Journal of the
Clandestine Laboratory Investigating Chemists Association 2002;12(4):28. [Presents a
computer program that calculates potential yield of common scheduled drugs when given
a known amount of precursor and the synthetic route.]

186) Janusz A, Kirkbride KP, Scott TL, Naidu R, Perkins MV, Megharaj M. Microbial
degradation of illicit drugs, their precursors, and manufacturing by-products:
Implications for clandestine laboratory investigation and environmental assessment.
Forensic Science International 2003;134(1):62. [Presents a study of the enviromental
degradation of phenylacetone and methamphetamine sulfate at clandestine laboratory
dumpsites in Australia.]

187) Kubicz-Loring EJ, Downs AA, Miller SJ, Jolley JM, Allen PC. The clandestine
laboratory – A recipe for disaster. Proceedings of the American Academy of Forensic
Sciences 2002;8:17. [A workshop providing overviews of the investigation, chemistry,
toxicology, and pathology of clandestine laboratories, especially methamphetamine
laboratories.]

188) White MJ. National initiatives and issues related to clandestine laboratory investigations
in Australia. Proceedings, 16th International Symposium on the Forensic Sciences,
Canberra 2002(16):(No pps given). [An overview of major counter-drug laboratory
initiatives in Australia during the time frame 1992-2002.]

Safety Issues - Case Reports:

189) Cameron M. Iodine: Inhalation Hazards, Detection, and Protection. Journal of the
Clandestine Laboratory Investigating Chemists Association 2002;12(4):18. [Presents a
safety overview of iodine, focusing on exposure as a result of clandestine laboratory
raids.]

234
190) Willers LJ. The detection of phosphine gas produced from hydriodic acid and the
evaluation of detection instruments for use in clandestine laboratory environments.
Journal of the Clandestine Laboratory Investigating Chemists Association 2003;13(2):14.
[Presents a comprehensive overview of the problem and a detailed evaluation of a
number of electronic detection devices.]

Miscellaneous:

191) Kelly CA, Lawrence DS, Murray GM, Uy OM. Methamphetamine Synthesis Inhibition:
Dissolving Metal Reductions. Journal of the Clandestine Laboratory Investigating
Chemists Association 2002;12(3):10. [Presents the preliminary results of research
investigating the development of inhibition reagents that would render anhydrous
ammonia unusable for illicit manufacture of methamphetamine from
ephedrine/pseudoephedrine via the lithium/ammonia (“Nazi”) reduction.]

192) Lewis LD. Method of disposing of hazardous wastes connected with criminal activity.
US 20030176756 A1 18 Sep 2003, U.S. Pat Appl. Publ. CLASS: ICM: A62D003-00.
NCL: 588213000. APLICATION: US 2002-100325 18 Mar 2002. [Presents the use of
a portable incinerator (however, only selected waste materials are suitable for
destruction).]

193) Worley D. Evaluation of ammonium test paper. Journal of the Clandestine Laboratory
Investigating Chemists Association 2002;12(2):17.

Reference Drug Standards and Total Syntheses

194) Brunner H. Narcotic drug methohexital: Synthesis by enantioselective catalysis.

Chirality 2001;13(8):420.

195) Chan KB. The identification, purification, and authentication of some reference drug
standards. Microgram 2001;34(8):214.

196) Jarikote DV, Siddiqui SA, Rajagopal R, Daniel T, Lahoti RJ, Srinivasan KV. Room
temperature ionic liquid promoted synthesis of 1,5-benzodiazepine derivatives under
ambient conditions. Tetrahedron Letters 2003;44(9):1835. [Presents a novel synthetic
approach to the title compounds.]

197) Khedkar V, Tillack A, Michalik M, Beller M. Efficient on-pot synthesis of tryptamines

and tryptamine homologues by amination of chloroalkynes. Tetrahedron Letters
2004;45(15):3123.

198) Klemenc S. 4-Dimethylaminopyridine as a catalyst in heroin synthesis. Forensic Science

International 2002;129(3):194. [Presents a study on the acetylation of morphine using 4-
dimethylaminopyridine (4-DMAP) as a catalyst.]

199) Kozma D, Fogassy E. Solvent-free optical resolution of N-methylamphetamine by

distillation after partial diastereoisomeric salt formation. Chirality 2001;13(8):428.

200) Pizarro N, delaTorre R, Farre M, Segura J, Liebaria A, Joglar J. Synthesis and capillary
electrophoretic analysis of enantiomerically enriched reference standards of MDMA and
its main metabolites. Bioorganic and Medicinal Chemistry 2002;10(4):1085. [Includes
the synthesis of enantiomerically enriched (S)-3,4-methylenedioxymethamphetamine.]

235
201) Pozarentzi M, Stephanidou-Stephantou J, Tsoleridis CA. An efficient method for the
synthesis of 1,5-benzodiazepine derivatives under microwave irradiation without solvent.
Tetrahedron Letters 2002;43(9):1755.

202) Shirota O, Hakamata W, Goda Y. Concise large-scale synthesis of psilocin and

psilocybin, principal hallucinogenic constituents of “Magic Mushroom” [sic]. Journal of
Natural Products 2003;66(6):885.

203) Trost BM, Tang WP. Enantioselective synthesis of (-)-codeine and (-)-morphine.
Journal of the American Chemical Society 2002;124(49):14542.

204) Van Zyl EF. A survey of reported synthesis of methaqualone and some positional and
structural isomers. Forensic Science International 2001;122(2-3):142.

205) William AD, Kobayashi Y. Synthesis of tetrahydrocannabinols based on an indirect 1,4-

addition strategy. Journal of Organic Chemistry 2002;67(25):8771. [Presents a novel
synthesis route to optically active THC and related compounds.]

206) Yoshida H, Shirakawa E, Honda Y, Hiyama T. Addition of ureas to arynes:

Straightforward synthesis of benzodiazepine and benzodiazocine derivatives.
Angewandte Chemie - International Edition 2002;41(17):3247.

Source Determination of Drugs (Impurity Profiling) and Comparative Analyses

Amphetamine(s):

207) Ballany J, Caddy B, Cole M, Finnon Y, Aalberg L, Janhunen K, Sippola E, Andersson K,

Bertler C, Dahlen J, Kopp I, Dujourdy L, Lock E, Margot P, Huizer H, Poortman A, Kaa
E, Lopes A. Development of a harmonised pan-European method for the profiling of
amphetamines. Science Justice 2001;41(3):193.

208) Blachut D, Czarnocki Z, Wojtasiewicz K. alpha-Phenylethylamine in illegally produced

amphetamine. Forensic Science International 2001;123(2-3):182.

209) Carter JF, Titterton EL, Grant H, Sleeman R. Isotopic changes during the synthesis of
amphetamines. Chemical Communications 2002;21:2590. [Presents a study of the
variations in C-13 and N-15 during various syntheses of amphetamine. The authors also
claim that isotopic characterization can assist in identifying the synthetic origins of illicit
MDMA and other amphetamines.]

210) Krawczyk W, Parczewski A. Application of chemometric methods in searching for illicit

Leuckart amphetamine sources. Analytica Chimica Acta 2001;446:107. [Presents an
impurity profiling methodology for linking amphetamine samples.]

211) Ottaviano V, Furnari C, Rosati F. Identification of di(beta-phenylisopropyl)amine as the

main ingredient in illicit amphetamine tablets. Annali dell’Instituto Superiore di Sanita
2002;38(3):331. [Presents the identification of the title compound as the primary
ingredient in several sets of amphetamine tablets sold in Rome during 1999-2000.]

236
Cocaine:

212) Chiarotti M, Marsili R, Moreda-Pineiro A. Gas chromatographic - mass spectrometric

analysis of residual solvent trapped into illicit cocaine exhibits using head-space solid-
phase microextraction. Journal of Chromatography B - Analytical Technologies in the
Biomedical and Life Sciences 2002;772(2):249.

Cocaine and Heroin:

213) Galimov EM, Sevast’yanov VS, Kul’bachevskaya EV, Golyavin AA. Determination of
isotopic compositions of carbon and nitrogen by the IRMS method: Implication for the
source of narcotic substance origin. Doklady Earth Sciences 2003;393(8):1109.
[Presents the title study on cocaine and heroin from different regions.]

Dimethylamphetamine:

214) Sato M, Hida M, Nagase H. Analysis of pyrolysis products of dimethyl-amphetamine.

Journal of Analytical Toxicology 2001;25(5):304.

Heroin:

215) Bora T, Merdivan M, Hamamci C. Levels of trace and major elements in illicit heroin.
Journal of Forensic Sciences 2002;47(5):959. [Ten elements in 44 illicit heroin samples
were determined using electrothermal atomic absorption spectrometry or inductively
coupled plasma-atomic emission spectrometry.]

216) Dams R, Benjits T, Lambert WE, Massart DL, De Leenheer AP. Heroin impurity
profiling: Trends throughout a decade of experimenting. Forensic Science International
2001;123(2-3):81.

217) Dams R, Benjits T, Guenther W, Lambert W. Sonic spray ionization technology:

Performance study and application to an LC/MS analysis on a monolithic silica column
for heroin impurity profiling. Analytical Chemistry 2002;74(13):3206. [Enables
analysis for 7 primary opium alkaloids in illicit heroin in 5 minutes.]

218) Dujourdy L, Barbati G, Taroni F, Gueniat O, Esseiva P, Anglada F, Margot P.

Evaluation of links in heroin seizures. Forensic Science International 2003;131(2-
3):171. [Presents a mathematical means for comparing chromatograms for degree of
similarity, without using decision thresholds.]

219) Esseiva P, Dujourdy L, Anglada F, Taroni F, Margot P. A methodology for illicit heroin
seizures comparison in a drug intelligence perspective using large databases. Forensic
Science International 2003;132(2):139. [Presents a methodology for comparing heroin
profiles. The authors claim that the methodology is solid, reliable, and simple.]

220) Hajdar M, Ruzdic E. Characterisation [sic] of heroin samples obtained in the area of the
Federation of Bosnia and Herzegovina. Journal of Environmental Protection and Ecology
2003;4(4):873. [Presents the title survey, using GC/FID analysis to detect 8 opium
alkaloids and 3 typical adulterants. The number of samples and the date range were not
specified in the abstract.]

237
221) Lurie IS, Anex DS, Fintchenko Y, Choi W-Y. Profiling of impurities in heroin by
capillary electrochromatography and laser induced fluorescence detection. Journal of
Chromatography A 2001;924(1):421.

222) Zhang D, Shi X, Yuan Z, Ju H. Component analysis of illicit heroin samples with
GC/MS and its application in source determination. Journal of Forensic Sciences
2004;49(1):81. [Presents a profiling analysis based on both GC and GC/MS. 500
samples were subclassified into nine groups using the presented techniques.]

Marijuana
:
223) Carita EJ, Coyle HM, Ladd C, Palmbach TM, Lee HC. Expansion of an AFLP DNA
marijuana (Cannabis sativa) state, national, and international database. Proceedings of
the American Academy of Forensic Sciences 2004;10:79. [An overview of the use of
AFLP to characterize marijuana.]

224) Germane-Presby J, Coyle HM, Palmbach TM, Pagliaro EM, Ladd C, Harper A, Lee HC.
Development of a nationwide AFLP DNA database for marijuana (Cannabis sativa).
Proceedings of the American Academy of Forensic Sciences 2003;9:32. [A status report
of an ongoing project by the Connecticut State Forensic Science Laboratory.]

Methamphetamine:

225) Inoue H, Kanamori T, Iwata YT, Ohmae Y, Tsujikawa K, Saitoh S, Kishi T.

Methamphetamine impurity profiling using a 0.32 mm i.d. nonpolar capillary column.
Forensic Science International 2003;135(1):42. [The presented method allows for
determination of 24 different characteristic starting materials and manufacturing
byproducts.]

226) Jacobs JL, Martinez FS, Skinner HF. Extraction of reaction by-products of common cold
tablet ingredients via hydriodic acid reduction. Journal of the Clandestine Laboratory
Investigating Chemists Association 2003;13(1):13. [Presents a study of the HI/red P
reduction of a variety of co-ingredients found in ephedrine or pseudoephedrine based cold
tablets.]

227) Koester CJ, Andresen BD, Grant PM. Optimum methamphetamine profiling with sample
preparation by solid-phase microextraction. Journal of Forensic Sciences
2002;47(5):1002. [Volatile and semi-volatile components are recovered from illicit
methamphetamine by SPME and analyzed by GC/MS. The method is claimed to be
superior for profiling illicit methamphetamine.]

228) Kubicz-Loring E. Illicit methamphetamine profiling. Proceedings of the American

Academy of Forensic Sciences 2003;9:30. [The impurity profiles of methamphetamine
produced via the HI/red P reduction and Li/NH3 reductions are discussed and contrasted.]

229) Makino Y, Urano Y, Nagano T. Impurity profiling of ephedrines in methamphetamine

by high-performance liquid chromatography. Journal of Chromatography A
2002;947(1):151.

230) Puthaviriyakorn V, Siriviriyasomboon N, Phorachata J, Pan-ox W, Sasaki T, Tanaka K.

Identification of impurities and statistical classification of methamphetamine tablets (Ya-
Ba) seized in Thailand. Forensic Science International 2002;126(2):105.

238
231) Vu D-TT. SPME/GC-MS characterization of volatiles associated with
methamphetamine: Toward the development of a pseudomethamphetamine training
material. Journal of Forensic Sciences 2001;46(5):1014.

4-Methoxyamphetamine and 4-Methoxymethamphetamine:

232) Blachut D, Maurin JK, Starosta W, Wojtasiewicz K, Czarnocki Z. (2S)-1-(4-

Methoxyphenyl)-N-[(1R)-2-(4-methoxyphenyl)-1-methylethyl]-2-propanamine in crude
p-methoxyamphetamine (PMA) produced by the Leuckart method. Zeitschrift fuer
Naturforschung B: Chemical Sciences 2002;57(5):593. [The title compound is
established as a synthetic marker for Leuckart produced PMA.]

233) Blachut D, Wojtasiewicz K, Czarnocki Z. Identification and synthesis of some

contaminants present in 4-methoxyamphetamine (PMA) prepared by the Leuckart
method. Forensic Science International 2002;127(1-2):45.

234) Kochana J, Wilamowski J, Parczewski A, Surma M. Synthesis of standards of the most

important markers of Leuckart p-methoxymethamphetamine (PMMA). Examination of
the influence of experimental conditions and a drug diluent on SPE/TLC profiling.
Forensic Science International 2003;134(2-3):207.

235) Waumans D, Bruneel N, Tytgat J. Anise oil as para-methoxyamphetamine (PMA)

precursor. Forensic Science International 2003;133(1-2):159. [Presents a study of a
large-scale PMA laboratory using anise oil as a precursor source. Includes impurity
profiling studies that identified marker compounds for this synthesis.]

236) Waumans D, Bruneel N, Hermans B, Tytgat J. A rapid and simple GC/MS screening
method for 4-methoxyphenol in illicitly prepared 4-methoxy-amphetamine (PMA).
Microgram Journal 2003;1(3-4):184. [Confirms that
4-methoxyphenol is a marker compound for syntheses of PMA starting from anethole.]

Methylenedioxyamphetamines:

237) Armellin S, Brenna E, Fronza G, Fuganti C, Pinciroli M, Serra S. Establishing the

synthetic origin of amphetamines by H-2 NMR spectroscopy. Analyst 2004;129(2):130.
[The title study was applied to nine samples of N+acetyl-MDA.]

238) Bell SEJ, Barrett LJ, Burns DT, Dennis AC, Speers SJ. Tracking the distribution of
“ecstasy” tablets by Raman composition profiling: A large scale feasibility study.
Analyst 2003;128(11):1331. [Approximately 1500 tablets (all primarily MDMA) from
different seizures in Northern Ireland were analyzed and found to have significant
differences in their Raman spectra due to the presence of impurities and the degree of
hydration of the MDMA. The results indicated that sample-sample comparisons could be
accomplished using Raman spectroscopy.]

239) Carter JF, Titterton EL, Murray M, Sleeman R. Isotopic characterization of

3,4-methylenedioxyamphetamine and 3,4-methylenedioxymethylamphetamine (Ecstasy).
Analyst 2002;127(6):830. [Via analysis by IRMS and Deuterium NMR.]

239
240) Cheng W-C, Poon N-L, Chan M-F. Chemical profiling of 3,4-methylenedioxy-
methamphetamine (MDMA) tablets seized in Hong Kong. Journal of Forensic Sciences
2003;48(6):1249. [Presents an overview of the results of analysis for 600,000 ecstasy
tablets (2,600 cases) seized in Hong Kong during 2000 - 2001.]

241) Gimeno, P, Besacier F, Chaudron-Thozet H, Girard J, Lamotte A. A contribution to the

chemical profiling of 3,4-methylenedioxymethamphetamine (MDMA) tablets. Forensic
Science International 2002;127(1-2):1. [An extensive study of profiling illicit MDMA
tablets via a variety of chromatographic/mass spectrometric techniques.]

242) Gimeno P, Besacier F, Chaudron-Thozet H. Optimization of extraction parameters for

the chemical profiling of 3,4-methylenedioxymethamphetamine (MDMA) tablets.
Forensic Science International 2003;132(3):182. [Presents an optimized extraction
procedure for recovery of impurities from MDMA tablets using diethyl ether extraction
from a pH 11.5 buffered solution, followed by GC/MS analysis.]

243) Makino Y, Kurobane S, Miyasaka K, Nagano K. Profiling of ecstasy tablets seized in

Japan. Microgram Journal 2003;1(3-4):169. [Presents the title study, focusing on tablets
seized during the first half of CY-2002. Several trends are reported. ]

244) Palhol F, Boyer S, Naulet N, Chabrillat M. Impurity profiling of seized MDMA tablets
by capillary gas chromatography. Analytical and Bioanalytical Chemistry
2002;374(2):274. [Presents a study of MDMA tablets seized in France (total number not
specified in the abstract). The authors claim that the results suggest that MDP2P is the
most commonly used precursor, and that reductive amination is the most common
synthetic route used to prepare the MDMA found in the tablets.]

245) Palhol F, Lamoureux C, Naulet N. N-15 Isotopic analyses: A powerful tool to establish
links between seized 3,4-methylenedioxymethamphetamine (MDMA) tablets. Analytical
and Bioanalytical Chemistry 2003;376(4):486. [Forty-three samples were analyzed by
GC-Combustion-IRMS; the authors indicate that the technique can help establish
common origins between samples.]

246) van der Peijl GJQ, van den Boom CPH, Bolck A, Dobney AM. XTC characterisation
[sic] using ICPMS. Proceedings of the American Academy of Forensic Sciences
2004;10:53. [Presents the results of an ICPMS study of about 100 ecstasy samples.]

247) Titterton E, Carter J, Murray M, Sleeman R. Characterisation [sic] of ecstasy tablets by

isotope ratio mass spectrometry. Proceedings of the 16th Meeting of the International
Association of Forensic Sciences, Montpellier, France, September 2-7, 2002, pps 111-
115. [MDA- and MDMA-based Ecstasy tablets were analyzed for deuterium, carbon-13,
and nitrogen-15 to derive a isotopic fingerprint. Deuterium substitution was also
determined via deuterium NMR.]

248) Vohlken BA, Layton SM. Instrumental separation of 3,4-methylenedioxy-amphetamine

(MDA) from 1-(3,4-methylenedioxyphenyl)-2-propanol, a co-eluting compound.
Microgram Journal 2003;1(1-2):32. [Presents a study of the referenced co-elution
problem; includes the mass spectra for the title alcohol.]

249) Vu D-TT. Logo and headspace comparison for source determination of ecstasy seizures.
Microgram 2001;34(9):244.

240
250) Waddell RJH, NicDaeid N, Littlejohn D. Classification of ecstasy tablets using trace
metal analysis with the application of chemometric procedures and artificial neural
network algorithms. Analyst 2004;129(3):235. [Presents a study of the practicality of
ICP-MS for sample-sample comparisons. Several statistical analyses are evaluated.]

Opium and Opium Alkaoids

:
251) Al-Amri AM, Smith RM, El-Haj BM, Juma’a MH. The GC-MS detection and
characterization of reticuline as a marker of opium use. Forensic Science International
2004;140(2-3):175. [Reticuline was detected as its trimethylsilyl ethers, acetyl esters, and
methyl ethers, in opium and in the urine of opium users. The results can be used to
differentiate between opium and heroin users.]

252) Hosokawa K, Shibata T, Nakamura I, Hishida A. Discrimination among species of

Papaver based on the plastid rp116 gene and the rp116-rp114 spacer sequence. Forensic
Science International 2004;139(2-3):195. [Five of six species of papaver were
distinguishable using the title technique.]

253) Kelly SA, Glynn PM, Madden SJ, Grayson DH. Impurities in a morphine sulfate drug
product identified as 5-(hydroxymethyl)-2-furfural, 10-hydroxymorphine and 10-
oxomorphine. Journal of Pharmaceutical Sciences 2003;92(3):485. [The referenced
impurities were isolated by semi-prep HPLC and identified via MS and NMR. The
presence of sugars in the drug formulation was implicated in the formation of the
impurities.]

Occluded Solvent Analyses:

254) Camarasu CC. Unknown residual solvents identification in drug products by headspace
solid phase microextraction gas chromatography-mass spectrometry. Chromatographia
2002;56(Suppl. S):S131. [Presents a sensitive headspace SPME method for the
extraction of residual solvents from pharmaceutical products (the specific products were
not detailed in the abstract). The SPME method appears to be more sensitive than static
headspace techniques.]

Multi-Drug and Miscellaneous:

255) Binder R, Machata G, Stead H. Analysis of potassium permanganate as a narcotic drug

precursor. Archiv fur Kriminologie 2003;211:160. [Thirty-one samples were analyzed
for 9 metallic elements using emission spectroscopy and ICP-OES. The results did not
allow classification of the samples according to origin.]

256) Lachance PA. Nutraceutical/drug/anti-terrorism safety assurance through traceability.

Toxicology Letters 2004;150(1):25. [Presents an overview of techniques used to ensure
traceability of nutraceutical products.]

257) Muratsu S, Ninomiya T, Kagoshima Y, Matsui J. Trace elemental analysis of drugs of

abuse using synchrotron radiation total reflection X-ray fluorescence analysis (SR-
TXRF). Journal of Forensic Sciences 2002;47(5):944. [Trace elements in amphetamine,
cocaine, heroin, marijuana, methamphetamine,
3,4-methylenedioxymethamphetamine, and opium were determined using the title
technique.]

241
258) Palhol F. Contribution of isotopic analyses to the fight against drug trafficking. Actualite
Chimique 2003;(8-9):27. [Appears to be an overview of the topic (not clear from the
abstract).]

259) Shearer GL. Contaminant identification in pharmaceutical products. Microscope

2003;51(1):3. [A review of the title topic.]

260) Watanabe S, Shibata M, Kataoka K. Comparison of data obtained by various GC

methods for impurity profiling of stimulant drugs. Kanzei Chuo Bunsekishoho
2002;42:73. [Three different GC methods were used for impurity profiling of 10 typical
impurities in 12 samples of stimulant drugs (not specified in abstract).]

261) Xu Q, Du L, Cao X. Simultaneous determination of 8 kinds of components in cannabis,

opium, and heroin by gas chromatography. Fenxi Huaxue 2003;31(8):961. [Presents the
title study using wide-bore GC.]

Analysis of Non-Controlled Pharmaceuticals, Pseudo-Drugs, Adulterants, Diluents, and

Precursors

262) Dash AK, Mo Y, Pyne A. Solid state properties of creatine monohydrate. Journal of
Pharmaceutical Sciences 2002;91(3):708.

263) Dash AK, Sawhney A. A simple LC method with UV detection for the analysis of
creatine and creatinine and its application to several creatine formulations. Journal of
Pharmaceutical and Biomedical Analysis 2002;29(5):939. [Presents a simple and
sensitive LC method for the determination of creatine and creatinine in various creatine
supplement formulations.]

264) Persky AM, Hochhaus G, Brazeau GA. Validation of a simple liquid chromatography
assay for creatine suitable for pharmacokinetic applications, determination of plasma
protein binding, and verification of percent labeled claim of various creatine products.
Journal of Chromatography B - Analytical Technologies in the Biomedical and Life
Sciences 2003;794(1):157. [Includes the analysis of OTC creatine containing products.]

265) Wagner SD, Kaufer SW, Sherma J. Quantification of creatine in nutrition supplements
by thin layer chromatography-densitometry with thermochemical activation of
fluorescence quenching. Journal of Liquid Chromatography and Related Technologies
2001;24(16):2525.

Ephedra, Ephedrine, and/or Pseudoephedrine and Related Compounds

:
266) Abourashed EA, El-Alfy AT, Khan IA, Walker L. Ephedra in perspective – A current
review. Phytotherapy Research 2003;17:703. [A comprehensive review.]

267) Bicker W, Hebenstreit D, Lammerhofer M, Lindner W. Enantiomeric profiling in

ephedrine samples by enantioselective capillary electrochromatography. Electrophoresis
2003;24(15):2532. [Presents a non-aqueous CEC method for the analysis of ephedrine.]

268) Chen HL, Chen XG, Pu QS, Hu ZD, Zhao ZF, Hooper M. Separation and determination
of ephedrine and pseudoephedrine by combination of flow injection with capillary
electrophoresis. Journal of Chromatographic Science 2003;41(1):1.

242
269) Jacob P, Haller CA, Duan MJ, Yu L, Peng M, Benowitz NL. Determination of ephedra
alkaloid and caffeine concentrations in dietary supplements and biological fluids. Journal
of Analytical Toxicology 2004;28(3):152.

270) Kim HK, Choi YH, Chang WT, Verpoorte R. Quantitative analysis of ephedrine
analogues from ephedra species using H1-NMR. Chemical and Pharmaceutical Bulletin
2003;51(12):1382.

271) Li HX, Ding MY, Lv K, Yu JY. Separation and determination of ephedrine alkaloids and
tetramethylpyrazine in ephedra sinica Stapf by gas chromatography-mass spectrometry.
Journal of Chromatographic Science 2001;39(9):370.

272) Niemann RA, Gay ML. Determination of ephedrine alkaloids and synephrine in dietary
supplements by column-switching cation exchange high-performance liquid
chromatography with scanning-wavelength ultraviolet and fluorescence detection.
Journal of Agricultural and Food Chemistry 2003;51(19):5630.

273) Palabiyik IM, Dinc E, Onur. Simultaneous spectrophotometric determination of

pseudoephedrine hydrochloride and ibuprofen in a pharmaceutical preparation using ratio
spectra derivative spectrophotometry and multivariate calibration techniques. Journal of
Pharmaceutical and Biomedical Analysis 2004;34(3):473. [Presents a comparison of
five different statistical evaluation methods for the title drug combination.]

274) Sullivan D, Wehrmann J, Schmitz J, Crowley R, Eberhard J. Determination of ephedra

alkaloids by liquid chromatography/tandem mass spectrometry. JAOAC International
2003;86(3):471. [Presents an LC-MS/MS methodology for determination of six major
ephedra alkaloids in various substrates, ranging from raw ephedra to a high-protein drink
mix containing ephedra.]

275) Tseng YL, Hsu H-R, Kuo F-H, Shieh M-H, Chang C-F. Ephedrines in over-the-counter
cold medicines and urine specimens collected during sport competitions. Journal of
Analytical Toxicology 2003;27(6):359. [Presents an analytical protocol using GC/NPD
and GC/MS. Compounds include ephedrine, pseudoephedrine, phenylpropanolamine,
and methylephedrine. 91 OTC medications were analyzed.]

276) Verdu-Andres J, Herraez-Hernandez R, Campins-Falco P. Analysis of enantiomers

giving partially overlapped peaks by using different treatments of the chromatographic
ultraviolet signals: Quantification of pseudoephedrine enantiomers. Journal of
Chromatography A 2001;930(1-2):95.

277) Wallace K. Separation of ephedra alkaloids by GC-MS. Journal of the Clandestine

Laboratory Investigating Chemists Association 2002;12(2):14.

278) Wedig M, Laug S, Christians T, Thunhorst M, Hozgrabe U. Do we know the mechanism

of chiral recognition between cyclodextrins and analytes? Journal of Pharmaceutical and
Biomedical Analysis 2002;27(3-4):531. [Chiral separation of ephedrine-type
phenethylamines using various cyclodextrins is examined by CE and NMR.]

279) Ye NS, Gu XX, Zou H, Zhu RH. Separation and determination of ephedrine enantiomers
by capillary electrophoresis using l-leucine as chiral selector. Chromatographia
2002;56(9-10):637. [The technique was applied to the analysis of ephedra plant extracts.]

243
280) Zhang XH, Ouyang J, Yang YP. A simple method for chiral separation of ephedrines
using (R)-1-naphthylglycine and 3,5-dinitrobenzoic acid as stationary phase. Analytical
Letters 2001;34(11):1851.

281) Zhang JY, Xie JP, Chen XG, Hu ZD. Sensitive determination of ephedrine and
pseudoephedrine by capillary electrophoresis with laser-induced fluorescence detection.
Analyst 2003;128(4):369. [The title technique was applied to the analysis of ephedra
and ephedra preparations.]

282) Zhang JY, Xie JP, Liu JQ, Tian JN, Chen XG, Hu ZD. Microemulsion electrokinetic
chromatography with laser-induced fluorescence detection for sensitive determination of
ephedrine and pseudoephedrine. Electrophoresis 2004;25(1):74. [The two substrates
were derivatized with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazol prior to analysis. The
technique was applied to Chinese traditional herbal preparations.]

Phenylpropanolamine:

283) Rind FMA, Khuhawar MY, Rajper AD. HPLC determination of phenylpropanol-amine
in pharmaceutical preparations using 4-dimethylaminobenzaldehyde as a derivatizing
reagent. Journal of Pharmaceutical and Biomedical Analysis 2001;26(2):331.

Other Adulterants/Diluents (including mixtures containing Ephedrine and/or

Pseudoephedrine):

284) Chen W, Liu F, Zhang X, Li KA, Tong S. The specificity of a chlorphenamine-imprinted

polymer and its application. Talanta 2001;55(1):29 [Note: chlorphenamine =
chlorpheniramine].

285) Garcia A, Ruperez FJ, Marin A, delaMaza A, Barbas C. Poly(ethyleneglycol) column for
the determination of acetaminophen, phenylephrine and chlorpheniramine in
pharmaceutical formulations. Journal of Chromatography B - Analytical Technologies in
the Biomedical and Life Sciences 2003;785(2):237. [Presents a rapid, isocratic HPLC
method for determination of the three title compounds in cold medications. UV detection
at 215 nm and 310 nm was used.]

286) Geer LC, Hays PA. Letrozole (Femara®) Microgram Journal 2003;1(3-4):190.
[Presents analytical data (GC/MS, FTIR, and NMR) for the title compound.]

287) Laasonen M, Harmia-Pulkkinen T, Simard C, Rasanen M, Vuorela H. Development and

validation of a near-infrared method for the quantitation of caffeine in intact single
tablets. Analytical Chemistry 2003;75(4):754. [Presents a technique for analyzing
pharmaceutical products containing primarily caffeine.]

288) Mabrouck MM, ElFatatry HM, Hammad S, Wahbi AAM. Simultaneous determination of
loratadine and pseudoephedrine sulfate in pharmaceutical formulation by RPLC and
derivative spectrophotometry. Journal of Pharmaceutical and Biomedical Analysis
2003;33(4):597. [Presents an HPLC method (using first derivative spectrophotometric
detection) for analysis of the title compounds in pharmaceuticals. Note that loratadine is
the active ingredient in prescription Claritin.]

244
289) Marin A, Garcia E, Garcia A, Barbas C. Validation of a HPLC quantification of
acetaminophen, phenylephrine and chlorpheniramine in pharmaceutical formulations:
Capsules and sachets. Journal of Pharmaceutical and Biomedical Analysis
2002;29(4):701. [Presents the simultaneous determination and quantitation of the title
compounds (and also phenylpropanolamine) in various pharmaceutical formulations.]

290) Metwally FH. Kinetic spectrophotometric methods for the quantitation of triprolidine in
bulk and in drug formulations. Journal of Pharmaceutical and Biomedical Analysis
2001;26(2):265.

291) Qi ML, Wang P, Zhou L, Sun Y. Simultaneous determination of four active components
in a compound formulation by liquid chromatography. Chromatographia 2003;58(3-
4):183. [Describes a rapid and accurate LC method for determination of
pseudoephedrine, acetaminophen, dextromethorphan, and diphenhydramine, in a
compound formulation.]

292) Qi ML, Wang P, Zhou L, Gu JL, Fu RN. Simultaneous determination of acetaminophen,

detromethorphen [sic] and pseudoephedrine hydrochloride in a new drug formulation for
cold treatment by HPLC. Chromatographia 2003;57(3-4):139. [Presents a validated
method for the referenced analysis, which is completed in less than 10 minutes per run.]

293) Rothchild R. Identification of a heroin diluent: One- and two-dimensional proton and
carbon-13 NMR studies of procaine hydrochloride: Computational studies of procaine
and its conjugate acid. Spectroscopy Letters 2003;36(1&2):35. [Presents the isolation
(from a street sample of heroin) and identification of the title compound, and also
presents ab initio molecular modeling calculations.]

294) Suntornsuk L, Pipitharome O, Wilairat P. Simultaneous determination of paracetamol

and chlorpheniramine maleate by micellar electrokinetic chromatography. Journal of
Pharmaceutical and Biomedical Analysis 2003;33(3):441. [For analysis of cold tablets.]

295) Zhang S, Zhuang YF, Ju HX. Flow-injection chemiluminescence determination of

papaverine using cerium(IV)-sulfite system. Analytical Letters 2004;37(1):143. [The
method is adequate for determination of papaverine in both pharmaceuticals and
biological fluids.]

Theophylline:

296) Huan L, Kan Q, Wang X, Lui X, Bi K. Simultaneous determination of the contents of

five components in compound theophyllini [sic] tablets by statistical-simulation
spectrometry. Huaxue Fenxi Jiliang 2002;11(4):11. [Compounds determined included
amidopyrine [sic], phenacetine [sic], theophylline, theobromine, and caffeine.]

297) Senturk Z, Erk N, Ozkan SA, Akay C, Cevheroglu S. Determination of theophylline and
ephedrine HCl in tablets by ratio-spectra derivative spectrophotometry and LC. Journal
of Pharmaceutical and Biomedical Analysis 2002;29(1-2):291.

245
New and/or Improved Instrumental Techniques

Capillary Electrophoresis (and Related Techniques, including Tandem Techniques):

298) Altria KD, Elder D. Overview of the status and applications of capillary electrophoresis
to the analysis of small molecules. Journal of Chromatography A 2003;1023(1):1. [A
review of the literature, 1999 - 2002, including forensic applications (not specified in
abstract).]

299) Descroix S, Varenne A, Geiser L, Cherkaoui S, Veuthey J-L, Gareil P. Influence of

electrolyte nature on the separation selectivity of amphetamines in nonaqueous capillary
electrophoresis: Protonation degree versus ion pairing effects. Electrophoresis
2003;24(10):1577. [Presents the title analysis as applied to ecstasy and (unspecified)
derivatives.]

300) Hilhorst MJ, Somsen GW, deJong GJ. Capillary electrokinetic separation techniques for
profiling of drugs and related products. Electrophoresis 2001;22(12):2542.

301) Issaq HJ. Thirty-five years of capillary electrophoresis: Advances and perspectives.
Journal of Liquid Chromatography and Related Technologies. 2002;25(8):1153. [An
overview of the development of CE, including forensic applications for analysis of illicit
drugs.]

302) Javerfalk-Hoyes E. Development of methods in CE, CE-MS, and MS/MS: Applications

in pharmaceutical, biomedical, and forensic sciences. Diss. Abstr. Int., C 2002;63(1):77.

303) Lemos NP, Bortolotti F, Manetto G, Anderson RA, Cittadini F, Tagliaro F. Capillary
electrophoresis: A new tool in forensic medicine and science. Science Justice
2001;41(3):203.

304) Schmitt-Kopplin P, Frommberger M. Capillary electrophoresis - mass spectrometry; 15

years of developments and applications. Electrophoresis 2003;24(22-23):3837. [An
overview and review.]

305) Sherma J. A field guide to instrumentation: Capillary electrophoresis. Inside Laboratory

Management (AOAC International) 2003;7(1):19. [Presents an overview of the
technique, and a brief review of recent advances in commercial CE instrumentation.]

306) Tavares MFM, Jager AV, da Silva CL, Moraes EP, Pereira EA, de Lima EC, Fonseca FN,
Tonin FG, Micke GA, Santos MR, de Oliveira MAL, de Moraes MdLL, van Kampen
MH, Fujiya NM. Applications of capillary electrophoresis to the analysis of compounds
of clinical, forensic, cosmetological, environmental, nutritional and pharmaceutical
importance. Journal of the Brazilian Chemical Society 2003;14(2):281.

307) Thormann W, Lurie IS, McCord B, Marti U, Cenni B, Malik N. Advances of capillary
electrophoresis in clinical and forensic analysis (1999-2000). Electrophoresis
2001;22(19):4216. [A general review article, covering the CE analyses of a wide variety
of substrates of forensic interest.]

308) Weinberger R. The evolution of capillary electrophoresis. American Laboratory

2002;34(10):32. [A general overview and review.]

246
Gas Chromatography (and Tandem GC Techniques):

309) Chang W-T, Lin DL, Liu RH. Isotopic analogs as internal standards for quantitative
analyses by GC/MS – Evaluation of cross-contribution to ions designated for the analyte
and the isotopic internal standard. Forensic Science International 2001;121(3):174.
[Focus is on drugs and metabolites in biological matrices.]

310) Dallabetta-Keller T. Trace analysis by GC/MS using pulsed splitless injections.

Proceedings - NOBCChE 2001;28:4. [A pressure pulsed injection technique for GC/MS
allows for enhanced detection of trace level controlled substances.]

311) Gorecki T, Harynuk J, Panic O. Comprehensive two-dimensional gas chromatography

(GC x GC). New Horizons and Challenges in Environmental Analysis and Monitoring
[Workshop], Gdansk, Poland, Aug. 18-29, 2003, pps 61-83. [Presented examples include
(unspecified) forensic samples.]

312) Matsuda K, Nakatoh S, Minatogawa Y, Suzuki K, Kimura H, Yamamoto S, Kohama A,

Tohyama K. Development of a GC/MS library for analyzing pesticides and drugs.
Rinsho Byori 2003;51(10):63871009-B963. [Presents the development of a library with
20 pesticides and herbicides, and 57 drugs (not specified in the abstract).]

High-Performance Liquid Chromatography (and tandem HPLC techniques):

313) Conemans JMH, Van Der Burgt AAM, Van Rooij JML, Pijnenburg CC. The
simultaneous determination of illicit drugs with HPLC-DAD. Bull TIAFT
2004;34(1):11. [The presented method is applied to drug powders, various dosage forms,
and various biological matrices, in a clinical setting.]

314) De Boeck G, Wood M, Samyn N. Recent applications of LC-MS in forensic science.

LC-GC 2002;15(11):19. [An overview of the use of LC/MS in forensic science (illicit
drugs are not specifically covered).]

315) Flanagan RJ, Harvey EJ, Spencer EP. HPLC of basic drugs on microparticulate strong
cation-exchange materials – A review. Forensic Science International 2001;121(1-2):97.

316) Nakashima K. Determination of stimulants by HPLC. Japanese Journal of Forensic

Toxicology 2003;21(3):197. [A review of the use of HPLC and common detection
systems.]

317) Perrin C, Matthijs N, Mangelings D, GranierLoyaux C, Maftouh M, Massart DL,

VanderHeyden Y. Screening approach for chiral separation of pharmaceuticals; Part II.
Reversed-phase liquid chromatography. Journal of Chromatography A 2002;966(1-
2):119. [A screening strategy for the rapid separation of drug enantiomers by reversed-
phase liquid chromatography is presented. Results for 37 diverse chiral pharmaceuticals
are presented (the specific products were not detailed in the abstract).]

318) Perrin C, Vu VA, Matthijs N, Maftouh M, MassartDL, VanderHeyden Y. Screening

approach for chiral separation of pharmaceuticals. Part 1. Normal-phase liquid
chromatography. Journal of Chromatography A 2002;947(1):69.

247
319) Sagmuller B, Schwarze B, Brehm G, Trachta G, Schneider S. Identification of illicit
drugs by a combination of liquid chromatography and surface-enhanced Raman scattering
spectroscopy. Journal of Molecular Structure 2003;661-662:279. [Presents a novel
HPLC-SERS technique for analysis of illicit drugs (not specified in abstract).]

320) Sherma J. High-performance liquid chromatography/mass spectrometry analysis of

botanical medicines and dietary supplements: A review. J Assoc Off Anal Chem
2003;86(5):873. [Includes discussion of related techniques.]

321) Sychev KS, Sychev SN. Application of universal mobile phases in high-effective liquid
chromatography for analysis of the objects of food industry, criminology and
pharmaceutical chemistry. Zavodskaya Laboratoriya, Diagnostika Materialov
2003;69(9):8. [Various diethylammonium based run buffers are examined for RP-
HPLC.]

322) Xiang Y, Wu N, Lippert JA, Lee ML. Separation of chiral pharmaceuticals using
ultrahigh pressure liquid chromatography. Chromatographia 2002;55(7-8):399.

Inductive Coupled Plasma- Mass Spectrometry (ICP-MS):

323) Almirall JR, Furton KG. New approaches to forensic chemical analysis. Proceedings,
16th International Symposium on the Forensic Sciences, Canberra 2002(16):(No pps
given). [An overview of SPME and ICP/MS methodologies.]

324) Cottingham K. ICPMS: It’s elemental. Analytical Chemistry 2004;76(1):35A. [An

overview of the title topic.]

325) Smith WD. Controversy over forensic ICPMS method. Analytical Chemistry
2002;74(15):411A.

Infrared and Raman Spectroscopy:

326) Bartick E. Forensic analysis by Raman spectroscopy: An emerging technology.

Proceedings of the 16th Meeting of the International Association of Forensic Sciences,
Montpellier, France, September 2-7, 2002, pps 45-50. [A general introduction and
review of Raman for forensic analysis.]

327) Enculescu AL, Steiginga JR. Raman spectroscopy - A powerful tool for non-routine
analysis of pharmaceuticals. American Pharmaceutical Review 2002;5(1):81. [A minor
review of the title technique, with an emphasis on non-routine pharmaceutical samples.]

328) Ishihara A, Nakamura H. Qualitative and quantitative analysis of principal ingredients in

tablets by near-infrared spectroscopy. Bunseki Kagaku 2002;51(10):899. [Presents a
study of NIRS for qualitative and quantitative analyses of the principal ingredients in
tablets (for forensic purposes).]

329) Jarman JL, Seerley SI, Todebush RA, de Haseth JA. Semiautomated depositor for
infrared microspectrometry. Applied Spectroscopy 2003;57(9):1078. [Presents a novel
method for depositing minute samples for IR microspectrometry (the authors suggest
applicability to forensic analyses).]

330) Ryder AG. Classification of narcotics in solid mixtures using principal component
analysis and Raman spectroscopy. Journal of Forensic Sciences 2002;47(2):275.

248
Ion Spectroscopy:

331) Aristarkhova AA, Volkov SS, Dmitrevskii YE, Kitaeva TI, Ognev VI, Plotkin DM,
Timashev MY. Characteristics of ion spectroscopy use in forensic science [sic].
Vzaimodeistvie Ionov s Poverkhnost’yu Materialy Mezhdunarodnoi Konferentsii, 15th,
Zvenigorod, Russian Federation, Aug. 27-31, 2001 2001;1:335. [A review on the use of
ion spectroscopic methods in forensic science.]

332) Derringer B, Leigh T. Solving problems in ion mobility measurements of forensic

samples with thermal desorption and dynamic modeling. Dissertations Abstracts
International B 2003;64(4):1715.

Mass Spectrometry:

333) Aebi B, Bernhard W. Advances in the use of mass spectral libraries for forensic
toxicology. Journal of Analytical Toxicology 2002;26(3):149.

334) Libong D, Pirnay S, Bruneau C, Rogalewicz F, Ricordel I, Bouchonnet S. Adsorption-

desorption effects in ion trap mass spectrometry using in situ ionization. Journal of
Chromatography A 2003;1010(1):123. [Quadrupole mass spectrometers were compared
for the GC/MS analyses of diazepam, alprazolam, triazolam, LSD, trimethylsilylated
LSD, and trimethylsilylated buprenorphine.]

335) Yinon J. Advances in forensic applications of mass spectrometry. CRC Press LLC:Boca
Raton, FL, 2004.

Microchip Technology:

336) Anonymous. Forensic sample analysis on a microchip. Analytical Chemistry

2004;76(7):117A.

337) Belder D, Deege A, Maass M, Ludwig M. Design and performance of a microchip

electrophoresis instrument with sensitive variable-wavelength fluorescence detection.
Electrophoresis 2002;23(14):2355. [A modular instrument for high-speed microchip
electrophoresis equipped with a sensitive variable-wavelength fluorescence detection
system was developed and evaluated using fluorescein isothiocyanate (FITC)-labelled
amines, including amphetamine.]

338) Felton MJ. Lab on a chip: Poised on the brink. Analytical Chemistry
2003;75(23):505A. [A review of the topic, and an overview of the available
instrumentation in the field.]

339) Harris CM. Shrinking the LC landscape. Analytical Chemistry 2003;75(3):65A. [A

conversational overview of recent developments in chip-based technologies.]

340) Schwarz MA, Hauser PC. Rapid chiral on-chip separation with simplified amperometric
detection. Journal of Chromatography A 2001;928(2):225.

341) Verpoorte E. Microfluidic chips for clinical and forensic analysis. Electrophoresis
2002;23(5):677.

249
Nuclear Magnetic Resonance Spectroscopy:

342) Tishmack PA, Bugay DE, Byrn SR. Solid-state nuclear magnetic resonance spectroscopy
- pharmaceutical applications. Journal of Pharmaceutical Sciences 2003;92(3):441. [A
minor review of the title topic, focusing on solid pharmaceutical drug formulations.]

Osmolality:

343) Wesley JF. Osmolality - A novel and sensitive tool for detection of tampering of
adulterated with ethanol, gamma-butyrolactone, and 1,4-butanediol, and for detection of
dilution-tampered demerol syringes. Microgram Journal 2003;1(1-2):8. [Presents the
title technique and various real-world applications.]

Solid Phase Micro-Extraction:

344) Liu B, Chang Y. Solid-phase microextraction and its application in the analysis of drugs
of abuse. Zhongguo Yaowu Yilaixing Zazhi 2002;11(4):313. [A review of the title
topic.]

345) Vas G, Vekey K. Solid-phase microextraction: A poweful sample preparation tool prior
to mass spectrometric analysis. Journal of Mass Spectrometry 2004;39(3):233. [An
overview and review of SPME.]

Thin Layer Chromatography

:
346) Azoury M, Zelkowicz A, Goren Z, Almog J. Evaluation of ninhydrin analogues and
other electron-deficient compounds as spray reagents for drugs on thin layer
chromatograms. Microgram Journal 2003;1(1-2):23.

347) Spangenberg B, Ahrens B, Klein KF. TLC analysis in forensic sciences using a diode
array detector. Chromatographia 2001;53(Part 2, Suppl S):S438.

348) Spangenberg B, Ahrens B, Klein K-F. Diode-array HPTLC in forensic sciences. GTFCh
Symposium: Toxikologische Aspekte der Sterbehilfe - Neue Drogen: Chemische,
Analytische und Toxikologische Aspekte, Beitraege zum Symposium der Gesellschaft
fuer Toxikologische und Forensische Chemie, 12th, Mosbach, Germany, April 26-28,
2001, pps 356-61, 2001. [The primary focus is forensic analysis of biological matrices.]

X-Ray based Techniques:

349) Muratsu S. An application of synchrotron radiation to the analysis of forensic samples,

mainly drugs of abuse. Bunseki Kagaku 2003;52(11):1061.

350) Rendle DF. Use of X-rays in the United Kingdom Forensic Science Service. Advances
in X-ray Analysis 2003;46:17. [Presents four case studies, including the use of XRD in
the analysis of “street drug seizures” (not specified in the abstract)]

250
Portable Detection and Analytical Instrumentation

351) Allen WC. Method of analyzing the constituents of air extracted from the interior of a
piece of luggage. U.S. Pat. Appl. Publ. US 20040035185 A1 26 Feb 2004, 17 pp.
CLASS: ICM: G01N033-22. NCL: 073031020; 073863810. APPLICATION: US
2002-224688 21 Aug 2002. [The primary application is for explosives, but the technique
can be applied to drugs.]

352) Bannister WW, Chen C-C, Curby WA, Chen EB, Damour PL, Morales A. Thermal
analysis for detection and identification of explosives and other controlled substances.
U.S. US 6406918 B1 18 June 2002. [Includes identification of illicit drugs (i.e., in
addition to explosives).]

353) Barzilov AP, Womble PC, Vourvopoulos G. NELIS - A neutron inspection system for
detection of illicit drugs. AIP Conference Proceedings 2003;680:939. [For inspection of
cargo pallets.]

354) Brestel M, Gft M, Sharon U. Controlled substance detection and identification system.
U.S. Pat. Appl. Publ. US 20040051867 A1 18 Mar 2004. CLASS: ICM: G01J003-44.
ICS: G01J003-30. NCL: 356318000; 356301000. APPLICATION: US 2003-428398 2
May 2003. PRIORITY: IL 2002-151745 12 Sep 2002. [The controlled substances not
specified in abstract.]

355) Buryakov IA, Kolomiets YN. Rapid determination of explosives and narcotics using a
multicapillary-column gas chromatograph and an ion-mobility spectrometer. Journal of
Analytical Chemistry - Russia (translation of Zhurnal Analiticheskoi Khimii)
2003;58(10):944. [The title technique was applied to detection of heroin, cocaine HCl
and cocaine base (crack).]

356) Buryakov IA. Express analysis of explosives, chemical warfare agents, and drugs with
multicapillary column gas chromatography and ion mobility increment spectrometry.
Journal of Chromatography B - Analytical Technologies in the Biomedical and Life
Sciences 2004;800(1-2):75. [The title technique was applied to analysis of heroin,
cocaine hydrochloride, and cocaine base.]

357) Cottingham K. Ion mobility spectrometry rediscovered. Analytical Chemistry

2003;75(19):435A. [A mini-review of IMS, focusing on potential applications in
proteomics. Includes an overview of current instrumentation.]

358) Halamek J, Makower A, Skladal P, Scheller FW. Highly sensitive detection of cocaine
using a piezoelectric immunosensor. Biosensors and Bioelectronics 2002;17(11-
12):1045. [Presents a rugged, highly sensitive competitive immunoassay-based
piezoelectric sensor for cocaine.]

359) Hallowell SF. Screening people for illicit substances: A survey of current portal
technology. Talanta 2001;54(3):447.

360) Harris CM. GC to Go. Analytical Chemistry 2002;74(21):585A. [A minor review of

the current status of portable GC and GC/MS instrumentation.]

251
361) Harris CM. Raman on the run. Analytical Chemistry 2003;75(3):75A. [A
conversational overview of recent developments in portable Raman, including a
comparative listing of five commercially available instruments.]

362) Kiraly B, Sanami T, Doczi R, Csikai J. Detection of explosives and illicit drugs using
neutrons. Nuclear Instruments & Methods in Physics Research, Section B: Beam
Interactions with Materials and Atoms 2003;213:452. [Presents a Thermal Neutron
Activation technique for the title analyses. The “illicit drugs” were not specified in the
abstract.]

363) Kuo C, Nagarajan R, Bannister WW, Loder RA, Furry JW, Chen C-C. Detection of
concealed explosives and drugs by thermal analysis and thermal profiles of samples with
microsensors. PCT Int. Appl. WO 2004027386 A2 1 Apr 2004. CLASS: ICM: G01N.
APPLICATION: WO 2003-US29741 22 Sep 2003. PRIORITY: US 2002-PV412619
20 Sep 2002. [Presents the title patent (the explosives and drugs were not specified in the
abstract).]

364) Litman MA. Rapid-acting drug analysis system. U.S. Pat. Appl. Publ. US 2003 224,474
(Cl. 435-28; C12Q1/28), 4 Dec US Appl. PV 383,840, 30 May 2002. [Appears to be a
methodology for detecting date-rape type drugs in liquids.]

365) Nguyen DH, Berry S, Geblewicz JP, Couture G, Huynh P. Chemiluminescent detection
of explosives, narcotics, and other chemical substances. U.S. Pat. Appl. Publ. US
20040053421 A1 18 Mar 2004. CLASS: ICM: G01N021-76. NCL:
436172000;436164000; 436117000; 436155000; 436159000; 422052000; 422078000;
422080000;422082050; 422082080. APPLICATION: US 2002-241407 12 Sep 2002.
[The narcotics not specified in abstract.]

366) Ochoa ML, Harrington PB. Detection of methamphetamine in the presence of nicotine
using in situ chemical derivatization and ion mobility spectrometry. Analytical
Chemistry 2004;76(4):985.

367) Smith WD. SAW chip sniffs out cocaine. Analytical Chemistry 2003;75(23):492A.
[Presents an overview of the use of surface acoustic wave based devices for detecting
cocaine vapor or particulates.]

368) Stojanovic MN, Landry DW. Aptamer-based colorimetric probe for cocaine. Journal of
the American Chemical Society 2002;124(33):9678.

369) Stubbs DD, Lee S-H, Hunt WD. Cocaine detection using surface acoustic wave
immunoassay sensors. Proceedings of the IEEE International Frequency Control
Symposium & PDA Exhibition, New Orleans, LA, United States, May 29-31, 2002, 289-
298. [Presents a study of real-time, vapor-phase detection of cocaine using a specialized
SAW device.]

370) Stubbs DD, Lee SH, Hunt WD. Investigation of cocaine plumes using surface acoustic
wave immunoassay sensors. Analytical Chemistry 2003;75(22):6231. [Presents the
results of a series of experiments demonstrating real-time vapor phase detection of
cocaine in the gas phase with SAW-based instruments.]

252
Miscellaneous

Analytical Artifacts:

371) Varshney K-M. HPTLC study of the stability of heroin in methanol. Journal of Planar
Chromatography 2002;15(1):46. [Presents the results of a degradation study of heroin in
methanol (at room temperature). The results indicate degradation is measurable on Day
2, and is complete in around 38 weeks.]

Chemometrics:

372) Praisler M, Van Bocxlaer J, De Leenheer A, Massart DL. Chemometric detection of

thermally degraded samples in the analysis of drugs of abuse with gas chromatography-
Fourier-transform infrared spectroscopy. Journal of Chromatography A 2002;962(1-
2):161. [For the identification of the reference standard peak in cases where the GC-
FTIR analysis gives multiple peaks.]

Cocaine:

373) Brachet A, Rudaz S, Mateus L, Christen P, Veuthey J-L. Optimisation [sic] of

accelerated solvent extraction of cocaine and benzoylecgonine from coca leaves. Journal
of Separation Science 2001;24(10-11):865. [A variety of extraction parameters were
varied to achieve the optimal results. Analysis was conducted by GC/FID and CE with
UV detection.]

374) Tanaka S, Lio R, Chinaka S, Takayama N, Hayakawa K. Analysis of reaction products

of cocaine and hydrogen peroxide by high performance liquid chromatography/mass
spectrometry. Biomedical Chromatography 2002;16(6):390. [Various hydroxy and
dihydroxy cocaines were identified.]

Counterfeit Drugs:

375) Rudolf PM, Bernstein IBG. Counterfeit drugs. New England Journal of Medicine
2004;350:1384.

376) Scafi SHF, Pasquini C. Identification of counterfeit drugs using near-infrared

spectroscopy. Analyst 2001;126(12):2218.

Dragon’s Blood:

377) Edwards HGM, de Oliveira LFC, Prendergast HDV. Raman spectroscopic analysis of
Dragon’s Blood resins - Basis for distinguishing between Dracaena (Convallariaceae),
Daemonorops (Palmae), and Croton (Euphorbiaceae). Analyst 2004;129(2):134.

378) Hu Y, Ning Z, Liu D. Determination of pterostilbene in Dragon’s Blood by RP-HPLC.

Yaowu Fenxi Zazhi 2002;22(6):428.

379) Hu Y, Zhang J, Liu C-h, Deng C. Difference of Dragon’s Blood from different extract
processing. Zhongcaoyao 2002;33(8):697. [Analysis by TLC, UV, and HPLC.]

253
380) Hu Y, Li L, Han H. HPLC determination of loureirin A and B in Dragon’s Blood.
Yaowu Fenxi Zazhi 2003;23(1):7. [Presents an HPLC/UV method for detection of the
title compounds.]

Drugs on Currency:

381) Jenkins AJ. Drug contamination of US paper currency. Forensic Science International
2001;121(3):189. [Includes cocaine, heroin, 6-monoacetylmorphine, morphine, codeine,
methamphetamine, amphetamine, and phencyclidine, by GC/MS.]

382) Jourdan TH, Malak K, Cavett V, Eckenrode BA. Continuing exploration of cocaine
contamination of U.S. currency. Proceedings of the American Academy of Forensic
Sciences 2003;9:33. [An overview of this issue.]

Heroin:

383) Brazier JS, Morris TE, Duerden BI. Heat and acid tolerance of Clostridium novyi Type A
spores and their survival prior to preparation of heroin for injection. Anaerobe
2003;9(3):141. [Presents the title study. This study was in followup to the outbreak of
clostridium illnesses and deaths in the United Kingdom as a result of the use of
contaminated heroin. The results indicate that typical heroin preparation procedures (by
abusers) are not adequate to kill the spores.]

Khat:
384) Al-Motarreb A, Baker K, Broadley KJ. Khat: Pharmaceutical and medical aspects and
its social use in Yemen. Phytotherapy Research 2002;16:403. [An overview of the
history, cultivation, and constituents of khat; however, the primary focus is
pharmacological.]

Methamphetamine:

385) Yudko E, Hall HV, McPherson SB, Eds. Methamphetamine use: Clinical and forensic
aspects. CRC Press LLC: Boca Raton, Fla.) 2003.

Qualitative Tests:

386) Deakin AL. A study of acids used for the acidified cobalt thiocyanate test for cocaine
base. Microgram Journal 2003;1(1-2):40. [A study of the use of substitute acids for
concentrated hydrochloric acid in the referenced test, with recommendations.]

387) Friedman AJ. Method for identification of flunitrazepam. U.S. US 6713306 B1 30 Mar
2004. CLASS: ICM: G01N033-00. NCL: 436096000; 436106000;436164000;
436150000; 436901000. APPLICATION: US 2001-946225 5 Sep 2001. [Presents a
field method for detection of flunitrazepam in a sample (few details provided in the
abstract).]

388) Glattstein O, Glattstein B. A method for the detection of compounds comprising

methylenedioxyphenyl and testing kit for the same. PCT Int. Appl. WO 2003052426 A1
26 Jun 2003, 22 pp. CLASS: ICM: G01N033-94. APPLICATION: WO 2002-IL1024
19 Dec 2002. PRIORITY: IL 2001-147185 19 Dec 2001.

254
389) Makarov SA, Simonov EA, Makarov VG, Kozlov AS. Method for determination of
narcotic, psychotropic and offensive substances of plant and synthetic origin. Russ. RU
2,205,385 (Cl. G01N21/78) 27 May 2003, Appl. 2,002,103,845, 18 Feb 2002. [Appears
to present a narcotics test kit (abstract is not clear).]

390) Murray RA, Doering PL, Merves ML, McCusker RR, Chronister CW, Goldberger BA.
Putting an ecstasy test kit to the test. Proceedings of the American Academy of Forensic
Sciences 2003;9:307. [Presents a study of the DanceSafe ecstasy testing kit.]

391) Murray RA, Doering PL, Boothby LA, Merves ML, McCuster RR, Chronister CW,
Goldberger BA. Putting an Ecstasy test kit to the test: Harm reduction or harm
induction? Pharmacotherapy 2003;23(10). [Presents a critical analysis and evaluation of
the DanceSafe Complete Adulterant Screening Kit for Ecstasy®.

392) Zhang H, Tang J, Liu Y, Shao W, Fan X, Qin Y. Method and test paper for semi-
quantitative detection of drugs/medicine by color band-degressive immunological
chromatography. Faming Zhuanli Shenqing Gongkai Shuomingshu CN 1,381,729 (Cl.
G01N33/558), 27 Nov 2002, Appl. 2,002,114,110, 30 Apr 2002. [The title methodology
was applied to over 24 drugs.]

Quality Assurance:

393) Chang W-T, Chiu J, Liang Y-H, Liu RH. Characteristics of calibration curve resulting
from the use of an H2-analog of the analyte as the internal standard – Methamphetamine
example. Proceedings of the American Academy of Forensic Sciences 2002;8:275.
[Presents a discussion of the causes of deviations in the referenced calibration curve.]

394) Chang W-T, Smith J, Liu RH. Isotopic analogs as internal standards for quantitative
GC/MS analysis - Molecular abundance and retention time differences as interference
factors. Journal of Forensic Sciences 2002;47(4):873. [Isotopic analogues of five
barbiturates were evaluated as internal standards.]

395) Coyle HM, Neylon S, Ladd C, Palmbach T, Lee HC. Validation of the AFLP technique
for the individualization of marijuana (C. sativa L.) samples. Proceedings of the
American Academy of Forensic Sciences 2002;8:68. [Presents the results of the
referenced validation study.]

396) Epstein DM, Tebbett IR, Boyd SE. Eliminating sources of pipetting error in the forensic
laboratory. Forensic Science Communications 2003;5(4):No Page Number (Internet
Reference: www.fbi.gov/hq/lab/fsc/current/index.htm) [Presents an overview of the
potential sources of error when utilizing air-displacement pipettes.]

397) Hibbert DB. Scientist vs the law. Accreditation and quality assurance 2003;8(5):179.
[Presents an analysis of an Australian court case where convicted clandestine laboratory
operators were acquitted on appeal due to alleged shortcomings in the laboratory’s
standard operating procedures.]

398) Liu RH, Lin D-L, Chang W-T, Liu C, Tsay W-i, Li J-H, Kuo T-L. Isotopically labeled
analogues for drug quantitation. Analytical Chemistry 2002;74(23):618A.

255
399) Moeller MR. Forensic conclusiveness and quality assurance of toxicological results.
Research in Legal Medicine 2003;30:55. [An overview of the legal consequences of
toxiciological analyses.]

400) Poortman Van Der Meer AJ, Van Egmond HE. Quantitation of amphetamine-type
compounds for which no reference compound is available: The validation of a theoretical
model. Science Justice 2001;41(3):185.

Sampling Plans:

401) Coulson SA, Coxon A, Buckleton JS. How many samples from a drug seizure need to be
analyzed? Journal of Forensic Sciences 2001;46(6):1456.

Surveys and Overviews:

402) Anonymous. Poppers, ketamine, and GHB. Drugscope Drug Notes 2002(9):1 [A
generic overview of the title compounds.]

403) Baylor MR, Wong L, Sapienza FL, Strom KJ, Rachal V. National Forensic Laboratory
Information System: 2003 data analysis. Proceedings of the American Academy of
Forensic Sciences 2004;10:75. [An overview of NFLIS.]

404) Briellmann TA, Dussy FE, Bovens MG. Forensic analysis of heroin and cocaine
seizures. Chimia 2002;56:74. [Presents a survey and overview of seizures in
Switzerland (date range not specified in abstract).]

405) Chuang S-F, Tsay W-I, Li J-H, Sun M-P, Hsieh S-S, Yang Y-T, Hsu J-F, Wun J-H, Lee
T-C, Lin D-L, Liu J-T, Liu RH.. Characteristics and trends of MDMA and MDMA-
alleged samples seized in Taiwan during the period of January 2000 – May 2001.
Proceedings of the American Academy of Forensic Sciences 2002;8:57. [A survey of
MDMA/ketamine abuse and seizures for the referenced time frame.]

406) Corkery JM, Airs J. Seizures of drugs in the UK 2001. Home Office Findings
2003;202:1. [Presents a survey of Class A, B, and C drug seizures made in the U.K.
during 2001.]

407) Freeman S, Alder JF. Arylethylamine psychotropic recreational drugs: A chemical

perspective. European Journal of Medicinal Chemistry 2002;37(7):527. [A review of
drug web sites and literature, and review, with a comparison versus the scientific and
regulatory literature.]

408) King LA. New synthetic drugs in the European Union. Science Justice 2001;41(3):200.

409) King L. What’s in a drug? Druglink 2003;18(4):21. [A minor survey of the typical
contents of illicit drugs in the United Kingdom.]

410) Laing RR. Hallucinogens: A forensic drug handbook. Elsevier Science Ltd.: London,
UK, 290 pp.

411) Logan BK. Amphetamines: An update on forensic issues. Journal of Analytical

Toxicology 2001;25(5):400.

256
412) Lora-Tamayo C, Tena T, Rodriguez A, Moreno D, Sancho JR, Ensenat P, Muela F. The
designer drug situation in Ibiza. Forensic Science International 2004;140(2-3):195.
[Presents a survey of designer drugs used on Ibiza Island, based on analyses of urine and
serum samples.]

413) Liu J-T, Liu RH. Enantiomeric composition of abused amine drugs: Chromatographic
methods of analysis and data interpretation. Journal of Biochemical and Biophysical
Methods 2002;54(1-3):115. [A review describing various chromatographic methods for
the enantiomeric analyses of various amine drugs, concentrating on amphetamine and
methamphetamine.]

414) Lua AC, Lin B-F, Tseng Y-T, Chen T-H, Chen T-C, Chiang C-K. Drugs of abuse pattern
in Taiwan. Yaowu Shipin Fenxi 2002;10(1):69. [Presents a survey of drugs of abuse in
Taiwan based on samples collected from February 1997 to January 1998.]

415) Mostad A. Marijuana: The Devil’s little finger? Kjemi 2002;62(4):14. [A historical
overview of marijuana, plus a survey of the chemistry of cannabinoids.]

416) Myers S. Forensic science. Nature 2003;421(6925):872. [A minor overview of the

development of forensic DNA laboratories; includes some general comments of interest
on the “real-life value” of forensic laboratories.]

417) Nasiadka K, Rutkowska A, Brandys J. Hallucinogenic amphetamines.

Z-Zagadnien-Nauk-Sadowych 2002;52:64. [A (primarily) pharmacological overview.]

418) Newell CJ. Potency of cannabis seized in central Florida during June 2002. Microgram
Journal 2003;1(1-2):37. [A minor review of the title topic, that compares the results
versus the national statistics for 2002.]

419) Poon NL, Chong WC. Ecstasy in Hong Kong. Proceedings of the American Academy of
Forensic Sciences 2002;8:60. [An overview of the trends in ecstasy seizures in Hong
Kong, including a review of tablet characteristics that might be valuable in source
determinations.]

420) Porrata T. The Rave and Club Drug phenomenon: Dancing with darkness and danger.
Medical Legal Aspects of Drugs. Burns M, Ed. Lawyers and Judges Publishing
Co.:2003, Chapter 10 (pps. 253-278). [Presents an overview of the title topic, and
discusses its associated health and social problems.]

421) Salimov AA, Hajiyev SF. Contemporary state of narcotics expertise. Azerbaycan
Eczaciliq Jurnali 2002;2(1):23. [Appears to be a mini-review of the state of forensic
analysis of drugs in Azerbaijan (not clear in abstract).]

422) Schaefer T. Chemists in criminal technology. Nachrichten aus der Chemie

2004;52(2):223. [A mini-review covering criminalists and forensic chemists.]

423) Simonsen KW, Kaa E, Nielsen E, Rollman D. Narcotics at street level in Denmark. A
prospective investigation from 1995 to 2000. Forensic Science International
2003;131(2-3):162. [A survey of illicit drug seizures made in six selected police districts
in Denmark during the referenced time frame.]

257
424) van Zundert M. Travel-pills, ecstasy pills, or Grandma’s heart-rhythm pills?
Pharmaceutisch Weekblad 2002;137(51/52):1825. [Appears to be a conversational
overview presenting the use of TLC and GC for the identification of unknowns at a Dutch
emergency pill identification lab.]

425) Wadler GI. Future and designer drugs: Emerging science and technologies.
Performance-Enhancing Substances in Sport and Exercise 2002:305. [A review of
performance enhancing drugs, with a discussion of new developments.]

Other:

426) Altun A, Golcuk, Kumru M, Jalbout AF. Electron-conformational study for the structure-
hallucinogenic activity relationships of phenylalkylamines. Bioorganic & Medicinal
Chemistry 2003;11(18):3861. [A theoretical study of the topic.]

427) Ballou S, Goodpaster J, MacCrehan W, Reeder, D. Forensic Analysis. Analytical and

Bioanalytical Chemistry 2003;376(8):1149.

428) Bilia AR, Bergonzi MC, Lazari D, Vincieri FF. Characterization of commercial kava-
kava herbal drug and herbal drug preparations by means of nuclear magnetic resonance
spectroscopy. Journal of Agricultural and Food Chemistry 2002;50(18):5016. [NMR
was used to determine the kavalactones in both a finely powdered herbal drug and a
commercial extract.]

429) Day JS, Edwards HGM, Dobrowski SA, Voice AM. The detection of drugs of abuse in
fingerprints using Raman spectroscopy I: Latent fingerprints. Spectrochimica Acta, Part
A: Molecular and Biomolecular Spectroscopy 2004:60(3):563. [Codeine phosphate,
cocaine hydrochloride, amphetamine sulfate, barbital, nitrazepam, caffeine, aspirin,
paracetamol, starch, and talc were successfully identified in fingerprints using the title
technique.]

430) Dirbashi OY, Ikeda K, Takahashi M, Kuroda N, Ikeda S, Nakashima K. Drugs of abuse
in a non-conventional sample; detection of methamphetamine and its main metabolite,
amphetamine in abusers’ clothes by HPLC with UV and fluorescence detection.
Biomedical Chromatography 2001;15(7):457.

431) Garkani-Nejad Z, Karlovits M, Demuth W, Stimpfl T, Vycudilik W, Jalali-Heravi M,

Varmuza K. Prediction of gas chromatographic retention indices of a diverse set of
toxicologically relevant compounds. Journal of Chromatography A 2004;1028(2):287.
[Kovats retention indices for 846 compounds are presented.]

432) Harris HA, Newman MS, Montreuil RS, Goodrich JT. Comparison of extraction in a
drop and solid phase microextraction. Proceedings of the American Academy of
Forensic Sciences 2003;9:33. [Explains and compares the two referenced extraction
techniques. Drugs utilized include cocaine, phenylpropanolamine, brompheniramine, and
dextromethorphan.]

433) James SH, Nordby JJ, Eds. Forensic science: An introduction to scientific and
investigative techniques. CRC Press LLC: Boca Raton, FL.

434) Mausolf N. The name of the test. Microgram 2001;34(9):235. [On the Duquenois and
related tests for cannabis.]

258
435) Negrusz A, Gaensslen RE. Analytical developments in toxicological investigation of
drug-facilitated sexual assault. Analytical and Bioanalytical Chemistry
2003;376(8):1192. [A general overview of the drug-facilitated sexual assault
phenomenon, that discusses recent analytical/toxicological developments.]

436) Pitts SJ, Thomson CI. Analysis and classification of common vegetable oils. Journal of
Forensic Sciences 2003;48(6):1293. [Presents methods of analysis for canola, corn,
olive, peanut, safflower, soybean, and sunflower oils. (Although not stated, this study
may also have value in the analysis of preparations of steroids in oils.)]

437) Puschel K, Stein S, Stobbe S, Heinemann A. Analysis of 683 drug packages seized from
“body stuffers”. Forensic Science International 2004;140(1):109. [Presents a short
overview of the practice of internal carrying of controlled substances, with a discussion of
packaging and drug types, as observed in Hamburg, Germany.]

438) Sun Q. Novel method for identifying Chinese herbal medicine. Faming Zhuanli
Shenqing Gongkai Shuomingshu CN 1370839 A 25 Sept 2002, 6 pp. CLASS: ICM:
C12Q001-25. APPLICATION: CN 2001-104457 27 Feb 2001. [Presents an application
of PCR with Taq enzyme to identify Chinese herbal medications.]

439) Wong SK, Tsui SK, Kwan SY. Analysis of proprietary Chinese medicines for the
presence of toxic ingredients by LC/MS/MS. Journal of Pharmacology and Biomedical
Analysis 2002;30:161. [Presents the title analysis of 12 products.]

259
 Forensic Toxicology

— A Review: 2001 to 2004 —

Laboratoires de Police Scientifique (LPS) in FRANCE

Marie Hélène GHYSEL, Ph D; Florence DESCAMPS (Master in Science),

Emilie BESTEL(pharmacist)
LPS de Lille

Marie-Thérèse THEVENOT(pharmacist-biologist), Catherine COQUEL(pharmacist) ,

Stéphanie COURCELLES (engineer)
LPS d'Ecully (Lyon)

Pascale VISINONI (engineer), Carine DUPUIS (pharmacist)

LPS de Toulous

Name and adress of author responsible for correspondence about manuscript :

Marie Hélène GHYSEL, Ph D
Laboratoire de Police Scientifique
7 boulevard Vauban
F- 59000 Lille
France

260
CONTENTS

Introduction

Products

Alcohol & Volatils

Drugs of abuse :
new drugs, cannabis, opiates, cocaine, amphetamines, LSD, Phencyclidine,
GHB.
Miscellaneous ( carbon monoxide, cyanides, pesticides, metals)

Samples and specificity

Conventional : blood
Alternatives : hair, saliva, sweat, nails, vitreous humor
Adulterant

Analysis & apparatus

Colorimetric method
Immunoanalyse
Extraction
Progress in GC, LC, CE, RMN, ICP

Interpretation

Post-mortem redistribution
Quality of the conservation, degradation in vitro
Pharmacogenomic
Data on blood levels

Important items in forensic toxicology.

Alcohol, drugs & driving

Drug facilitate sexual assault
Doping
Legal medicine
Quality

Information Sources

Scientific literature
Web sources
Forensic toxicology societies

References

Abreviations.

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INTRODUCTION

Toxicology is a science always in movement. Toxicologists are charged with the responsibility
for detecting and identifying different kinds of drugs and poisons in the body. This challenge is
difficult and depends on the means in time, materials, and money. Advanced analytical
techniques have opened new frontiers to forensic toxicologists. It is now possible to examine
biological specimens with great resolution and selectivity to reveal substances at trace levels,
using increasingly sophisticated ways.

Here are reported novelties in toxicology. We have chosen to present the latest progresses and
recent papers concerning different categories: alcohol, drugs and miscellaneous poisons;
biological samples and specificities, analyses and apparatuses, questions of interpretation, varied
preoccupations regarding alcohol, drugs & driving, drug-facilitated sexual assaults, doping, legal
medicine, quality assurance and at last, information sources and toxicological societies.

PRODUCTS

Alcohol and volatils

A major branch of forensic toxicology deals with the measurement of alcohol in the body (1).
First of all, breath test devices. Many different types are available, with the choice depending on
the standard of proof required in each case, the support services available, and the associated
costs. A review of breath testing technology that outlines the history of this technique before
considering the various breath test devices available today have been published (2-4). These
devices include those based on wet chemistry, infrared detection, electrochemical techniques,
semiconductor sensors, and passive alcohol sensors (5) or new technologies as stick-type
enzyme electrode or Sol-gel MoO3-WO3 thin films for ethanol vapor sensing (6-10). These
apparatuses are evaluated (11-14).

At the time of the evaluation of the alcoholic impregnation in the expired air, some substances
can interfere with the taken measures. Studies have been presented on the influence of methyl
tert-butyl ether, acetone, oral hygiene liquids, citric acid and fructose (15-18) and the problem of
some pathologies as gastroesophageal reflux disease (19).

Ethanol concentration in the expired air is correlated with the blood concentration, however it is
necessary to hold account of the hours when the samples has been taken and of pharmacokinetic
of ethanol. Although it was the subject of Widmark's work at the beginning of the XX century,
it's still the subject of many studies (20-28).

Ethanol concentrations in blood are generally carried out by head space extraction and gas
chromatography coupled with flame ionization detector (HS-GC-FID), nevertheless other
technologies can be used, for example solid phase microextraction (SPME) and GC coupled with
mass detector (29-31) or the kit of detection of ethanol QED applicable to other biological
specimens (32-33).

In forensic medicine the ratios of ethanol concentration between various biological specimens
such as blood, saliva, urine, vitreous humour can help the forensic toxicologist in his
interpretations during the investigations into the death circumstances (34-39) and especially in
the case of postmortem ethanol formation (40).

Approximately 95% of ethanol undergoes oxidative metabolism, with a small percentage

undergoing non-oxidative one to generate products including fatty acid ethyl esters,

262
phosphatidylethanol and ethyl glucuronide (EG). Ethanol also influences the metabolic pathway
of serotonin (5 hydroxytryptofol) and transferrin. Features such as long biological half-life and
accumulation in tissues allow non oxidative metabolites of ethanol, serotonin and carbohydrate
deficient transferrin to serve as markers for ethanol consumption. Cocaethylene, dolichol, ketone
bodies, acetaldehyde protein adducts and salsolinol are also markers of alcohol consumption (41-
50). EG is a promising biologic state marker of recent alcohol consumption that detects alcohol
use reliably over a definite time period (51). It's also a suitable marker of excessive alcohol
consumption in serum, urine and hair (52-54), but it is recommended that urinary EG be
expressed as a ratio to creatinine in order to balance urinary dilution (55-57).

Other volatils

Some works have been published on other volatils, for example, tissue distribution of
trichloroethylene in a case of accidental acute intoxication by inhalation (58) and sensitive
analysis of alkyl alcohols as decomposition products of alkyl nitrites in human whole blood and
urine (59).

DRUGS OF ABUSE

Some new drugs of abuse have been described:

Benzylpipérazines (60-63); 4'-methyl-r-pyrrolidinopropiophenone(64), in Canada, Foxy, a

designer tryptamine hallucinogen (65) and in England, arylethylamine psychotropic recreational
drug (66).

Cannabis

Some studies about recent pratices of analysis have been published: new studies about
immunoanalysis, gas chromatography/mass spectrometry (GC/MS) analysis (67-68).
Cannabinoïds have been determined in hair using electrochemical detection (69). Cannabinoïds
in plasma or serum to whole blood concentrations distribution ratios in blood samples taken from
living and dead people are presented (70).

Studies realized on cannabis given to pigs, show that even if there is no more
tetrahydrocannabinol (THC) left in blood and that there is still inactive metabolite as THC-
COOH, THC can be present in brain (71). THC blood levels decrease in vitro, even at – 20°C,
if sample is stored on sodium fluoride, and levels increase if they are kept on lithium heparinate
(72).

Opiates

Reticuline, a marker of opium use, can differentiate use of it because it can't be detected in
heroin and poppy seeds (73). Interpretation of opiate results in the presence of pholcodine is
presented (74). In some countries, as Switzerland, heroin is given to addicts, presence of
acetylcodeine in hair can prove illicit heroin consumption (75). Effects on human performance
and behavior of opioids are published (76)

Cocaïne

It is more and more important, even in Europe, where before heroin was predominant. Different
studies have been published: on in vitro degradation of anhydroecgonine methyl ester (AEME or

263
methylecgonidine) in human plasma (77); on metabolism following different routes of
administration (78); on urinary elimination of cocaine metabolites in chronic cocaine users
during cessation (79).

The detection of the pyrolysis product, AEME, after cocaine smoking using GC-MS is hampered
by the artifactual production. Authentic AEME in serum can be differentiated from the artifact
(80).

Amphetamine

Plasma, oral fluid and sweat wipe ecstasy concentrations in controlled and real life conditions
has been studied (81).

Informations on chemical syntheses is widely available on the Internet as well as in publications

and some people, followers of Shulgin, have synthetised and consummed 2,5-diméthoxy-4-
chloroamphetamine (DOC), 2,4,5-trimethoxyamphétamine (TMA-2); 5-diméthoxy-4-
ethylthiophenylethylamine (2-CT-2) and 2,5-diméthoxy-4-(n)-propyl-thiophenylmethylamine (2-
CT-7). Metabolism and toxicological detection of 2C-T-2 by GC-MS is presented (82).
Metabolism, including cytochrome P 450 isoenzyme dependency and mass spectral screening
procedures of amphetamine-derived designer drugs have been studied (83). A review of the
public domain literature regarding 2C-B ( 4-Bromo-2,5-dimethoxyphenethylamine) is published
(84). Few deaths have been reported with para-methoxyamphetamine (85-87) and 2 CT-7 (88).
Effects on human performance and behavior of MDMA are published (89)

Lysergic acid diethylamide (LSD)

New studies have been published:

- Performed LSD detection with ion trap GC-MS: trimethylsilylation of LSD decreases the
detection threshold by a factor 10, although, chemical ionization provides a seven times
more sensitive method than electron ionization (90);
- Short-term stability of LSD, N-Desmethyl-LSD, and 2-Oxo-3-hydroxy-LSD in urine
(91);
- Comparison of EMIT II, CEDIA, and DPC RIA assays for the detection of LSD in
forensic urine samples (92).
- LSD has been determined in phaneres (93).

Phencyclidine

Effects on human performance and behavior of phencyclidine are published (94).

Gamma-hydroxybutyric acid (GHB)

Some techniques for research and identification are presented. About interpretation, difficulties
come from the fact than GHB can be endogenous, and can increase after death. Endogenous
GHB levels in ante-mortem urine or blood and factors affecting endogenous production are
determined (95-98) as well as in vitro production of GHB in antemortem urine samples (99). In
71 autopsies where the cause of death can exclude GHB exposure, GHB was tested positive in
all cardiac bloods with concentrations in the range 0.4 to 409 mg/L, femoral blood or vitreous
humor are the best specimens to support drug exposure (100). In the cases in which the
postmortem intervals were 24 h or less, GHB concentrations in fire victims were lower (3.80
g/L), than those in non-fire victims (7.50 g/L). The heat inactivation of the enzymes involved in

264
the formation of GHB should be responsible for these lower levels (101). Some forensic cases,
involving the use of GHB, have been described (102-103).

MISCELLANEOUS

A lot of fatal intoxications have been reported. Among them, a multiple drug fatality involving
MK-801 (dizocilpine), a mimic of phencyclidine (104); pholedrine (105); fenarimol (Rubigan), a
pyrimidine ergosterol biosynthesis inhibitor used as a systemic fungicide (106)...

Carbon monoxide

About carbon monoxide, different methods are described, for example one rapid determination
of carboxyhemoglobin in blood by Oximeter is compared with other methods (107).
Interpretation of the results is sometimes difficult, an experimental study on changes in COHb
level in blood due to changes in carbon monoxide level in the air is presented (108).

Cyanide

Cyanide in blood was determined by HPLC (109), headspace GC/MS (110) and capillary
electrophoresis with fluorescence detection (111). Chemical factors affecting the interpretation
of blood cyanide concentrations in fire victims are presented (112).

Pesticides

In case of organophosphate intoxication a method was developed for the detection of

alkylphosphates in urine (113). Organophosphorus compounds adducts of serine proteases are
analysed by liquid chromatography-tandem mass spectrometry (LC-MS-MS) (114). Human
serum paraoxonase (PON1) activity is determined in acute organophosphorous insecticide
poisoning (115)

Metals

Different studies are presented:

- a review about speciation of arsenic compounds in biological samples by high
performance liquid chromatography inductively coupled plasma mass spectrometry
system (116);
- a technique, coupling solid phase microextraction (SPME) with GC-MS, for the
determination of trimethylarsine oxide and other arsenic metabolites (117);
- post-mortem toxicological findings in sub-acute fatal aluminium poisoning in dialyzed
patients (118);
- a review on the toxicity of Thallium in humans after acute and chronic exposure, its
mechanism of action, and treatment (119);
- a fatal overdosage of an anticancer agent of Platinum, Cisplatin, (120).

SAMPLES AND SPECIFICITY

Blood, urine, gastric content are always useful for toxicological analysis, but also
unconventional samples as hair, nails, saliva, sweat and other biological matrices or even clothes
(121) or larvae (122), as either alternatives or complements to other samples.

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Hair analysis

Advanced technology such as GC/MS and LC/MS are generally used. Tandem spectrometry for
the two types of chromatography is being developed (93, 123-124). New techniques have been
found in order to improve extraction and detection. For example: off-line supercritical fluid
extraction (SFE) using large volume injection (125), HPLC using a restricted access extraction
column (126), automated column switching LC/MS (127), high pH non aqueous electrolytes and
electrochemical detection (69), GC/NCI and high volume injection (128), HS-SPE-GC/MS (129-
130), ToF-SIMS (131). In an other way, simple pre-tests for the examination of drugs in hair
become more and more sensitive too (132-134).

A great concern about hair analysis is external contamination. The risk of false positives exists
(135-136). A part of external contamination could penetrate inside the hair-shaft. Results have to
be interpreted cautiously depending on the wash procedures (137-138).

Another concern is drug melanin interactions. These have been studied (139-144). Basic drugs
have a greater affinity for melanin than their neutral analogues (145-146).

Nowadays, a single exposure can be detectable in hair. This has been demonstrated with
betamethasone (147), flunitrazepam and its metabolites (148), clonazepam and its metabolites
(149), selegiline metabolites (150) and GHB (151). The detection methods need to be very
sensitive to detect pg/mg of hair.

Particular compounds are of great interest in hair analysis, not only for the forensic science (with
the ethanol dosage, the chemical submission..) but also for the sport (with doping agents): For
ethanol, the determination of

- ethylglucuronide (EG) which is not found amongst social drinkers, (54,152);

- fatty acid ethyl esters which can be used to determine heavy alcohol consumption (45,
153-155), however, hair cosmetics and hair care may interfere (156).

For drugs facilitate sexual assault, GHB can be detected after a single exposure when hair is
collected about one month after the crime (151, 157-158). Other drugs, such as zolpidem (159),
thiopental (160), LSD, clonazepam, zopiclone, niaprazine (161), buprenorphine (162), have been
linked to cases of drug facilitated sexual assaults.

For doping agents, control in sport is more and more important. In human hair, methenolone
(163), prednisone (164), other general anabolics compounds, ephedrine and clenbuterol (165)
have been studied. Controls may exist in hair cattle or hair horse too (ethinylestradiol (166),
clenbuterol (167)).

Literature is very rich of various analyses: sildenafil (168), cathine (169), propofol (170),
amphetamines (171), arsenic (172), furosemide (173), LSD (93), search of explosives on the hair
surface (174). Suitable quality controls are recommended (175-176).

Saliva ,

Saliva is a very interesting sample to investigate research of drugs of abuse. So a lot of work
have been published (177-178). Saliva can be analysed directly on site or in a laboratory (179).
HS-SPME and direct immersion-solid phase microextraction (DI-SPME), followed by GC/MS
analyses are used for simultaneous detection of some drugs of abuse in saliva samples (180).
Detection of Flunitrazepam and 7-aminoflunitrazepam in oral fluid after controlled

266
administration of Rohypnol has been presented (181). A study about high prevalence of 6-
acetylmorphine in morphine-positive oral fluid specimens, based on controlled dose studies of
heroin administration, shows that ratios >1 of 6-acetylmorphine/morphine in oral fluid are
consistent with heroin use within the last hour before specimen collection, concentrations of 6-
acetylmorphine in oral fluid are ranged from 3 to 4095 ng/mL (182).

Sweat

Fastpatches have been used for example for crack and cocaïne (183), or for the detection of
MDMA after a single-dose administration. MDMA was detected as early as 1.5 h after
consumption and peaked at 24 h (184)

Nails

Recent work on detection of morphine, 6-acetylmorphine and cocaïne in toenails has been
published and compared with hair (185)

Vitreous humor

The use of vitreous humor (VH) to detect or confirm the presence of medical substances has
been studied (186). A study about postmortem production of GHB shows that levels increase
after death in cardiac blood but they remain low in VH (100)

Adulterants

A review and discussion about adulteration of urine samples and its effects on drugs of abuse
testing using on-site testing devices is presented (187-189). The determination of chromate
adulteration by automated colorimetric and capillary ion electrophoretic analyses, or oxidizing
adulterants by automated spectrophotometric analysers, or bromine using liquid chemistry or
rapid spot tests are presented (190-194), in particular effects of oxidizing adulterants on
detection of 11-nor-delta 9-THC-carboxylic acid in urine (195).

A combination of drug test and adulterant test device comprises a container having an adulterant
test strip and a drug test strip is proposed (196)

ANALYSIS

Simple colorimetric method

Authentication of artemether, artesunate and dihydroartemisinin, antimalarial tablets using a

simple colorimetric method (197) and rapid ferric hydroxamate screening test for GHB in human
urine are described (198).

Immunoanalyse

Immunological techniques, instrumented or non-instrumented, are generally the first step in

modern forensic toxicological analysis because the methods are simple and sensitive, take short
time and are reasonably cost-effective.

Comparisons of several commercial on-site testing devices have been reported in order to assess
their relative performance and their reliability and to determine their accuracy when used by
non-scientists versus trained laboratory analysts (199-203). The efficiency of a one-site urine

267
drug-testing device, the ONTRAK Testcup®-er, was discussed toward an instrumented
technique, the EMIT® II monoclonal immunoassay (204).

The effectiveness and usefulness of various immunoassays were evaluated:

- Kinetic Interaction of Microparticles in Solution (KIMS) assay for determination of

cannabinoid metabolites (205) and of amphetamine analogues: 3,4-
methylenedioxyamphetamine (MDA),
3,4-methylenedioxymethamphetamine (MDMA),
3,4-methylenedioxyethylamphetamine (MDEA) (206).

- Cloned Enzyme Donor Immunoassay (CEDIA) to screen broader for amphetamine and
its derivatives with Multiplex CEDIA Amphetamine/Ecstasy assay (207) and to screen
specifically for 6-monoacetylmorphine with CEDIA 6-MAM (208-209).
- Enzyme Linked ImmunoSorbent Assay (ELISA), a new validated test for buprenorphine
determination (210) and the description of a new test for determination of
methylphenidate in urine (211). Semi quantitative analysis of opiates in oral fluid can be
done on microplate EIA (212).

Some of these immunoassays have been applied for the screening of whole and/or post-mortem
blood samples (213-215); a modified EMIT method was proposed in post-mortem blood (216).

The suitability of different immunological techniques have been compared in order to choose the
more appropriate one to detect LSD (92,217), flunitrazepam (218-219), 4-methylaminorex (220),
piperazine-like compounds (63), amphetamine analogues (221), and clonazepam and 7-amino-
clonazepam (222).

Cross reactivity have been studied on ELISA Kit for the determination of amanitins (223).
Interferences of 13 quinolones with 5 immunoassays for opiates (224) and of apomorphine and
its derivatives with CEDIA and FPIA (225) were determined. The possibility of false-positive
results were recognised especially with amphetamine assays (226-230). The ability of EMIT to
successfully discriminate methylamphetamine enantiomers has been reported (231).

Various immunological techniques were used to analyse unconventional matrices such as

vitreous humour (232), bone and bone marrow (233-234), oral fluid, sweat (235-236), brain
tissues and pituitary gland (237).

Some processes by which immunoassay tests are made (test card, preparation of antigens or
antibodies,...) have been developed (238-240).

The construction of mathematic model from calibration data of the TdxFLx is used for a better
understanding of the abused drug-protein binding phenomena and to try to explain why this
methodology is only semi-quantitative (241).
A preliminary work was made in order to find out the potentiality of a genetically modified
bacterial biosensor and its applications in forensic toxicology analysis (242).

Todays immunological techniques, instrumented or not, are efficient and very popular, but
nevertheless all positive immunoassay results must be confirmed by another specific procedure.

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Extractions

Prior to analysis, sample preparation techniques are often required. Acid hydrolysis is necessary
for xenobiotics in urine and improved when the sample is heated by microwave (243-244).

Extraction is one of the most important step to clean up the matrix, to concentrate the analytes
and finally to bring out the best conditions for instrumental analysis.

Liquide/liquide extraction is still used today for post-mortem material (245).

Solid phase extraction (SPE) is becoming a commonly used extraction technique. The SPE
mechanism is based on interactions between sample compounds and the column sorbents. Polar
and apolar silica sorbents are used for one or a group of drugs in a relatively clean biological
matrix as plasma, serum, or urine (246). Mixed mode bonded silica sorbents have been created to
extract acidic, basic and neutral compounds on the same column in two fractions by a proper
ajustement of pH and choice of solvent. These methods have been optimized for screening whole
blood or forensic samples (247-253).

Now, the polymer-based sorbents are developed to overcome the limitation of silica sorbents in
combination or not with a cation exchange sorbents. Whole blood and tissues can be extracted
successfully for a screening (254-263). Some techniques have been tested with these columns to
extract one or a group of substances (264-267). SPE can be improved by membranes with
chemically bonded chromatographic particles emmershed in polytetrafluoroethylen (PTFE)
microfibrils (268). The SPE extraction procedures can be automated (269).

Solid phase micro extraction (SPME) is under investigation for its usefulness in the
determination of some analytes such as local anesthetics (270), amphetamines (271) and
cannabinoids (129).

In tube solid phase micro extraction (in tube SPME) is a new sample preparation technique.
Organic compounds in aqueous samples, blood or urine, are directly extracted and concentrated
into stationary phase (polymer fibrous) of a capillary column (272-273). This procedure can be
used in combination with GC-MS (274-275), microcolumn liquid chromatography (276), HS-
GC-MS (30,277), high performance liquid chromatography (HPLC) and capillary
electrophoresis (278). In tube SPME can be automated (279). To increase the detectability, it is
possible to practise a direct derivatization on fiber (280-281).

Liquid phase micro extraction (LPME) is a new concept for drug preparation. A small piece of a
porous hollow fiber, containing an organic solvent, is immersed in a simple vial. This allows
coupling LPME with gas chromatography, high performance liquid chromatography (282). This
procedure can be applied to the detection of drugs of abuse (283).

Headspace solid-phase dynamic extraction (HS-SPDE) has been described for cannabinoïds in
hair (284).

Supercritical fluid extraction (SFE) and chromatography procedures are usually developed to
analyse the lipids on hair which are different according to gender, age and race (125, 285). This
technique is also performed to isolate drugs from hair (286).

269
Analytical techniques

Apart from the first-line automated immunoassays available for the most common drugs, the
general unknown screening (GUS) procedures currently used in clinical and forensic toxicology
involve chromatographic techniques, ideally coupled to specific detectors (GC-MS or HPLC
coupled to UV-diode-array detection, (DAD)). Nevertheless, none of these is sufficient on its
own to identify all possible toxic compounds. For instance, some polar compounds with no or
little UV absorbency will not be detected neither by GC-MS nor HPLC-DAD. With MS being
more specific and reliable than DAD and GC being limited to volatile and thermally stable
compounds, the coupling of MS to HPLC seems to be a possible way of increasing the range of
compounds amenable to MS The development of benchtop mass selective detectors in liquid
chromatography/mass spectrometry (LC/MS) made these techniques very useful for
toxicologists(287-288).

Concerning GC, recent developments are:

- techniques for saving time, as fast-GC (289)

- for GC/MS, advances in the use of mass spectral libraries for forensic toxicology (290),
pesticides and drugs (291) or, in the web: library of the American Academy of Forensic
Sciences:
- http://www.ualberta.ca/~gjones/mslib.htm; the collections of more than 200 mass spectra
home-made reference electron impact mass spectra of derivatives produced by TIAFT
members for TIAFT members: (http://www.tiaft.org/main/mslib.html)

For liquid chromatography, the main development comes from improvements of LC-MS.
Applications to forensic or clinical toxicology have greatly increased due to technical
improvements and to the advent of atmospheric pressure ionization (API). Most of these
applications use electrospray ionization (ESI) and atmospheric pressure chemical ionization
(APCI) because of their simplicity, quickness and compatibility with biological samples and
mobile phases containing buffers. Moreover, ESI and APCI, which can be achieved on the same
instrument, allow the detection of polar and non polar compounds.

The use of different types of analysers (quadrupole, ion-trap, time of flight) and tandem mass
spectrometry (MS-MS) increases the range of drug detection (292). In comparison with single
quadrupole, MS-MS offers superior sensitivity and selectivity (293). These instruments enable
the quantification of low levels of compounds in biological matrices often with much reduced
sample preparation and analysis time (294). Libraries are developed (295-298). They allow to
detect a lot of drugs in systematic toxicological analysis (287,292, 299-303) and for peptides,
proteins, alkaloids, drugs of abuse (304-306), LSD (307), dimethylamphetamine (308),
methamphetamine in hair (127), methadone and metabolites (309), anabolic steroids (300,310-
311), several synthetic opioids, benzodiazepines or hypnotic agents (312-316), neuroleptics
(317-318), coumarin-based anti-coagulants, drug-facilitated sexual assaults (161), plant
intoxication (319), pesticides as organophosphate insecticide oxydemeton-Me and its metabolite
demeton-S-methylsulfon (320), quaternary nitrogen muscle relaxants (321), tetrodoxine and
aconitum alcaloïds (322)...
LC-MS and even LC-MS-MS are now applied in toxicology to compounds previously analyzed
by less specific high performance liquid chromatography (HPLC) techniques or even by gas
chromatography-mass spectrometry (GC-MS) due to the simpler sample preparation generally
needed (293). Nevertheless, LC-MS is not always convenient for very lipophilic or very
hydrophilic compounds. Moreover, the lack of inter-instrument robustness of LC-MS as a GUS
technique still limits its widespread use (287,293,323-325).

270
Ultra Performance LC™ (UPLC™) is a new category of separation science that will be the
catalyst for great advancements in analytical separation sciences. It won the first price in
innovation Pitsburg conference 2004. This new category of analytical separation science retains
the practicality and principles of HPLC while increasing the overall interlaced attributes of
speed, sensitivity, and resolution (326).

Capillary electrophoresis (CE)

A recent book and articles report clinical and forensic applications of CE and development in
CE, CE-MS and MS-MS (327-330) Particularly the determination of LSD in blood by capillary
electrophoresis/fluorescence spectroscopy with sweeping techniques in micellar electrokinetic
chromatography (331), determination of GHB in human urine by capillary electrophoresis with
indirect UV detection and confirmation with electrospray ionization ion-trap mass
spectrometry(332-333), detection of mushroom peptide toxins in body fluids by capillary
electrophoresis (334), analysis of antibiotics (335), rapid analysis of 3,4-MDMA by comparison
between non-aqueous capillary electrophoresis/fluorescence detection and GC/MS (336).

The techniques of Raman and nuclear magnetic resonance (NMR) spectroscopy are in progress
for the analysis of xenobiotics (337-338), herbicides (339), GHB (340), ecstasy derivatives (341)
or rodenticides (342).

Some multi-elementary method using inductively coupled plasma mass spectrometry (ICP-MS)
are developed to allow determination of numerous metals in biological fluids (343-344).

The choice of instruments depends on the work to do and on the financial means, a practical tool
for making decisions when purchasing analytical instruments and reagents is given in The
Journal of Analytical Toxicology (www.jatox.com) by the link to the Journal of
Chromatographic Science’s International Chromatography Guide.

INTERPRETATION

Sometimes after a long and difficult analytical work, interpretation can be delicate or critical. We
must take care of several points.

Post-mortem drug levels in biological matrices may fluctuate according to the sampling site and
the interval time between death and sampling. The knowledge of these variations, called post-
mortem redistribution, is crucial as it influences the result’s interpretation in forensic toxicology.

The underlying mechanisms are complex and of different types. Cell autolysis, putrefaction
process, pharmacokinetic characteristics of the drugs and passive drugs released from organs
called «reservoirs» (myocardium, lungs) are involved in the redistribution phenomenon (345).
Two diffusion mecanisms are implied: cellular and/or vascular pathway. For example MDMA
cellular diffusion is more important than vascular pathway in rabbits models after intravenous
administration and this drug is metabolized to MDA after death (346-347).

Some physico-chemical properties such as lipophily (Kp) are investigated. A rabbits model and
three betablockers with different Kp and similar pKa were used in a study in order to determine
the influence of the lipophilicity on the drugs post-mortem redistribution (348).

Because of the concentration variation in post-mortem matrix, some data as the drug’s post-
mortem stability and potential redistribution must be incorporated into result’s interpretation
(349). Unfortunately, published data are often reported without mention of sampling sites, post-
mortem delay, or autopsy conditions. Results of drug’s distribution are variable (350). Further

271
investigations in this field should include establishment of reference concentration ranges of both
parent drugs and metabolites also in tissues other than blood; for example distribution of
nitrazepam and 7–aminonitrazepam in a case of nitrazepam intoxication (351).

Different studies have been conducted: distribution of butalbital in post-mortem tissues and
fluids suggests that tissue could be used to estimate drug levels in blood (352); carbamazepine’s
redistribution on 16 cases (353); post-mortem blood ketamine distribution in two fatalities
showed the importance of considering both heart and peripheral blood samples in the
investigation (354), post-mortem redistribution of xylazine (355), or oxycondin (356);
elimination of 7-aminoclonazepam in urine after a single dose of clonazepam in urine collected
from 10 healthy volunteers who received a single 3-mg dose of clonazepam. The urine from
every subject was still positive for 7-aminoclonazepam 14 days after administration of the drug.
One volunteer was still positive 28 days after administration. Clonazepam was not detected in
any of the samples (357).

The condition of conservation of the body, drug characteristics, matrix, and site analyse are
factors which need to be considered in the proper interpretation of an autopsy specimen results
(349).

Quality of the conservation is very important, the influence of temperature and time of storage
on the stability of some medications has been studied:
- fluoxetine in biological material showed consistent stability in samples which were stored
at -20°C, it was stable in biological material stored at +4°C and +25°C for a period of
only one month(358);
- 37 antidepressants and neuroleptics in whole blood shows that olanzapine, fluvoxamine,
levopromazine, haloperidol, alimemazine, chlorpromazine, mianserine ... are unstable in
blood even at –20°C and 21others (cyamemazine, tiapride, fluoxetine, amisulpride,
sertraline, citalopram, paroxetine, venlafaxine, loxapine...) are stable (359-360);
- suxamethonium and its major hydrolysis product (361).

Pharmacogenomic
Defects in the genes encoding drug metabolising enzymes (DMEs) may lead to adverse drug
effects, even to death. To help interpretation of the forensic toxicological results studies are done
for example on the genetic variation of the cytochrome CYP2D6 gene and its implication in
tramadol metabolite ratios found in post-mortem samples (362); to interprete methadone toxicity
of poor and intermediate metabolizers (363); on the relationship between genetic polymorphism
of CYP2C19 and metabolism of omeprazole in order to assess the severity and to predict the
outcome of poisoning for forensic and clinical toxicology (364); on the influence of cytochrome
P450 2D6 on the metabolism of TFMPP (1-(3-trifluoro-methyl-phenyl)piperazine) and studies
using in vitro and in vivo techniques (365)

Data on blood levels

In order to assess the significance of drug levels measured in clinical and forensic toxicology as
well as for Therapeutic Drug Monitoring (TDM) it is essential that good collections of data are
readily available. For more than 800 substances, therapeutic ("normal") and, if data is available,
toxic, and fatal plasma concentrations as well as elimination half-lives were compiled in a table
(366-367).

Two compilations can also be consulted on the Internet, one has been prepared by R.J. Flanagan
of London UK(www.leeds.ac.uk/acb/annals) and contains data on about 700 compounds of
toxicological interest, the second site is one prepared by Donald Uges (Groningen, The
Netherlands), this compilation of data on over 500 compounds can be viewed at the TIAFT web-

272
site (www.tiaft.org). However difficulties remain when several toxics are present, an example is
given with coexistence of ethanol and diazepam in 234 cases of forensic autopsy (368)

IMPORTANT ITEMS IN FORENSIC TOXICOLOGY

Alcohol, drugs and driving

More and more, governments are struggling against road insecurity and engage national
mobilization. Specific meeting are organised on this subject. For example, the 16th International
Conference on Alcohol, Drugs and Traffic Safety (ICADTS 2002) organised in Montreal,
Canada. Session topics were covered: driver characteristics, pharmacology and toxicology,
epidemiology, rehabilitation, prevention, driving performance and new issues (369). Prevalence
of alcohol, cannabinoids, opiates, cocaine metabolites, amphetamines and therapeutic
psychoactive drugs in blood samples from drivers injured in road accidents in France has been
evaluated(370).

Strategy differs according to the country. Some countries have drug recognition experts.
Evaluations using limited data are presented (371).

A forensic science review's publications (2003; 15(1)) on alcohol, drug and human performance
and behavior has been published, and effects on human performance and assessment of driving
impairment are discussed for marijuana (372); benzodiazepines (373-374), MDMA (375).

A new technology is being marketed to rapidly test oral fluids for drugs of abuse at the roadside
or in a police station. Most devices performed well for the detection of amphetamines and
opiates, but all performed poorly for the detection of cannabinoïds (376-377). Some analytical
strategies are presented (378-379).

A recent review about drugs of abuse monitoring in blood for control of driving under the
influence of drugs is presented. Basic data about the biosample assayed, internal standard,
workup, GC or LC column and mobile phase, detection mode, references data, and validation
data of each procedure are summarized (380).

The question of threshold values for absolute driving inability is discussed (381).

The project Rosita-2, funded by the European Commission, NHTSA (National Highway Traffic
Safety Administration), NIDA (National Institute on Drug Abuse) and ONDCP, (Office of
National Drug Control Policy) is a 3-year project for the evaluation of roadside oral fluid drug
tests, carried out in six countries in Europe and five states in the USA. Scientists not directly
involved in the work of Rosita-2, have the possibility of register for the Rosita-2 meetings. Their
final results are expected at the end of 2005.

On the rosita.org website, several documents, the results of the first (1999-2000) Rosite project,
are available. They cover drugs and medicines suspected to have a detrimental impact on road
user performances; inventory of state-of-the-art road side testing equipment; operational, user
and legal requirements across EU member states for roadside drug testing equipment; evaluation
of different roadside drug tests.

Drug-facilitated sexual assaults

This phenomenon is more and more studied. The list of drugs reportedly associated with sexual
assault is long and includes among others flunitrazepam with other benzodiazepines such as

273
diazepam, temazepam, clonazepam, oxazepam as well as gamma-hydroxybutyrate acid (GHB),
ketamine, and scopolamine. Medicolegal approach is presented (382) and analytical
developments in toxicological investigation too (383).

Test devices are provided to detect drugs in drinks, in particular drugs which are used in rape.
Benzodiazepines including Rohypnol® and GHB or ecstasy can be detected (384-385).
Screening method by micellar electrokinetic chromatography for common sexual assault drugs
administred in beverages is presented (386)

A method for detection of 4-hydroxybutyric acid and its precursor(s) in fluids is described (387).
Ultra-rapid procedure to test it in blood and urine by gas chromatography-mass spectrometry is
presented (388). A single exposure to GHB or benzodiazepine in a case of sexual assault can be
documented by hair collection one month after the crime (151,161).

Doping

New and emerging technologies including gene transfer therapy, stem cell transplantation and
bio-regenerative medicine, growth factors, muscle fiber phenotype transformation, red blood cell
substitutes including modified hemoglobines and perfluorochemicals, and new drug delivery
systems are published (389)

The development of techniques and detectors allow to detect very small traces, and make easier
the research of some types of products(310,311). Few developments and studies have been
published:
- urinary testosterone can increase as a result of microbial action, however, the increases
observed were small, and hence, the changes in the Testosterone/Epitestosterone ratio
were minor (390);
- evaluation of human hepatocyte incubation as a new tool for metabolism study of
androstenedione and norandrostenedione in a doping control perspective (391)
- Oxygen carriers or blood substitutes might represent the next step of fraudulent
improvement of the physical performance (392).

Legal Medicine

Forensic medicine is progressing towards the use of high-tech methods, particularly 3D

photogrammetry with the possibility to document the internal body morphologicaly using
modern computed tomography (CT) and magnetic resonance techniques (393-394).

For sudden unexpected death in infancy, postmortem screening for fatty acid oxidation disorders
by analysis of Guthrie cards with tandem mass spectrometry is presented (395). For autopsy
investigations, a reliable coagulation test, the PIVKA (Proteins Induced by Vitamine K Absence)
II test can be used during the post-mortem period (396). Less than 48 h after death, the C-
reactive post-mortem protein (CRP) can differentiate acute of non acute death (397). A book “
Time since death” has been published (398).

Quality

More and more quality assurance takes place in laboratories. Approach in USA (399) and special
approach for alcohol (400), and hair (175-176, 401) are presented. Forensic analysts need to be
trained (402). Several articles deal with strategy guidelines and recommendations for forensic
toxicology practice as those used in Japan (319)

274
INFORMATION SOURCES

Scientific Literature

Some important books for toxicologists are presented:

- The clarke’s: Isolation and identification of drugs (403);
- The 4th volume of Mass spectral and GC data of drugs, poisons, pesticides, pollutants and
their metabolites (404);
- Criminal Poisoning: an investigational guide for law enforcement, toxicologists, forensic
scientists, and attorneys (405);
- Handbook of analytical separations vol 2 : Forensic Sciences (406).
- “Molecules of death” present aflatoxin, botulinus toxin, domoic acid, ecstasy, heroin
hydrogen sulphide, mercury, nerve gases, nicotine and the tobacco alkaloids, phosphorus,
radon, ricin, snake toxins, spider toxins, strychnine, tetrodotoxin, thallium (119).

Some papers summarized a lot of data: an overview of current resources in the field of
toxicology (407); a concise survey of Forensic sciences's articles appearing in publications (68)
or a recent presentation of toxicological expertise (408). A Lot of book of forensic or
pharmacologic interest are reported on medlina .com

Web sources

The internet provides abundant web-sites and resources for practicing forensic toxicologists and
people interested in this field.

All the relevant journals related to the field of analytical and forensic toxicology are present on
the web and provide on-line access to the tables of contents of their current and past issues. For
example: the Journal of Analytical Toxicology (JAT,www.jatox.com), with a link to PubMed;
Forensic Science International (www.elsevier.nl/locate/issn/03790738) offers free access to
tables of contents, authors, and keywords indexes. Abstracts and full text of articles are available
to subscribers through ScienceDirect (www.sciencedirect.com); Journal of Forensic Sciences
(www.aafs.org); International Journal of Legal Medicine
(link.springer.de/link/service/journals/00414/index.htm); Journal of Clinical Forensic Medicine
(www.harcourt-international.com/ journals/jcfm); Journal of the Canadian Society of Forensic
Science (www.csfs.ca/journal/journal.htm); Annales de Toxicologie Analytique
(www.sfta.org/ATA/ATAintro.html). The catalogue of the available issues of The Journal of
Psychoactive Drugs can be viewed at (www.hafci.org/journal), although, with no on-line access
to the table of contents.
Two on-line peer-reviewed scientific journals currently exist on the Internet, the International
Journal of Drug Testing (www.criminology.fsu.edu/journal) and Forensic Science
Communications (www.fbi.gov/search.htm)

Certain organization as The Centre for Substance Abuse Prevention (CSAP) maintains a
workplace resource centre (www.drugfreeworkplace.gov) which includes access to information
regarding the drug-free federal and commercial workplace programs, substance abuse, drug
testing, and workplace drug prevention research, or rosita (www.rosita.org) for roadside
problems, or the National Institute for drug abuse (www.nida.nih.gov) ;

A review includes a description of web-sites, databases of toxicological and analytical data, and
web-based journals, forums and mailing lists (409).

275
Forensic Toxicology Societies

A lot of countries have forensic toxicology societies and some organisations are international, as
The International Association of Forensic Toxicology (TIAFT), The International Council on
Alcohol, Drugs and Traffic Safety (ICADTS). They usually organise meeting, and use a forum
for discussion and exchange of ideas on the web.

Organizations such as The International Association for Chemical Testing (IACT), Society of
Forensic Toxicologists (SOFT), American Academy of Forensic Science (AAFS), California
Association of Toxicologists (CAT), the American Board of Forensic Toxicologists (ABFT),
Forensic toxicologists, Canadian Society of forensic science (CSFS) La Societe Francaise de
Toxicologie Analytique (SFTA)... have also web sites, forum and mailing lists so that, forensic
toxicologists could exchange ideas, opinions, and news.

Remarque

We do our best to collect a maximun of development in toxicology until beginning of 2004. It's
possible than we forget some, if we forgot our work, please accept our apologies.

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003 Schoknecht G. Comparison of quality of both breath and blood alcohol analysis with
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104 Mozayani A, Schrode P, Carter J, Danielson TJ. A multiple drug fatality involving
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105 Romhild W, Krause D, Bartels H, Ghanem A, Schoning R, Wittig H. LC-MS/MS
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106 Proenca P, Marques EP, Teixeira H, Castanheira F, Barroso M, Avila S, Vieira DN.
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116 Kaise T. Speciation of arsenic compounds in biological samples by high performance
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125 Goodpaster JV, Bishop JJ, Brenner BA. Forensic analysis of hair surface components
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315 Miki A, Tatsuno M, Katagi M, Nishikawa M, Tsuchihashi H. Simultaneous
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349 Leikin JB, Watson WA. Post-mortem toxicology: what the dead can and
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350 Henry JL, Epley J, Rohrig TP. The analysis and distribution of mescaline in
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351 Moriya F, Hashimoto Y. Tissue distribution of nitrazepam and 7-aminonitrazepam in a
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352 Lewis RJ, Johnson RD, Southern TL, Canfield DV. Distribution of butalbital in
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353 Klys M, Bystrowska B, Bujak-Gizycka B. Post-mortem Toxicology of
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354 Lalonde BR, Wallage HR. Post-mortem blood ketamine distribution in two fatalities.
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355 Moore-KA, Ripple MG, Sakinedzad S, Levine B, Fowler DR. Tissue distribution of
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356 Anderson DT, Fritz KL, Muto JJ. Oxycontin: The concept of a «ghost pill» and the
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357 Negrusz A, Bowen AM, Moore CM, Dowd SM, Strong MJ, Janicak PG. Elimination
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362 Levo A, Koski A, Ojanpera I, Vuori E, Sajantila A. Post-mortem SNP analysis of
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363 Wong SH, Wagner MA, Jentzen JM, Schur C, Bjerke J, Gock SB, Chang CC.
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366 Schulz M, Schmoldt A. Therapeutic and toxic blood concentrations of more than 800
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392 Audran M. Oxygen carriers or blood substitutes. Lettre du Pharmacologue 2002,
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ABBREVIATIONS

AEME anhydroecgonine methylester (cocaine metabolite)

APCI-LC-MS Atmospheric pressure chemical ionization. - Liquide chromatography - Mass spectrometry :
BZE. Benzoylecgonine
BZPou BP Benzyl Pipérazine
CE Capillary electrophoresis
CEDIA Cloned Enzyme Donor Immunoassay
CI Chemical ionisation
COC Cocaïne
DAD Diode Array Detector
DI-SPME direct immersion-solid phase microextraction.
DOB 2,5-diméthoxy-4-bromoamphétamine
DOET 2,5-Diméthoxy-4- éthylamphétamine
DOM 2,5-diméthoxy-4-méthylamphétamine
DPC Diagnostic Product Corporation
ECD Electron capture detector
ECG Ecgonine
EG ethyl glucuronide
EI Electron impact
ELISA Enzyme Linked ImmunoSorbent Assay
EME Ecgonine Méthyl Ester
EMIT Enzyme Multiplied Immunoassay Technique
ES Electron Spray
FID Flame ionisation detector
FPIA Fluorescence polarisation immunoassay

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GHB gamma-hydroxybutyrate acid
GC-MS Gas chromatography / mass spectrometry
GC-FID Gas chromatography-Flame ionisation detector
GUS General unknown screening
HFBA Heptafluorobutyrique anhydrid
HPLC High performance liquid Chromatography
HS Head-Space
HS-SPME Head space-solid phase microextraction
ICP-MS inductively coupled plasma mass spectrometry
IE impact electronique
IR Infrared
KIMS Kinetic Interaction of Microparticles in Solution
LC Liquid Chromatography
LC-MS Liquid Chromatography-mass spectrometry
LPME Liquid phase micro extraction
LSD Lysergide acide diethylamine
MDA Méthylènedioxyamphétamine
MDEA Méthylènedioxyéthamphétamine
MDMA Méthylènedioxyméthamphétamine
MAM Mono acetyl morphine
MSTFA Méthylsilyl trifluoroacétamide
MTBSTFA N-méthyl-N-tert-butyldiméthylsilyl trifluoroacétamide
NICI Negative ion chemical ionisation
NIDA National Institute for Drug of Abuse
NPD Nitrogen-Phosphorus detector
PFPOH Pentafluoropropanol
PICI Positive ion chemical ionisation
QED Quantitative ethanol detector
RIA Radio immunoassay
SID surface ionisation détector
SIM Selected ion monitoring
SIMS surface ionisation spectrométrie de masse
SM Mass Spectrometry
SFE supercritical fluid extraction
SPDE Solid phase dynamic extraction
SPE Solid phase extraction
SPEC MP1 Solide phase Extraction Concentrators, Mixed Phase
SPME Solid phase microextraction
THC Tetrahydrocannabinol
THC-COOH tétrahydrocannabinol carboxylic acid (metabolite)
TOF Time of Flight
U.V Ultra-violet
VH Vitous Humor

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Fire Cause and Fire Debris Analysis

— A Review: 2001 to 2004 —

Dr. P. Mark L. Sandercock

Forensic Scientist, Royal Canadian Mounted Police
Forensic Laboratory Service - Edmonton
15707 - 118th Avenue
Edmonton, Alberta, Canada T5V 1B7

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CONTENTS

Introduction

Scene examination and general fire investigation

General
Combustion studies and modeling
Electrical fires
Non-electrical fires
Vehicle fires
Spontaneous combustion
Accelerant detection canines
Sample collection and packaging
Training and research
Internet resources

Laboratory analysis of fire debris samples

General
Sampling and sample preparation techniques
Chromatographic analysis (GC-MS, GC-MS-MS, isotope ratios, GC x GC)
Data interpretation (includes chemical fingerprinting)
Other analytical methods
Analysis of liquids, new products and other materials

Miscellaneous studies

Accelerant transfer and persistence

Contamination and background interference

Conclusions

References

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INTRODUCTION

This review paper covers advances in scientific methods applied to fire cause and fire debris
analysis, as well as emerging scientific methods that have application in these fields, since the
13th Interpol Forensic Science Symposium in October 2001. A literature review of the forensic
science, fire investigation, and scientific journals was conducted for the period commencing in
October 2001 to the present. The primary sources used to conduct the literature review were
Current Contents (Thomson – Institute for Scientific Information ) and Scirus (Elsevier Science)
and was supplemented by searches of UMI Proquest for dissertations and the Internet. Major
forensic laboratories around the world were also asked to provide information. This final report
brings together the information received from all sources used.

SCENE EXAMINATION AND GENERAL FIRE INVESTIGATION

General

There have been a few articles published that examine the incidence of fire and explosions in
industry and the workplace, as well as an analysis of dwelling fires in London, United Kingdom
(UK). A review examining incidents of fires, explosions, runaway chemical reactions and
unignited releases of flammable materials at work sites in the UK between April 1, 1998 and
March 31, 2000 has been published. [A1] This review examined 2220 incidents of workplace
fire and explosions that resulted in 729 injuries and 19 deaths. A total of 3819 fires in the work
place that occurred between 1996 and 1999 have been reported. [A2] This review includes
analysis of residential workplace fires (e.g. hotels, boarding houses and hospitals), as well as
office and commercial fires and identifies which type of workplace is more likely to suffer from
a deliberate or accidental fire. Common risk factors were identified in an analysis of 259 fatal,
unintentional dwelling fires that occurred between 1996 and 2000 in London, UK. [A3]
Although not the focus of the report, the authors noted that of the 358 dwelling fire deaths in
London during this period, 61 (17%) were the result of a deliberately set fire.

A survey of 243 fires and explosions at German companies involved in the woodworking
industry has been reported. [A4] A study of 194 unintentional injuries sustained by people in the
United States involved in the burning of garbage or brush identified the use of an accelerant (e.g.
gasoline) in over 80% of the injuries. [A5] A review of 69 suicides by fire in South Africa has
been reported. [A6] An accelerant (typically kerosene) was used by the victims in the majority
of these deaths (53 or 77%). A summary of the fire loss in the United States of America (USA)
in 2001 documented 521,500 structure fires, approximately 45,000 of which were incendiary in
nature. [A7] Intentionally set structure fires in the USA resulted in 330 civilian deaths and $1
billion in property losses (not including the deaths and property damage from the World Trade
Centre attack on September 11, 2001). Only 39,500 intentionally set vehicle fires causing $219
million in property damage were reported in the USA in 2001, a decrease of 15.1% from the
previous year.

General fire investigation is the topic of a number of articles. In a three part series, DeHaan
explored the changes that have occurred in the past 30 years in the composition of furniture and
floor coverings, the creation of many new petroleum solvents and other related products, as well
as the improvements in analytical instrumentation, methods and sensitivity. [A8,A9,A10]
Sanderson provides practical advice for the excavation of debris at a fire scene and the
information that can be gained from this process. [A11]. Rochon describes fire investigation in
the context of a criminal investigation in Canada. [A12] Olge has written about the need for
scientific fire investigations [A13], while Charney and Goldstein discuss the applicability of
digital images in the reconstruction of a fire event. [A14] Certuse explains the causes of

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residential steam boiler failures and how these lead to fires. [A15] Full text articles from the Fire
and Materials eighth international conference (January 2003, in San Francisco, USA) have been
compiled, along with papers from earlier conferences, and published electronically on compact
disk. [A16]. Specific articles from this compilation are cited throughout this review.

Several books related to fire scene investigation have been published during this review period.
A new, 1116 page resource for fire investigators, the Ignition Handbook, contains a discussion
on combustion theory as well as information on specific materials and devices from “accelerants
in incendiary fires” to “wool.” [A17] A new textbook, Forensic Fire Scene Reconstruction,
looks at the application of forensic engineering techniques to fire scene reconstruction. [A18]
Another new book, Fire Investigation, is aimed at providing the fire scene investigator with the
knowledge necessary to correctly determine whether a fire was accidental or malicious was also
published. [A19]

Kocsis and Cooksey have conducted an extensive study into psychological profiling of serial
arsonists. [A20] From their research these authors have developed an empirical model of serial
arsonist behaviours and have identified four discrete behaviour patterns which may prove helpful
to the fire investigator. A serial arsonist does not necessarily suffer from pyromania and,
according to Doley, fires resulting from true pyromania be not be a frequent as once assumed.
[A21] Doley has attempted to clarify the apparent confusion about the nature and extent of
pyromania within the arsonist population, concluding that we know the most about the least
successful arsonists (the ones who got caught and are, therefore, available for mental health
studies), and that there are many misconceptions surrounding pyromania that may unnecessarily
distract investigators. Statistical data has been published describing the characteristics of
juvenile fire setters (age, gender and family unit) in the State of Oregon, USA and includes
incident characteristics such as types of structures, month of occurrence, and ignition sources.
[A22] A retrospective study of the criminal careers of convicted arsonists between 1951 and
2001 has also been examined. [A23] The authors found that while a minority of people
convicted of arson had previous convictions for violent offences, those now coming before the
courts for an arson offence are increasingly likely to have committed an arson that endangered
life or have been previously convicted of violent behaviour.

Combustion studies and modeling

The testing and reporting of the physical properties of flammable liquids is the subject of a few
articles. Itagaki explored the effect of initial pressure on the autoignition temperature of n-
decane. [B1] The author found that the autoignition temperature would decrease as the pressure
was increased and was able to describe the relationship mathematically. Britton discussed
different flammable limit test methods and made several observations with respect to
standardization of these tests. [B2] The reliability of determining the flash point of a flammable
liquid using manual or automatic testing apparatus is the subject of an article by Montemayor et
al. [B3] These authors concluded from an inter-laboratory study that flash point data collected
by either apparatus was equivalent.

The National Institute for Standards and Technology (NIST), in the United States of America
(USA) released the latest software versions of their Fire Dynamics Simulator (FDS) and
Smokeview. [B4] The Fire Dynamics Simulator is a computational fluid dynamics model of
fire-driven fluid flow which solves numerically a form of the Navier-Stokes equations
appropriate for low-speed, thermally-driven flow with an emphasis on smoke and heat transport
from fires. Smokeview is a visualization program that is used to display the results of an FDS
simulation. This software is available at no cost from the NIST web-site (www.fire.nist.gov).
The ignition of wood and the modeling of fire behaviour have been reported in a few studies. A

306
mathematical model was developed from experiments of both spontaneous and piloted ignition
of wood and could be used to predict the time to ignition of wood under different conditions.
[B5] Chen et al. also modeled the ignition time of wood when exposed to an external heat
source and found good agreement between their theoretical model and experimental data. [B6]
The modeling of fire behaviour in the upward spread of flame on a flat vertical surface has been
reported. [B7]

Modeling the backdraft phenomenon is the subject of two articles by Weng et al. The first
article [B8] used a simplified mathematical model to investigate the physical, catastrophic
mechanism of the backdraft phenomenon. The second article [B9] used a small compartment
fire to demonstrate that a critical value of unburned fuel must be reached before backdraft can
occur.

Carvel et al. have studied the effect of longitudinal ventilation systems on the development and
spread of fire within a road tunnel in which a fuel spill has occurred. [B10,B11] The size of the
pool fire and ventilation velocity were identified as key factors that will affect the development
and spread of a fire and that there is a more pronounced effect for a fire involving a heavy goods
vehicle than for a car.

Putorti reported the results of full-scale spill and fire experiments conducted with varying
quantities of gasoline and kerosene on vinyl, wood parquet, and carpet covered plywood floors
in order to predict the quantity of liquid fuel required to create burn patterns of a specific size.
[B12] Six room burns were conducted in a full scale, six storey wood frame building at
Cardington, England. [B13] Test burns were conducted both with and without the use of a
flammable liquid accelerant and a brief description of each test condition and the results is
provided. A study of fire-induced failure of polycarbonate windows in passenger railcars was
presented by Strege et al. [B14] They showed that larger windows can fail up to twice as fast as
smaller window allowing more air to support the fire. Dillon and Hamins [B15] provides an
initial look at the measured and computer-modeled characteristics of a candle flame.

Test burns conducted on pig carcasses demonstrated the ability of a localized fire to cause
extensive destruction of a body. [B16] Key elements identified in the study were the presence of
adequate body fat together with a blanket wrapped around the carcass and the presence of carpet
to act as a wick that would act together to establish a steady-state fire after initial acceleration of
the fire by gasoline. This study was supported by the findings of Christensen who examined the
effect of cloth to act as a wick in the combustion of tissue from a human leg and the
susceptibility of bones of differing densities to incineration. [B17]

Determining fire origin from measurements of depth of calcinations of fire-exposed gypsum wall
board was presented by Kennedy et al. [B18] Full scale room fires were used to test a system for
measuring depth of calcinations by volunteer investigators.

Electrical fires

A description of how electrical wiring faults can lead to over-heating and result in a structure fire
has been described. [C1,C2] In another article, Babrauskas describes a hazardous electrical
connector used to join electrical wires together in a light fixture. [C3] Goodson et al. have
reported the inhibition of heat transfer from household electrical wiring when it is surrounded by
polyurethane “spray-in” foam insulation. [C4] They warn that the lack of heat transfer from a
loaded circuit may raise the temperature of the wire to the point where ignition may occur.
Significant heating at the plug (up to 200 oC) was reported in a study of a loose connection
between plug and receptacle combined with an overcurrent. [C5] The authors found that the heat

307
generated degraded the polyvinyl chloride (PVC) plug insulating material which decreased the
arch tracking resistance of the plug (i.e. arcs through char), eventually resulting in fire. In
another report by the same authors, [C6] PVC and rubber-insulated electric cords were tested for
physical shorts (i.e. metal-to-metal contact) and arc tracking that occurred under radiant heat and
a variety of conditions, including twisting and pinching of the cord.

The non-destructive examination of materials from electrical fires has been described in the
literature. [C7,C8] Park et al. used X-ray diffraction (XRD), transmission electron microscopy
(TEM) and Scanning electron microscopy with energy dispersive X-ray (SEM-EDX) to
characterize the microstructure of molten marks (i.e. beads) on electric wires caused by a short-
circuit. [C9] They found that primary arc marks, caused by a short-circuit prior to the fire, could
be distinguished from secondary arc marks, those caused by a short-circuit as a result of the fire.
SEM-EDX and Raman spectroscopy was used to examine the carbon residue remaining on
molten marks caused by the short-circuit of PVC-coated wire. [C10] Using the methods
described, the authors were able to distinguish between primary and secondary molten (arc)
marks caused by short-circuit. Shefchick described two case studies in which auger electron
spectroscopy (AES) was used to examine melted copper beads from electrical-wiring to
determine if a primary or secondary short-circuit had occurred. [C11] The examination of arc
beads using secondary ion mass spectrometry (SIMS) to determine whether a primary or
secondary short-circuit occurred has also been reported. [C12] A detailed review of the methods
used to distinguish primary (“cause”) and secondary (“victim”) arc marks has been presented by
Babrauskas. [C13] Babrauskas argues that, to date, the limited data available has not
conclusively proven that primary and secondary arcing can been reliably distinguished.

Non-electrical fires

The malicious ignition of plastic domestic heating oil tanks has been reported by McAuley who
described the results of test burns that simulated the intentional ignition of these tanks. [D1] The
investigation of marine fires and explosions has been described, [D2] while Van Vaerenbergh
reported an unusual case where bricks soaked in kerosene were used in an attempt to initiate a
fire at a polyethylene recycling plant. [D3]

The reconstruction of events leading up to a liquefied petroleum gas (LPG) explosion and fire at
a petrochemical processing plant in India, the resulting damage, and dispersion modeling of the
vapour cloud that caused the incident, has been reported. [D4] A full-scale test burn to simulate
the burning of pressurized hydraulic fluid in a large industrial facility was presented. [D5] The
test burn was designed to simulate a fire at a food processing plant where 25 people died. Full-
scale test results were compared to computer model results generated by NIST FASTlite
software. Ignition tests and scale model burn tests were used to model the behaviour of a
discotheque fire in which 63 people died. [D6]

Vehicle fires

The results of motor vehicle test burns have been reported by Byers and Sutherland. [E1]
Hirschler et al. have presented a summary of the results obtained from full-scale test fires on
passenger vehicles as well as fire tests on a large number of car materials and commercial
plastics. [E2] DeHaan and Fisher reported the reconstruction of a fatal fire that occurred in a
parked motor vehicle [E3] while Chow and Li described the implications of a vehicle fire that
occurred in a cross-harbour tunnel in Hong Kong. [E4] Two cases of suspected fraud involving
fire damage to motor vehicles have been reported. [E5,E6] Adair and co-workers reported the
facts surrounding their investigation of an unusual case in which a person committed suicide by
fire while enclosed in the trunk of her vehicle. [E7] A new book, Investigation des Incendies de

308
Véhicles Automobiles, was recently published in French. [E8] This book is intended for scene
investigators to assist in the determination of vehicle fire cause (component/mechanical
malfunction or incendiary), and to identify common situations that result in vehicle fires.

Spontaneous combustion

The majority of work reported on spontaneous combustion was related to coal and several of
these articles are described here. A study of New Zealand coal suggested that the self-heating of
coal is dependent on the internal surface area which governs the available sites for oxidation,
[F1] and that sub-bituminous coals have the greatest propensity to spontaneous combustion. A
similar study reported the self-heating behaviour of sub-bituminous Australian coal in a two
meter adiabatic column. [F2] Spontanous combustion of coal dust is the subject of a study by
Amel’chugov et al. in which they demonstrated that the explosion has a two-stage character. [F3]
Spontaneous combustion experiments conducted on Turkish coals were used to predict the
progress of a fire in an underground coal mine, [F4] while modeling the spontaneous combustion
of coal in an underground mine is the subject an article by Sensogut et al. [F5]

The self-heating of other materials has also been described in the scientific literature. The
spontaneous heating of oils, [F6] as well as rubber tires and rubber mats [F7] has been reported.
Ruggeln and Rynk describe spontaneous combustion of different types of plant materials,
including Eucalyptus leaves and sawdust, in the presence of oxygen and a little water. [F8] They
also described several spontaneous fires that occurred at composting and mulching operations
and provided guidelines for the prevention of these types of fires. A study of cotton bales
demonstrated that they do not pose a fire hazard provided that the bales are compressed to a
minimum density of 360 kg/m3. [F9] A study on spontaneous heating of shale deposits that were
excavated and piled during the preparation of a sanitary landfill has been reported. [F10]
Wolters et al have presented work that demonstrates that bags of up to nine kg of charcoal
briquettes cannot self-ignite at ambient temperature. [F11]

In a two part series Jones examined the technical aspects of spontaneous combustion of laundry
in tumble dryers using “thermal ignition” theory [F12] and “hot spot” theory. [F13] In part one
[F12] the author concluded that natural or synthetic fabrics would not undergo spontaneous
ignition, while in part two [F13] Jones explored the dryer temperature required to ignite laundry
previously impregnated with oil or solvent.

The existence of “pyrophoric carbon” and its implications to a fire investigation has been
debated in the literature over a period of several years. Although some of the works were
published prior to 2001, and are technically beyond the scope of this review, they have been
included here for the benefit of the reader. A doctoral dissertation by Cuzzillo proposed that
physical changes in wood structure during “cooking” were the dominant mechanism leading to
self-heating of the wood and eventual ignition. [F14] Cuzzillo and Pagni published two reports
from this experimental data [F15,F16] to which Babrauskas wrote a commentary in support of
chemical changes, not just physical changes, in the wood structure as the cause of self-heating of
wood. [F17] A rebuttal was subsequently published [F18] to which Babrauskas replied [F19].
While Babrauskas suggested that additional experiments be conducted, [F17,F19] and Cuzzillo
et al have welcomed this idea, [F18] the debate continues with no new scientific information
being proffered at this time.

Accelerant detection canines

A small body of work has been reported regarding the training and handling of accelerant
detection canines. Williams and Johnston explored the effects of training canines sequentially

309
on different odours. [G1] They found that the canine’s ability to recognize previously learned
odours did not decrease as the number of substances trained increased, and that the amount of
time required to train a canine on a new odour decreased as more odour discriminations were
trained. Gazit et al. have described a device that allowed the researchers to study a canine’s
sniffing behaviour under a variety of situations and even to determine whether or not the canine
is actually sniffing during a search. [G2] Finally, Gazit and Terkel studied whether strenuous
physical activity, causing the canine to pant and interrupting its ability to sniff, affected the
canine’s performance in explosive detection. [G3] They found that an increase in the rate of
panting by the canine lead to a significant decrease in its ability to detect explosives. Jones et al.
presented their results on the accuracy rate of canine detection dogs at fire scenes, a study that
examined whether or not canines indicate on specific target compounds, and a program that
monitored the health of a canine over the course of a year of work. [G4] Finally, recent
theoretical work by Turin has shed new light on olfactory odour detection. [G5] Turin was able
to predict similarities and differences in odour character from ab initio vibration mode
calculations. These results are in direct contrast to the inability of molecular shape-based
theories to correctly predict odour similarities and differences and points to a new way of
understanding odour and, therefore, olfactory response.

Sample collection and packaging

Koussiafes examined whether or not using a gasoline powered, positive pressure ventilation fan
would contaminate a fire scene prior to sample collection. [H1] The findings of this study
indicated that exhaust from vehicles or power equipment operating near a fire scene would be
insufficient to contaminate samples taken from the scene. A general discussion on the legal
aspects, u nder Canadian law, of the preservation of evidence from a fire scene is presented by
Zakaib and Delovitch. [H2]

Training and research

The Bureau of Alcohol, Tobacco and Firearms’ (ATF) Fire Research Laboratory is described by
Donahue as a facility dedicated to the forensic needs of the fire-investigation community with
the capability to reconstruct fire scenes, study flashover, electrical fires and the impact of
accelerants on fire growth and spread. [I1] Madrzykowski provides an overview of the current
state of fire research and discusses the possible future direction of this research. [I2] Mannan et
al. have suggested a structured approach to evaluate the fire hazard of chemical reactions in the
process industries utilizing computational theory and experimental data. [I3]

Internet resources

A list of agencies and other organizations involved in fire investigation that are hosting web-sites
is provided. Some Uniform Record Locators (URLs) that were documented in the review for the
13th Interpol Forensic Science Symposium have been modified and the most up to date URLs are
referenced here. [J1 to J17] Additions to the list include: Canadian Association of Fire
Investigators (CAFI) [J4]; Arson Prevention Bureau (UK) [J1]; Canine Accelerant Detection
Association [J5]; Fire Protection Association Australia [J9]; National Association of Fire
Investigators (USA) [J14]. Forensic Science Journal, a new on-line journal, is published by the
Department of Forensic Science, Central Police University. [J11] Finally, the links page hosted
by Fire Science and Technology Incorporated and Fire Science Publishers web-site provides an
extensive list of fire-related associations, service organizations, journals, libraries, research
institutes and universities. [J10]

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LABORATORY ANALYSIS OF FIRE DEBRIS SAMPLES

General

The major role of the National Centre for Forensic Science (NCFS) in sponsoring the Technical
Working Group for Fire and Explosions (TWGFEX), and fostering the development of national
guides for the collection and analysis of fire and explosion debris, is presented by Minnich and
McCardle. [K1] A review of the American Society for Testing and Materials (ASTM) standards
for fire debris analysis has been published. [K2] A new book, Analysis and Interpretation of Fire
Scene Evidence, is intended to bridge the disciplines of fire investigation and forensic arson
analysis. [K3] The book begins with introductory chapters on fire dynamics and fire scene
investigation, including the use of canines, and continues with the analysis of fire debris and
interpretation of analytical results. A review describing recent advances in a variety of areas
related to fire debris analysis has also been published. [K4]

Sampling and sample preparation techniques

Snow and Slack have published a general review article in which they discuss the use of static
and dynamic headspace extraction, solid phase micro-extraction (SPME), as well as other
techniques that have generated recent interest. [L1] The authors provide application examples in
the fields of environmental, clinical, forensic, biological, food, flavor and pharmaceutical
analysis. A brief history of the development of SPME and a short literature review of SPME
applications to forensic science, including ignitable liquid extractions, has been published by
Almriall and Furton. [L2] Guidelines for the use of solid phase micro-extraction (SPME) as a
preparative technique for fire debris analysis has been published by the ASTM. [L3] Perr et al.
presented their work on the analysis of ignitable liquid residues using SPME/GC-MS-MS. [L4]
Rather than using thermal desorption, Harris and Wheeler desorbed SPME fibres with a small
volume of solvent and analyzed the solvent extracts using a conventional autosampler connected
to a gas chromatograph-mass spectrometer (GC-MS). [L5] Lloyd and Edmiston studied the
selectivity of polymethylsiloxane (PDMS) and Carboxen/PDMS SPME fibres toward different
compounds from the headspace above fire debris samples. [L6] Preferential extraction of
aliphatic and aromatic compounds was noted in this study and was found to be dependent on
temperature and fibre type. Garafano and co-workers presented a case in which they combined
the results obtained from activated charcoal extraction and SPME to identify a fuel used to
accelerate a fire. [L7] Hook et al. have described “field sampling” of workplace air
contaminants following a fire using SPME and GC-MS. [L8] The portability of the SPME
sampling technique demonstrated in this article may have broader applications to other areas
such as the sampling of volatiles at the fire scene. A comparison between air samples from
simulated fires collected using either a SPME fibre or a tube packed with Tenax and
CarbopackB has been published. [L9] The authors reported that volatile accelerants can be
trapped from the air more effectively with an adsorbent-packed sampling tube than with a SPME
fibre.

Massey and co-workers examined a number of solvents and solvent mixtures that could be used
to desorb Diffuse Flammable Liquid Extraction (DFLEX®) devices (activated charcoal strips) in
place of carbon disulfide. [L10,L11,12] Massey et al expanded their work with DFLEX®
devices to include an investigation of the best practices for using charcoal strips at the fire scene.
[L13] These authors found insertion of the strip at the laboratory instead of the scene could
result in significant loss of volatile vapours from the sample and recommended that samples be
refridgerated prior to insertion of the strip in the laboratory. Experimental work reported by
Smith and Warnke showed that optimum oven temperatures and heating times for extracting

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petroleum products from fire debris samples ranged from 60 0C for 2 hours (gasoline) to 90 0C
for 4 hours (diesel fuel). [L14]

Optimized conditions for supercritical fluid extraction (SFE) of petroleum-based fuels from fire
debris have been reported by Huang and Hsieh. [L15] Although ASTM method E1385 has been
maintained as an official standard practice, steam distillation has been all but abandoned by the
fire debris analysis community. However, Giang et al [L16] have recently described the efficacy
of micro-steam distillation and have adapted the technique to allow distillation directly from
metal cans used to collect fire debris. From a series of experiments the authors also showed that
gasoline could be recovered from concrete after heating at 1000oC in a furnace for 30 minutes,
and that accelerants could be recovered from wood and concrete substrates after the accelerant-
impregnated substrate was soaked in water.

Chromatographic analysis (GC-MS, GC-MS-MS, isotope ratios, GCxGC)

The field of gas chromatography (GC) is continually expanding. Emerging techniques such as
gas chromatography-isotope ratio mass spectrometry (GC-IRMS) and multi-dimensional gas
chromatography (two- and three-dimensional GC) are currently being explored in other scientific
fields such as geochemistry and environmental chemistry; however, their potential to be used in
the forensic examination fire debris and fire accelerant samples is clear. This section attempts to
not only review the use of chromatography as it has been applied to fire debris and fire
accelerant analysis, but also to explore the emerging techniques from other scientific fields to
indicate where this type of analysis may go in the future.

Coulombe reported the analysis of vegetable oils by gas chromatography-mass spectrometry

(GC-MS). [M1] The optimization of the sensitivity and selectivity of GC-MS and GC-MS-MS
for the identification of ignitable liquid residues has been presented. [M2] The authors proposed
methods that would improve the selectivity and sensitivity in the analysis of ignitable liquid
residues in the presence of pyrolysis products. [M3] The use of GC-MS-MS to analyze fire
debris samples for gasoline in the presence of other, potentially interfering pyrolysis products
has been described. [M4,M5] Sittidech used GC-MS-MS to increase target compound
selectivity and sensitivity and developed an “expert system” for pattern recognition of ignitable
liquids in fire debris samples. [M6]

Comprehensive, two-dimensional gas chromatography (GC x GC) is a recent development that

has received a lot of attention in the scientific literature over the past few years. [M7,M8] In GC
x GC the entire sample undergoes a two-dimensional separation with all of the components
being separated first by boiling point and second by polarity. The sample is first separated
conventionally on a non-polar column (e.g. 30 meter DB-5, 0.25 mm i.d., 1 µm film thickness);
the effluent from the first column is precisely modulated into sharp chemical pulses that then
undergo a second, fast separation on a shorter, polar column (e.g. 1 meter Carbowax, 0.1 mm
i.d., 0.1 µm film thickness). The effluent from the second column then goes to a detector. The
resulting output consists of two orthogonal retention time axes, one for each column. The key
element in GC x GC is the modulator and much work has focused on this aspect of the
technique. [M9] For example, Beens and co-workers have reported a simplied cryogenic
modulator that they used in the analysis of n-C8 to n-C18 alkanes. [M10] Adahchour et al. have
also described a simplified cryogenic modulator [M11] Another modulator, developed by
Burger et al., was used to analyze a light petroleum condensate. [M12] Other GC x GC systems
have also been described. [M13,M14,M15] Harynuk and co-workers caution that the
interpretation of two-dimensional chromatograms is a complex process that has not been
standardized. These authors have presented different ways of displaying and interpreting GC x
GC data of a gasoline. [M16]

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Blumberg has described the criteria necessary to optimize conditions for GC x GC. [M17]
Shellie and co-workers have determined the reproducibility of retention times based on an intra-
laboratory study, [M18] while the prediction of compound retention times in two-dimensional
space has been described by Western and Marriott. [M19] Reichenbach and co-workers have
reported a method for the subtraction of background levels from GC x GC chromatograms.
[M20]

One research group has demonstrated the application of GC x GC to a variety of samples, [M21]
including the separation of biomarker molecules in crude oils, [M22] petroleum contaminated
sediments, [M23] and the separation of ignitable liquids encountered in fire debris samples.
[M24] Another research group has also described petroleum separations using GC x GC. [M25]
Adahchour and co-workers have reported the extraction of flavour volatiles using headspace
SPME combined with analysis by GC x GC. [M26]

Comprehensive two-dimensional GC with time of flight mass spectrometry (TOF-MS) detection

for the separation of complex mixtures (e.g. cigarette smoke) [M27] and pesticides [M28] have
been reported. GC x GC-TOF MS has also been described by Dimandja. [M29]

Modifications to the “classical” GC x GC technique have also been described. Independent

temperature control of each column for faster, more efficient GC x GC separations was reported
by Johnson et al. [M30] Seeley et al. have described a comprehensive two-dimensional gas
chromatography technique the employs dual secondary columns (GC x 2GC). [M31] The
working temperature of GC x GC has been extended to allow semi-volatile analysis, [M32]
while a new liquid nitrogen cryogenic modulator has been described for the analysis of very
volatile compounds found in gasoline. [M33]

The use of GC-IRMS has been mainly used to characterize crude oil spills so that the source of
the spill can be determined. [M34,M35,M36,M37,M38,M39] This technique has also recently
been applied to the characterization of gasoline samples. [M40,M41] The potential use of GC-
IRMS in characterizing ignitable liquid residues in fire debris has been discussed in two articles
by Jasper et al. [M42,M43]

Data interpretation (includes chemical fingerprinting)

The identification of different ignitable liquids present in fire debris was presented by Comment
et al. [N1] as well as Moore and co-workers. [N2]

Interest in the discrimination between samples of liquid gasoline has experienced a resurgence.
Trimpe and Chasteen have briefly described an approach to gasoline comparisons. [N3] Dolan
and Ritacco were able to differentiate gasoline samples by comparing the ratios of sequential
peaks obtained from GC-MS analysis. [N4] They were able to demonstrate the utility of this
method to discriminate gasoline samples ranging from no evaporation to 50% evaporation.
Sandercock reported the discrimination of unevaporated gasoline samples by applying principal
component analysis (PCA) to the C0- to C2-naphthalene profiles obtained from GC-MS analysis.
[N5] This work was expanded and the method used to discriminate gasoline samples that were
up to 90% evaporated. [N6,N7,N8] Doble and co-workers applied PCA and artificial neural
networks (ANN) to GC-MS data to classify unevaporated regular and premium gasoline
samples. [N9] A method for the comparison of gasoline samples using the C4- and C5-
alkylbenzene profile obtained from steam distillation of samples has been presented. [N10]
Although intended to differentiate the detergent in different gasoline samples and not gasoline

313
samples per se, Carraze et al have published a method for obtaining the mass spectral
“fingerprints” of unknown detergents in gasoline from different parts of the world. [N11]

Chemical fingerprinting of hydrocarbons in order to identify a spill source has received a lot of
attention in the environmental forensics literature. [N12] Some of the concepts that have been
developed in the environmental forensic field may be helpful in the field of fire investigation.
For example, a four part series on the effects of refining on finished petroleum products has
recently been published. [N13,N14,N15,N16]

In the area of pattern recognition analysis, extensive work has been done by Lavine and co-
workers on the fingerprinting of jet fuel spills. [N17,N18] This research group has also explored
the use of SPME and pattern recognition techniques to classify jet fuels by type. [N19] Two-
dimension GC has also been used in conjunction with PCA to classify samples of jet fuel. [N20]

For the analysis of crude oil spills, different chemometric methods have been applied to mass
spectral data (without prior chromatographic separation) obtained from spilled oil samples.
[N21] Chromatographic fingerprinting has been applied in two case studies involving crude oil
spills, [N22] while the use of sesquiterpane biomarkers to distinguish between sources of heavy
fuels has been described. [N23]

Other analytical methods

A homebuilt Fourier-transform ion cyclotron resonance mass spectrometer (FT-ICR MS) was
used by Rogers and co-workers to obtain high resolution mass spectra (“fingerprints”) of a
variety of petroleum products. [O1] This research group has also presented results from their
experiments with FT-ICR MS on evaporated petroleum products, and went on to analyze fire
debris samples after Soxhlet extraction. [O2]

Although membrane introduction mass spectrometry (MIMS) has not yet been directly applied to
the field of fire analysis, it has received a lot of attention in the environmental analysis field and
is the subject of a review article. [O3] In MIMS the organic analytes are separated from air or
water by a thin membrane (e.g. polydimethylsiloxane) positioned between the sample and the
ion source of the mass spectrometer. The analytes diffuse through the membrane (drawn by the
vacuum in the ionization chamber) and are immediately volatilized once they enter the mass
spectrometer. The flow of organic compounds through the membrane tends to be greater than
that of air or water and so analyte concentration occurs. Alberici et al. have shown that MIMS
can be used to monitor the benzene, toluene, ethylbenzene and xylenes (BTEX) concentrations
in water after contact with gasoline. [O4] Multivariate analysis of their data showed that the
BTEX composition (in water) varied between the three different types of gasoline studied.

The use of vapour phase ultra-violet (UV) spectroscopy for the analysis of fire debris samples
has been described. [O5] This technique may offer additional information not obtained from
traditional gas chromatographic analysis and so is a complementary technique.

Analysis of liquids, new products and other materials

The analysis of the wax content of artificial fire place logs from different manufacturers by high
temperature gas chromatography (HT-GC) has been reported. [P1]

Woodrow analyzed samples of liquid jet fuel using gas chromatography and compared these
results to the analysis of the same samples by headspace gas chromatography. [P2] The vapour

314
pressure of each sample was determined for the two methods and was found to give similar
results.

Biodiesel fuel, a fuel with physical characteristics similar to petroleum diesel fuel but which is
derived from oils of biological origin (e.g. soybean, rapeseed, sunflower), is well established in
western Europe and is an emerging market in the North American fuel industry. Production
processes include cold pressing oil seeds while other use trans-esterification. It has been
reported that Germany, Austria and Sweden use 100% pure biodiesel (B100) in adapted vehicles.
[P3] In France, biodiesel is used as a 30% blend (B30) with petroleum diesel fuel for use in
captive fleets. [P3] In France and Italy it is used as a 5% blend (B5) in normal diesel fuel. [P3]
In some regions of the USA and Canada biodiesel is marketed as a 20% blend with petroleum
diesel fuel (B20). [P4]. It is anticipated that fire debris analysts will eventually see biodiesel
fuels in casework and so a number of recent publications have been included in this review. The
production of biodiesel fuel by transesterification of sunflower oil [P5] and via methanolysis of
used frying oil have been described. [P6] Lang and co-workers report on an assessment of the
physical properties of biodiesel fuel and compare them with conventional, petroleum-derived
diesel fuel. [P7] A comparison of different chromatographic techniques, including high-pressure
liquid chromatography-mass spectrometry (HPLC-MS), for the analysis of the acylglyerols and
methyl esters of fatty acids has been reported. [P8] Knothe describes a plethora of
chromatographic and spectroscopic methods, such as gas chromatography, gel permeation
chromatography, HPLC, MS, infrared spectroscopy (IR) and nuclear magnetic resonance
spectroscopy (NMR), including their advantages and disadvantages, for the analysis of biodiesel
fuels. [P9]

MISCELLANEOUS STUDIES

Accelerant transfer and persistence

The examination of a suspect’s hands for the presence of gasoline has been presented by Rolph
and co-workers. [Q1] They examined the use of a number of supports in combination with a
DLFEX® device. Lentini used passive headspace adsorption together with GC-MS to study the
persistence of solvents in floor coating materials, including stain, oil finish, and polyurethane
varnish, over a two-year period. [Q2] The volatile organic compounds present on a range of
clothing items were examined by GC-MS and the result presented. [Q3] This study showed that
some volatile organics can persist in clothing even after washing, and that plastic bags used to
wrap new clothing was one possible source for these compounds.

Chalmers and co-workers reported the effects of microbial action in soil on the chromatographic
profile of automotive gasoline, a barbecue starter fluid (medium petroleum distillate) and a diesel
fuel (heavy petroleum distillate). [Q4] From the environmental literature is a report on two case
studies of an oil spill that occurred in 1979 and chronic diesel fuel spills from 1953 to 1991. [Q5]
The authors examined the change in hydrocarbon distribution patterns resulting from long-term
anaerobic microbial degradation.

Contamination and background interference

The pyrolysis products from a large number of substrates, including wood, plastics and paper
products, were reported by Stauffer together with descriptions of proposed reaction mechanisms
involved in the production of these compounds. [R1,R2] Work describing the pyrolysis products
obtained from a variety of materials using both a non-oxidative pyrolysis technique (pyrolysis-
gas chromatography-mass spectrometry) and oxidative pyrolysis has been reported. [R3] Ballice
and Reimert used GC-MS to identify the pyrolysis products from different forms of

315
polypropylene. [R4] The pyrolysis products that emanate from car carpets, and how these
products interfere with the identification of gasoline, have been reported by Cavanah et al. [R5]
The authors also reported that the amount a vehicle is used, and the behaviour of the occupants
will affect the types of compounds found on previously uncontaminated carpeting. Fernandes
and co-workers studied the pyrolysis products obtained by partially burning some common
household items, including paper products, carpet, vinyl flooring, veneer, and shoe polish. [R6]
A commentary on this article [R7] and the author’s response have also been published. [R8]

An in depth review article on the toxicological effects of turpentine contains a wealth of valuable
information on the history, production and chemical composition of turpentine. [R9]

McGee and Lang studied the potential interference of a micelle encapsulator fire suppression
agent on the GC analysis of fire debris samples. [R10] The authors found that although the fire
suppression agent did affect the chromatographic results, it did not interfere with the
identification of common ignitable liquids.

CONCLUSIONS

A number of new resources, including fire dynamics software, for the fire investigator and
analytical chemist have been recently published:
Ignition Handbook by Babrauskas (reference [A14])
Forensic Fire Scene Reconstruction by Icove and DeHaan (reference [A15]);
Analysis and Intrepetation of Fire Scene Evidence, Almirall, JR and Furton, KG (editors)
(reference) [K3]; and,
NIST Fire Dyanmics Simulator (FDS) software and Smokeview software. Building and Fire
Research Laboratory, National Institute of Standards and Technology (reference [B4]).

In the area of fire scene examination a number of reports have focused on the examination of
origin and cause of electrical fires and the different aspects of spontaneous combustion. Very
little recent work has been published on vehicle fires and accelerant detection canines.

Analytical methods for fire debris that incorporate solid phase micro-extraction (SPME) and gas
chromatography-mass spectrometry (GC-MS) or GC-MS-MS have dominated the literature in
recent years. New techniques such as gas chromatography-isotope resonance mass spectrometry
(GC-IRMS), two-dimensional gas chromatography (GC x GC), and membrane introduction mass
spectrometry (MIMS) show promise as potential future techniques for fire debris analysis. A
resurgence of interest has occurred in the discrimination of accelerants, in particular gasoline,
resulting in a significant number of new approaches being evaluated and published. To date no
recent work has been reported on the forensic analysis of biodiesel fuel in the context of an arson
investigation. A small amount of recent work has added to our knowledge of accelerant transfer
and persistence as well as pyrolysis product backgrounds.

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July: 9.
C4. Goodson, ME and Perryman, T. Spray-in foam insulation - energy efficient and electric
nightmare. Proceedings of the American Academy of Forensic Sciences, Atlanta,
Georgia February 11-16, 2002.) (Goodson, ME; Perryman, T; Colwell, K. Effects of
polyurethane foam systems on wiring ampacity. Fire and Arson Investigator, 2002; July:
47-49.
C5. Okamoto, K; Watanabe, N; Hagimoto, Y. Fire hazard caused by thermal degradation of
organic insulating materials at plug and receptacle connection. Fire and Materials; eighth
international conference: January 27-28, 2003; San Francisco, USA. Full article
available in reference [A16].
C6. Hagimoto, Y; Watanabe, N; Okamoto, K. Short-circuit faults in electrical cables and
cords exposed to radiant heat. Fire and Materials; eighth international conference:
January 27-28, 2003; San Francisco, USA. Full article available in reference [A16].
C7. Wenzig, AM Jr. The value of using nondestructive examination techniques to assist in
forensic investigations. Fire and Arson Investigator, 2002; January: 40-41.
C8. Rochon, V. Non-destructive testing using X-rays. Canadian Association of Fire
Investigators, 2002; December: 7-9.
C9. Park, S-W; Kim, S-H; Park, N-K; Kim, Y-H; Kim, Y-M. A comparison of the
microstructures of surface melted Cu-wire. Proceedings of the American Academy of
Forensic Sciences, Atlanta, Georgia February 11-16, 2002.
C10. Lee, EP; Ohtani, H; Matsubara, Y, Seki, T; Hasegawa, H; Imada, S; Yashiro, I. Study on
discrimination between primary and secondary molten marks using carbonized residue.
Fire Safety Journal, 2002; 37(4): 353-368.
C11. Shefchick, TP. Limitations of the auger analysis of electrical arc beads. Proceedings of
the American Academy of Forensic Sciences, Atlanta, Georgia February 11-16, 2002.
C12. Chen, CY; Ling, YC; Wang, JT; Chen, HY. SIMS depth profiling analysis of electrical
arc residues in fire investigation. Applied Surface Science, 2003; 203: 779-784.
C13. Babrauskas, V. Fires due to electric arcing: can ‘cause’ beads be distinguished from
‘victim’ beads by physical and chemical testing? Fire and Materials; eighth international
conference: January 27-28, 2003; San Francisco, USA. Full article available in reference
[A16].

Non-electrical fires

D1. McAuley, D. The combustion hazard of plastic domestic heating oil tanks and their
contents. Forensic Science International, 2003; 43(3): 145-148.
D2. Rochon, V. Technical investigations of marine fire and explosions. Canadian
Association of Fire Investigators, 2002; March: 9-10.
D3. Van Vaerenbergh, G. An unusual arson case: polymer grains, a mineral spirit, solid
bricks containing kerosene and a glycolether used as fuels. Forensic Science
Communications, 2002; 4(1):
http://www.fbi.gov/hq/lab/fsc/backissu/jan2002/van.htm
D4. Rodante, TV Analysis of an LPG explosion and fire. Process Safety Progress, 2003;
22(3): 174-181.

319
D5. Grand, AF; Black, WZ; Beitel, JJ. Flammability of hydraulic fluid under pressure: real
scale simulation of a fire incident. Fire and Materials; eighth international conference:
January 27-28, 2003; San Francisco, USA. Full article available in reference [A16].
D6. Wickström, U; Ignason, H; Van Hees, P. The SP investigation of the discotheque fire in
Göteborg 1998. Fire and Materials; eighth international conference: January 27-28,
2003; San Francisco, USA. Full article available in reference [A16].

Vehicle fires

E1. Byers, KD and Sutherland, DA. Vehicle test burns. Canadian Association of Fire
Investigators, 2002; December: 19-21.
E2. Hirschler, MM; Hoffmann, DJ; Hoffmann, JM; Kroll, EC. Fire hazard associated with
passenger cars and vans. Fire and Materials; eighth international conference: January 27-
28, 2003; San Francisco, USA. Full article available in reference [A16].
E3. DeHaan, JD and Fisher, FL. Reconstruction of a fatal fire in a parked motor vehicle.
Fire and Arson Investigator, 2003; January: 42-46.
E4. Chow WK and Li, JSM. Case study: vehicle fire in a cross-harbour tunnel in Hong
Kong. Tunneling and Underground Space Technology, 2001; 16(1): 23-30.
E5. Service, AG and Lewis, RJ. The forensic examination of a fire-damaged vehicle.
Journal of Forensic Sciences, 2001; 46(4): 950-953.
E6. Jones, M. Investigation of fraudulent arson involving a racing car. Science & Justice,
2002; 42(4): 231-234.
E7. Adair, TW; DeLong, L; Dobersen, MJ; Sanamo, S; Young, R; Oliver, B; Rotter, T.
Suicide by fire in a car trunk: a case with potential pitfalls. Journal of Forensic Sciences,
2003; 48(5): 1113-1116.
E8. Du Pasquier, E. Investigation des Incendies de Véhicles Automobiles. Presses
Polytechniques et Universitaires Romandes, Laussane, Switzerland, 2003. ISBN 2-
88074-531-4.

Spontaneous combustion

F1. Beamish, BB; Barakat, MA; St George, JD. Spontaneous-combustion propensity of New
Zealand coals under adiabatic conditions. International Journal of Coal Geology, 2001;
45(2-3): 217-224.
F2. Beamish, BB; Lau, AG; Moodie, AL ; Vallance, TA. Assessing the self-heating
behaviour of Callide coal using a 2-metre column. Journal of Loss Prevention in the
Process Industries, 2002; 15(5): 385-390.
F3. Amel'chugov, SP; Bykov, VI; Tsybenova, SB. Spontaneous combustion of brown-coal
dust. Experiment determination of kinetic parameters and numerical modeling.
Combustion Explosion and Shock Waves, 2002; 38(3): 295-300.
F4. Guyaguler, T; Karpuz, C; Bagci, S. The spontaneous combustion characteristics of
Turkish lignite and correlation of the self-heating process with the actual fire. CIM
Bulletin, 2003; 96(1070): 75-79.
F5. Sensogut, C; Kaufmann, M; Petit, E. An approach to the modelling of spontaneous
combustion in the goaf. Journal of the South African Institute of Mining and Metallurgy,
2002; 102(5): 311-313.
F6. Anonymous. Role of oils in spontaneous combustion. Biocycle, 2003; 44(2): 14.
F7. Clothier, PQE and Pritchard, HO. Atmospheric oxidation and self-heating in rubber-
containing materials. Flame and Combustion, 2003; 133: 207-210.
F8. Ruggeln, R and Rynk, R. Self-heating in yard trimmings: conditions leading to
spontaneous combustion. Compost Science & Utilization, 2002; 10(2): 162-182.

320
F9. Wakelyn, PJ and Hughs, SE. Evaluation of the flammability of cotton bales. Fire and
Materials, 2002; 26(4-5): 183-189.
F10. Hudak, PF. Spontaneous combustion of shale spoils at a sanitary landfill. Waste
Management, 2002; 22(6): 687-688.
F11. Wolters, FC; Pagni, PJ; Frost, TR; Cuzzillo, BR. Size constraints on self ignition of
charcoal briquettes. Paper presented at: Fire Safety Science – Proceedings of the 7th
International Symposium, 2002; May 19-23: p593-604. Worchester, USA.
F12. Jones, JC. A theoretical examination of the possibility of spontaneous combustion of
laundry in tumble dryers. Journal of Fire Sciences, 2001; 19(3): 181-189.
F13. Jones, JC. A theoretical examination of the possibility of spontaneous combustion of
laundry in tumble dryers part 2: The role of reactive contaminants. Journal of Fire
Sciences, 2001; 19(5): 335-339.
F14. Cuzzillo, BR. Pyrophoria. PhD Dissertation, University of California, Berkeley, USA.
1997
F15. Cuzzillo, BR and Pagni, PJ. Low-temperature wood ignition. Fire Findings, 1999; 7(2):
7-10.
F16. Cuzzillo, BR and Pagni, PJ. The myth of pyrophoric carbon. Paper presented at: Fire
Safety Science – Proceedings of the 6th International Symposium, 1999; July 5-9: p301-
312. Poitiers, France.
F17. Babrauskas, V. Pyrophoric carbon…the jury is still out. Fire and Arson
Investigator, 2001; 52(1): 12-14.
F18. Cuzzillo, BR; Pagni, PJ; Williamson, RB; Schroeder, RA. The verdict is in! Pyrophoric
carbon is out! Fire and Arson Investigator, 2002; 53(1): 19-21.
F19. Babrauskas, V. Properly designed experiments are still needed in order to understand
low-temperature, long-term ignitions of wood. Fire and Arson Investigator, 2003; 53(3):
7-9.

Accelerant detection canines

G1. Williams, M and Johnston, JM. Training and maintaining the performance of dogs
(Canis familiaris) on an increasing number of odor discriminations in a controlled setting.
Applied Animal Behaviour Science, 2002; 78(1): 55-65.
G2. Gazit, I; Lavner, Y; Bloch, G ; Azulai, O; Goldblatt, A; Terkel, J. A simple system for
the remote detection and analysis of sniffing in explosives detection dogs. Behavior
Research Methods Instruments & Computers, 2003; 35(1): 82-89.
G3. Gazit, I and Terkel, J. Explosives detection by sniffer dogs following strenuous physical
activity. Applied Animal Behaviour Science, 2003; 81(2): 149-161.
G4. Jones, BJ; Du Pasquier, E; Ansett, V; Lear, A. Development and validation of canine
accelerant detection program. (Oral presentation). 16th International Symposium on the
Forensic Sciences, Canberra, May 2002.
G5. Turin, L. A method for the calculation of odor character from molecular structure.
Journal of Theoretical Biology, 2002; 216: 367-385.

Sample collection and packaging

H1. Koussiafes, MP. Evaluation of fire scene contamination by using positive-pressure

ventilation fans. Forensic Science Communications, 2002; 4(4):
http://www.fbi.gov/hq/lab/fsc/backissu/oct2002/koussiafes.htm
H2. Zakaib, GM and Delovitch, SA. Preserving the evidence - don't get burned. Canadian
Association of Fire Investigators, 2002 (Dec):12-16.

321
Training and research

I1. Donahue, ML. The ATF Fire Research Laboratory: a new forensic resource for fire-
scene investigations. Forensic Science Communications, 2002; 4(1):
http://www.fbi.gov/hq/lab/fsc/backissu/jan2002/donahue.htm
I2. Madrzykowski, D. Fire research: providing new tools for fire investigation. Fire and
Arson Investigator, 2002; July: 43-46.
I3. Mannan, MS; Aldeeb, AA; Rogers, WJ. Understanding the role of process chemistry in
fires and explosions. Process Safety Progress, 2002; 21(4): 323-328.

Internet resources

J1. Arson Prevention Bureau; http://www.arsonpreventionbureau.org.uk

J2. Building and Fire Research Laboratory - Fire on the Web; http://fire.nist.gov and
http://www.bflr.nist.gov
J3. Bureau of Alcohol, Tobacco and Firearms (ATF);
http://www.atf.treas.gov.explarson/index.htm
J4. Canadian Association of Fire Investigators (CAFI); http://www.cafi.ca
J5. Canine Accelerant Detection Association; http://www.cadafiredogs.com
J6. European Network for Forensic Science Institutes - Fire and Explosion Investigation
Working Group; http://homepages.strath.ac.uk/~cbas53/niamh/fire
J7. Fire Findings Newsletter; http://www.firefindings.com
J8. FireNet - Electronic Pages for the British Fire Service; http://fire.org.uk/home.htm
J9. Fire Protection Association Australia; http://www.fpaa.com.au
J10. Fire Science and Technology Incorporated: Fire Science Publishers;
http://www.doctorfire.com/links.html
J11. Forensic Science Journal; http://sun4.cpu.edu.tw/~fsjournal/
J12. InterFIRE Online; http://www.interfire.org
J13. International Association of Arson Investigators (IAAI); http://www.firearson.com
J14. National Association of Fire Investigators; http://www.nafi.org
J15. National Center for Forensic Sciences - Technical Working Group for Fire and
Explosions;http://ncfs.ucf.edu/twgfex/home.html and
http://www.ncfs.ucf.edu/databases.html
J16. National Fire Protection Association (NFPA);
http://www.nfpa.org/catalog/home/index.asp
J17. United States Fire Administration; http://usfa.fema.gov

Laboratory analysis of fire debris samples

General

K1. Minnich, TE and McCardle, R. National Centre for Forensic Science. Fire and Arson
Investigator, 2002; April: 33-37.
K2. Stauffer, T and Lentini, JJ. ASTM standards for fire debris analysis: a review. Forensic
Science International, 2003; 132(1): 63-67.
K3. Almirall, JR and Furton, KG (editors). Analysis and Intrepetation of Fire Scene
Evidence. CRC Press, Boca Raton, Florida, USA; 2004. ISBN 0-8493-7885-0.
K4. Dolan, J. Recent advances in the applications of forensic science to fire debris analysis.
Analytical and Bioanalytical Chemistry, 2003; 376(8): 1168-1171.

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Sampling and sample preparation techniques

L1. Snow, NH and Slack, GC. Head-space analysis in modern gas chromatography. TrAC -
Trends in Analytical Chemistry, 2002; 21(9-10): 608-617.
L2. Almirall, JR and Furton, KG. New developments in sampling and sample preparation for
forensic analysis. In: Comprehensive Analytical Chemistry XXXVII. Pawliszyn, J
(Editor), Chapter 27; Elsevier Science, 2002.
L3. American Society for Testing and Materials (2001). E 2154-01 Standard Practice for
Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by
Passive Headspace Concentration with Solid Phase Microextraction (SPME).
L4. Perr, JM; Diaz, CJ; Furton, KG, Almirall, JR. The analysis of ignitable liquid residues
and explosive material using SPME/GC/MS/MS. Proceedings from the American
Academy of Forensic Sciences, Chicago, IL, USA; February 17-22, 2003.
L5. Harris, AC and Wheeler, JF. GC-MS of ignitable liquids using solvent-desorbed SPME
for automated analysis. Journal of Forensic Sciences, 2003; 48(1): 41-46.
L6. Lloyd, JA and Edmiston, PL. Preferential extraction of hydrocarbons from fire debris
samples by solid phase microextraction. Journal of Forensic Sciences, 2003; 48(1): 130-
134.
L7. Garafano, L; Gregori, A; Santoro, M; Russo, A. The use of SPME in the recognition of
hydrocarbons in cases of arson. Proceedings of the American Academy of Forensic
Sciences, Atlanta, Georgia February 11-16, 2002.
L8. Hook, GL; Kimm, GL; Hall, T; Smith, PA. Solid-phase microextraction (SPME) for
rapid field sampling and analysis by gas chromatography-mass spectrometry (GC-MS).
TrAC - Trends in Analytical Chemistry, 2002; 21(8): 534-543.
L9. Kwon, M; Hong, S; Choi, H. Sampling of highly volatile accelerants at the fire scene.
Canadian Society of Forensic Science Journal, 2003; 36(4): 197-205.
L10. Massey, D; Du Pasquier, E; Lennard, C. Study for substitution of carbon disulfide by
another solvent for desorption of charcoal strip (DLFEXtm) in analysis of fire samples
(Poster). 16th International Symposium on the Forensic Sciences, Canberra, May 2002.
L11. Massey, D; Du Pasquier, E; Lennard, C. Solvent desorption of charcoal strips
(DFLEX®) in the analysis of fire debris samples: replacement of carbon disulfide.
Canadian Society of Forensic Science Journal, 2002; 35(4): 195-208.
L12. Egli, NM; Delemont, O; DeHaro, D; Lacarriere, J-F. Research for a substitute for carbon
disulfide as elution solvent of DFLEX® membranes used in the analysis of fire
accelerants: comparison of solvent mixtures. Proceedings of the European Academy of
Forensic Science, Triennial Meeting, September 22-27, 2003; Istanbul, Turkey.
L13. Massey, D, Du Pasquier, E, Lennard, C. Optimisation of Fire Debris Analysis with
DFLEX®. Proceedings of the International Association of Forensic Science,
Montpellier, France. September 1-7, 2002.
L14. Smith, ET and Warnke, MM. Arson analysis by static headspace enrighment and gas
chromatography using simplex optimization (Poster). 2003 Pittsburgh Conference on
Analytical Chemistry and Applied Spectroscopy (Pittcon), Orlando, FL, March 9-14,
2003.
L15. Huang, CT and Hsieh, YZ. Analysis of petroleum distillates from fire debris using
supercritical fluid extraction with a two-level orthogonal array experimental design.
Journal of the Chinese Chemical Society, 2002; 49(4): 517-525.
L16. Giang, Y-S; Chang, W-T; Wang, S-M; Chou, S-L. Looking into some basic properties of
accelerants in fire residues for higher performance in arson analysis. Forensic Science
Journal, 2003; 2: 19-26. Article available on-line, see reference [J11].

323
Chromatographic analysis (GC-MS, GC-MS-MS, isotope ratios, GC x GC)

M1. Coulombe, R. Chemical analysis of vegetable oils following spontaneous ignition.

Journal Forensic Sciences, 2002; 47(1): 195-201. Converted dried oil to fatty acid
methyl ester and analyzed with GC-MS.
M2. Perr, JM and Almirall, JR. Comprehensive approach to determine the absolute detection
limit for organic compounds in a standard accelerant mixture between GC/MS and
GC/MS/MS. Proceedings of the American Academy of Forensic Sciences, Atlanta,
Georgia February 11-16, 2002.
M3. Perr, JM; Furton, KG; Almirall, JR. A comprehensive approach for analyzing ignitable
liquid residues and explosive material using SPME/GC/MS/MS. Proceedings of the
International Association of Forensic Science, Montpellier, France. September 1-7,
2002.
M4. de Vos, BJ; Froneman, M; Rohwer, E; Sutherland, DA. Detection of petrol (gasoline) in
fire debris by gas chromatography/mass spectrometry/mass spectrometry (GC/MS/MS).
Journal of Forensic Sciences, 2002; 47(4): 736-756.
M5. Sutherland, DA; Perr, J; Almirall, J. Identification of Ignitable Liquid Residues in Fire
Debris by GC/MS/MS (Chapter 5). In: Advances in Forensic Applications of Mass
Spectrometry, Third Edition; Yinon, Y. (Editor). CRC Press, Boca Raton, USA; 2003.
M6. Sittidech, M. Part I. Analysis of aromatic amines in banned azo dyes by SPME and
GC/MS/MS. Part II. Analysis of residual ignitable fluids in fire debris by GC/MS/MS
and development of an expert system. PhD Thesis (2002), University of Alabama,
Tuscaloosa, Alabama,USA. ISBN 0-493-87075-X.
M7. Marriott, P and Shellie, R Principles and applications of comprehensive two-dimensional
gas chromatography. TRAC-Trends in Analytical Chemistry, 2002; 21(9-10): 573-583.)
M8. Ong, RCY and Marriott, PJ. A review of basic concepts in comprehensive two-
dimensional gas chromatography. Journal of Chromatographic Science, 2002; 40(5):
276-291.
M9. Pursch, M; Sun, K; Winniford, B; Cortes, H; Weber; A; McCabe, T; Luong, J.
Modulation techniques and applications in comprehensive two-dimensional gas
chromatography (GCxGC). Analytical and Bioanalytical Chemistry, 2002; 373(6): 356-
367.
M10. Beens, J; Adahchour, M; Vreuls, RJJ; van Altena, K; Brinkman, UAT. Simple non-
moving modulation interface for comprehensive two-dimensional gas chromatography.
Journal of Chromatography A, 2001; 919(1): 127-132.
M11. Adahchour, M; Beens, J; Brinkman, UAT. Single-jet single-stage cryogenic modulator
for comprehensive two-dimensional gas chromatography (GC x GC). Analyst, 2003;
128(3): 213-216.
M12. Burger, BV; Snyman, T; Burger, WJG; van Rooyen, WF. Thermal modulator array for
analyte modulation and comprehensive two-dimensional gas chromatography. Journal of
Separation Science, 2003; 26(1-2): 123-128.
M13. Haglund, P; Harju, M; Danielsson, C; Marriot, P. Effects of temperature and flow
regulated carbon dioxide cooling in longitudinally modulated cryogenic systems for
comprehensive two-dimensional gas chromatography. Journal of Chromatography A,
2002; 962(1-2): 127-134.
M14. Kallio, M; Hyötyläinen, T; Jussila, M; Hartonen, K; Palonen, S; Shimmo, M; Riekkola,
ML. Semi-rotating cryogenic modulator for comprehensive two-dimensional gas
chromatography. Analytical and Bioanalytical Chemistry, 2003; 375(6): 725-731.
M15. Hyötyläinen, T; Kallio, M; Hartonen, K; Jussila, M; Palonen, S; Riekkola, ML.
Modulator design two-dimensional for comprehensive gas chromatography: Quantitative
analysis of polyaromatic hydrocarbons and polychlorinated biphenyls. Analytical
Chemistry, 2002, 74(17): 4441-4446.

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M16. Harynuk, J; Gorecki, T; Campbell, C. On the interpretation of GC x GC data. LCGC
North America, 2002; 20(9): 877-891.
M17. Blumberg, LM. Comprehensive two-dimensional gas chromatography: metrics
potentials limits. Journal of Chromatography A, 2003; 985(1-2): 29-38.
M18. Shellie, RA; Xie, LL; Marriott, PJ. Retention time reproducibility in comprehensive two-
dimensional gas chromatography using cryogenic modulation - An intralaboratory study.
Journal of Chromatography A, 2002; 968(1-2): 161-170.
M19. Western, RJ and Marriott, PJ. Retention correlation maps in comprehensive two-
dimensional gas chromatography. Journal of Separation Science, 2002; 25(13): 832-838.
M20. Reichenbach, SE; Ni, MT; Zhang, DM; Ledford, EB. Image background removal in
comprehensive two-dimensional gas chromatography. Journal of Chromatography A,
2003; 985(1-2): 47-56.
M21. Frysinger, GS; Gaines, RB; Reddy, CM. GC x GC - A new analytical tool for
environmental forensics. Environmental Forensics, 2002; 3(1): 27-34.
M22. Frysinger, GS and Gaines, RB. Separation and identification of petroleum biomarkers by
comprehensive two-dimensional gas chromatography. Journal of Separation Science,
2001; 24(2): 87-96.
M23. Frysinger, GS; Gaines, RB; Xu, L; Rreddy, CM. Resolving the unresolved complex
mixture in petroleum-contaminated sediments. Environmental Science & Technology,
2003; 37(8): 1653-1662.
M24. Frysinger, GS and Gaines RB. Forensic analysis of ignitable liquids in fire debris by
comprehensive two-dimensional gas chromatography. Journal of Forensic Sciences,
2002; 47(3): 471-482.
M25. Hua, RX; Ruan, CH; Wang, JH; Lu, X; Liu, J; Xiao, K; Kong, HW; Xu, GW. Research
of group has described the optimization for the separation of petroleum fractions by
comprehensive two-dimensional gas chromatography. Acta Chimica Sinica, 2002;
60(12): 2185-2191.
M26. Adahchour, M; Beens, J; Vreuls, RJJ; Batenburg, AM; Rosing, EAE; Brinkman, UAT.
Application of solid-phase micro-extraction and comprehensive two-dimensional gas
chromatography (GCxGC) for flavour analysis. Chromatographia, 2002; 55(5-6): 361-
367.
M27. Dalluge, J; van Stee, LLP; Xu, XB; Williams, J; Beens, J; Vreuls, RJJ; Brinkman, UAT.
Unravelling the composition of very complex samples by comprehensive gas
chromatography coupled to time-of-flight mass spectrometry - Cigarette smoke. Journal
of Chromatography A, 2002; 974(1-2): 169-184.
M28. Dalluge, J; Vreuls, RJJ; Beens, J; Brinkman, UAT. Optimization and characterization of
comprehensive two-dimensional gas chromatography with time-of-flight mass
spectrometric detection (GC x GC-TOF MS). Journal of Separation Science, 2002; 25(4):
201-214.
M29. Dimandja, JMD. A new tool for the optimized analysis of complex volatile mixtures:
comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry.
American Laboratory, 2003; 35(3): 42-+.
M30. Johnson, KJ; Prazen, BJ; Olund, RK; Synovec, RE. GC x GC temperature programming
requirements to produce bilinear data for chemometric analysis. Journal of Separation
Science, 2002; 25(5-6): 297-303.
M31. Seeley, JV; Kramp, FJ; Sharpe, KS; Seeley, SK. Characterization of gaseous mixtures of
organic compounds with dual-secondary column comprehensive two-dimensional gas
chromatography (GC x 2GC). ) Journal of Separation Science, 2002; 25(1-2): 53-59.
M32. Sinha, AE; Johnson, KJ; Prazen, BJ; Lucas, SV; Fraga, CG; Synovec, RE.
Comprehensive two-dimensional gas chromatography of volatile and semi-volatile
components using a diaphragm valve-based instrument. Journal of Chromatography A,
2003; 983(1-2): 195-204.

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M33. Harynuk, J and Gorecki, T. New liquid nitrogen cryogenic modulator for comprehensive
two-dimensional gas chromatography. Journal of Chromatography A, 2003; 1019: 53-
63.
M34. Philp, RP. Application of stable isotopes and radioisotopes in environmental forensics.
In: Introduction to Environmental Forensics, Murphy, BL and Morrison, RD (editors);
Academic Press, 2002.
M35. Philp, RP; Allen, J; Kuder, T. The Use of the Isotopic Composition of Individual
Compounds for Correlating Spilled Oils and Refined Products in the Environment with
Suspected Sources. Environmental Forensics, 2002; 3(3-4): 341-348.
M36. Budzinski, H; Mazeas, L; Le Menach, K. C-13 analysis of PAH: A new dimension in
6source assessment studies. Chimia, 2003; 57(1-2): 41-43.
M37. Mazeas, L and Budzinski, H. Molecular and stable carbon isotopic source identification
of oil residues and oiled bird feathers sampled along the Atlantic coast of France after the
Erika oil spill. Environmental Science & Technology, 2002; 36(2): 130-137.
M38. Mazeas, L; Budzinski, H; Raymond, N. Absence of stable carbon isotope fractionation
of saturated and polycyclic aromatic hydrocarbons during aerobic bacterial
biodegradation. Organic Geochemistry, 2002; 33(11): 1259-1272.
M39. Pond, KL; Huang, YS; Wang, Y; Kulpa, CF. Hydrogen isotopic composition of
individual n-alkanes as an intrinsic tracer for bioremediation and source identification of
petroleum contamination. Environmental Science & Technology, 2002; 36(4): 724-728.
M40. Smallwood, BJ; Philp, RP; Allen, JD. Stable carbon isotopic composition of gasolines
determined by isotope ratio monitoring gas chromatography mass spectrometry. Organic
Geochemistry, 2002; 33(2): 149-159.
M41. Smallwood, BJ; Philp, RP; Burgoyne, TW; Allen, JD. The use of stable isotopes to
differentiate specific source markers for MTBE. Environmental Forensics, 2001; 2(3):
215-221.
M42. Jasper, JP; Edwards, JS; Ford, LC; Corry, RA. Putting the arsonist at the scene: “DNA”
for the fire investigator. Fire and Arson Investigator, 2002; (Jan):30-34.
M43. Jasper, JP; Edwards, JS; Ford, LC; Corry, RA. An initial report of the arson stable
isotope analysis project. Proceedings from the American Academy of Forensic Sciences,
Chicago, IL, USA. February 17-22, 2002.

Data interpretation (includes chemical fingerprinting)

N1. Comment, S; Ertan, E; Martin, J-C. Determination of the type of accelerant present in
fire debris using neural networks (Poster). 16th International Symposium on the Forensic
Sciences, Canberra, May 2002.
N2. Moore, PA; Crabtree, JH; Chin, GW; Gdowski, FM. A computer assisted GC-MS
method for identifying flammable substances in fire debris. Proceedings of the American
Academy of Forensic Sciences, Atlanta, Georgia; February 11-16, 2002.
N3. Trimpe, M and Chasteen, C. Comparing gasoline samples in the forensic laboratory.
Fire and Arson Investigator, 2002; (Jul): 28.
N4. Dolan, JA and Ritacco, CJ. Gasoline comparisons by gas chromatograph-mass
spectrometry utilizing an automated approach to data analysis. Proceedings of the
American Academy of Forensic Sciences, Atlanta, Georgia; February 11-16, 2002.
N5. Sandercock, PML and Du Pasquier, E. Chemical fingerprinting of unevaporated
automotive gasolines. Forensic Science International, 2003; 134(1): 1-10.
N6. Sandercock, PML. Forensic Comparison of Unevaporated and Evaporated Automotive
Gasoline Samples from Australia and New Zealand. PhD Thesis, University of
Technology, Sydney, NSW, Australia. December, 2002.

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N7. Sandercock, PML and DuPasquier, E. Chemical fingerprinting of gasoline. 2.
Comparison of unevaporated and evaporated automotive gasoline samples. Forensic
Science International, 2004; 140(1): 43-59.
N8. Sandercock, PML and DuPasquier, E. Chemical fingerprinting of gasoline. 3.
Comparison of unevaporated automotive gasoline samples from Australia and New
Zealand. Forensic Science International, 2004; 140(1): 71-77.
N9. Doble, P; Sandercock, M; Du Pasquier, E; Petocz, P; Roux, C; Dawson, M.
Classification of premium and regular gasoline by gas chromatography/mass
spectrometry principal component analysis and artificial neural networks. Forensic
Science International, 2003; 132(1): 26-39.
N10. Peshier, LJC. Comparison studies of automotive gasoline. Proceedings of the European
Academy of Forensic Science, Triennial Meeting, September 22-27, 2003; Istanbul,
Turkey.
N11. Carraze, B; Delafoy, J; Bertin, J; Beziau, J-F; Lange, CM. Mass spectral fingerprints of
detergents in gasolines using electospray ionization. Rapid Communications in Mass
Spectrometry, 2004; 18: 451-457.
N12. Stout, SA; Uhler, AD; McCarthy, KJ; Emsbo-Matingly, S. Chemical fingerprinting of
hydrocarbons. In: Introduction to Environmental Forensics. Murphy, BL and Morrison,
RD (editors), Chapter 6; Academic Press, 2002.
N13. Uhler, AD; Stout, SA; Douglas, GS; McCarthy, KJ; Emsbo-Mattingly, S. The influences
of refining on petroleum fingerprinting. Part 1. The refining process. Contaminated Soil
Sediment and Water, 2001: October.
Available on-line at <http://www.aehsmag.com/issues.htm>
N14. Stout, SA; Uhler, AD; McCarthy, KJ; Emsbo-Mattingly, S; Douglas, GS. The influences
of refining on petroleum fingerprinting. Part 2. Gasoline blending practices.
Contaminated Soil Sediment and Water, 2001: December. Available on-line: see Ref
[N13].
N15. Stout, SA; Uhler, AD; McCarthy, KJ; Emsbo-Mattingly, S; Douglas, GS. The influences
of refining on petroleum fingerprinting. Part 3. Distillate fuel production practices.
Contaminated Soil Sedient and Water, 2002: January-February. Available on-line: see
Ref [N13].
N16. Uhler, AD; Stout, SA; McCarthy, KJ; Emsbo-Mattingly, S; Douglas, GS; Beall, PW.
The influences of refining on petroleum fingerprinting. Part 4. Residual fuels.
Contaminated Soil Sedient and Water, 2002: April. Available on-line: see Ref [N13].
N17. Lavine, BK; Brzozowski, D; Moores, AJ; Davidson, CE; Mayfield, HT. Genetic
algorithm for fuel spill identification. Analytical Chimica Acta, 2001; 437(2): 233-246.
N18. Lavine, BK; Vesanen, A; Brzozowski, DM; Mayfield, HT. Authentication of fuel spill
standards using gas chromatography/pattern recognition techniques. Analytical Letters,
2001; 34(2): 281-293.
N19. Lavine, BK; Brzozowski, DM; Ritter, J; Moores, AJ; Mayfield, HT. Fuel spill
identification using solid-phase extraction and solid-phase microextraction. 1. Aviation
turbine fuels. Journal of Chromatographic Science, 2001; 39: 501-507.
N20. Johnson, KJ and Synovec, RE. Pattern recognition of jet fuels: comprehensive GC x GC
with ANOVA-based feature selection and principal component analysis. Chemometrics
and Intelligent Laboratory Systems, 2002; 60(1-2): 225-237.
N21. Pavon, JLP; Sanchez, MD; Pinto, CG; Laespada, MEF; Cordero, BM; Pena, AG. A
method for the detection of hydrocarbon pollution in soils by headspace mass
spectrometry and pattern recognition techniques. Analytical Chemistry, 2003; 75(9):
2034-2041.
N22. Stout, SA. Applications of petroleum fingerprinting in known and suspected pipeline
releases - two case studies. Applied Geochemistry, 2003; 18(6): 915-926.

327
N23. Stout, SA; McCarthy, KJ; Uhler, AD. Bicyclic sesquiterpane biomarkers - useful
hydrocarbons in the chemical fingerprinting [of] Class 4 and Class 5 petroleum
distillates. Proceedings of the American Academy of Forensic Sciences, Atlanta,
Georgia; February 11-16, 2002.

Other analytical methods

O1. Rodgers, RP; Blumer, EN; Freitas, MA; Marshall, AG. Compositional analysis for
identification of arson accelerants by electron ionization Fourier transform ion cyclotron
resonance high-resolution mass spectrometry. Journal of Forensic Sciences, 2001; 46(2):
268-279.
O2. Rodgers, RP; Hughey, CA; Blumer, EN; Hendrickson, CL; Marshall, AG. Forensic
analysis of petroleum products by FT-ICR mass spectrometry. Proceedings of the
American Academy of Forensic Sciences, Atlanta, Georgia; February 11-16, 2002.
O3. Ketola, RA; Kotiaho, T; Cisper, ME; Allen, TM. Environmental applications of
membrane introduction mass spectrometry. Journal of Mass Spectrometry, 2002; 37:
457-476.
O4. Alberici, RM; Zampronio, CG; Poppi, RJ; Eberlin, MN. Water solubilization of ethanol
and BTEX from gasoline: on-line monitoring by membrane introduction mass
spectrometry. Analyst, 2002; 127(2): 230-234.
O5. McCurdy, RJ; Atwell, T; Cole, MD. The use of vapour phase ultra-violet spectroscopy
for the analysis of arson accelerants in fire scene debris. Forensic Science International,
2001; 123(2-3): 191-201.

Analysis of liquids, new products and other materials

P1. Kuk, RJ. Analysis of artificial fireplace logs by high temperature gas chromatography.
Journal of Forensic Sciences, 2002; 47(6): 1288-1293.
P2. Woodrow, JE. The laboratory characterization of jet fuel vapor and liquid. Energy &
Fuel, 2003; 17(1): 216-224.
P3. Platts: Global Commodity News. <http://www.platts.com/features/biofuels/> Accessed
January 9, 2003)
P4. Canadian Clean Fuels. <http://www.canadacleanfuels.com/biodiesel.html> Accessed
January 9, 2003)
P5. Antoln, G; Tinaut, FV; Briceno, Y; Castano, V; Perez, C; Ramrez, AI. Optimisation of
biodiesel production by sunflower oil transesterification. Bioresource Technology, 2002;
83(2): 111-114.
P6. Tomasevic, AV and Siler-Marinkovic, SS. Methanolysis of used frying oil. Fuel
Processing Technology, 2003; 81(1): 1-6.
P7. Lang, X; Dalai, AK; Bakhshi, NN; Reaney, MJ; Hertz, PB. Preparation and
characterization of bio-diesels from various bio-oils. Bioresource Technology, 2001;
80(1): 53-62.
P8. Holcapek, M; Jandera, P; Fischer, J. Analysis of acylglycerols and methyl esters of fatty
acids in vegetable oils and in biodiesel. Critical Reviews in Analytical Chemistry, 2001;
31(1): 53-56.
P9. Knothe, G. Analytical methods used in the production and fuel quality assessment of
biodiesel. Transactions of the ASAE [American Society Agricultural Engineers], 2001;
44(2): 193-200.

328
Miscellaneous studies
Accelerant transfer and persistence

Q1. Rolph, E; Du Pasquier, E; Lennard, C; Royds, D Petrol on hands: handling method and
validity of results (Poster). 16th International Symposium on the Forensic Sciences,
Canberra, May 2002.
Q2. Lentini, JJ. Persistence of floor coating solvents. Journal of Forensic Sciences, 2001;
46(6): 1470-1473.
Q3. Fox, J. Volatile organics on clothing. Proceedings of the European Academy of
Forensic Science, Triennial Meeting, September 22-27, 2003; Istanbul, Turkey.
Q4. Chalmers, D; Yan X; Cassista, A; Hrynchuk, R; Sandercock, PML. Degradation of
gasoline, barbecue starter fluid, and diesel fuel by microbial action in soil. Canadian
Society of Forensic Science Journal, 2001; 34(2): 49-62.
Q5. Hostettler, FD and Kvenvolden, KA. Alkyleyelohexanes in environmental geochemistry.
Environmental Forensics, 2002; 3(3-4): 293-301.

Contamination and background interference

R1. Stauffer, E. Identification and Characterization of Interfering Products in Fire Debris

Analysis. MS Thesis (2001), Florida International University, Miami, Florida, USA.
R2. Stauffer, E. Concept of pyrolysis for fire debris analysts. Science & Justice, 2003;
43(1): 29-40.
R3. Almirall, JR and Furton, KG. Characterization of background and pyrolysis products
that may interfere with the forensic analysis of fire debris. Journal of Analytical and
Applied Pryolysis, 2004: 71(1): 51-67.
R4. Ballice, L and Reimert, R. Classification of volatile products from the temperature-
programmed pyrolysis of polypropylene (PP), atactic-polypropylene (APP) and
thermogravimetrically derived kinetics of pyrolysis. Chemical Engineering and
Processing, 2002; 41(4): 289-296.
R5. Cavanagh, K; Du Pasquier, E; Lennard, C. Background interference from car carpets -
the evidential value of petrol residues in cases of suspected vehicle arson. Forensic
Science International, 2002; 125(1): 22-36.
R6. Fernandes, MS; Lau, CM; Wong, WC. The effect of volatile residues in burnt household
items on the detection of fire accelerants. Science & Justice, 2002; 42(1): 7-15.
R7. Stauffer, E. Commentary on: MS Fernandes CM Lau and WC Wong “The effect of
volatile residues in burnt household items on the detection of fire accelerant” Science &
Justice, 2002; 42(1): 7-15. Science & Justice, 2002; 42(2): 129-130.
R8. Lau, CM; Wong, WC; Fernandes, MS. Erratum and commentary on: MS Fernandes CM
Lau and WC Wong “The effect of volatile residues in burnt household items on the
detection of fire accelerant”, Science & Justice, 2002; 42(1): 7-15. Science & Justice,
2002; 42(4): 243-244.
R9. Haneke, KS. Turpentine (turpentine oil, wood turpentine, sulfate turpentine, sulfite
turpentine) [8006-64-2]: review of toxicological literature. National Institute of
Environmental Health Sciences, North Carolina, USA. February 2002. <http://ntp-
server.niehs.nih.gov/htdocs/Chem_Background/ExSumPdf/turpentine.pdf> Accessed on
November 12, 2003.
R10. McGee, E and Lang, TL. A study of the effects of a micelle encapsulator fire
suppression agent on dynamic headspace analysis of fire debris samples. Journal
Forensic Science, 2002; 47(2): 267-274.

329
Detection and Characterization of
Explosives and Explosives Residues

— A Review: 2001 to 2004 —

Mary Lou Fultz, Ph.D.

Chief, Forensic Science Laboratory – Washington

Bureau of Alcohol, Tobacco, Firearms and Explosives
6000 Ammendale Road
Ammendale, Maryland 20705, USA

330
INTRODUCTION

Interest in the detection and characterization of explosives reaches several different audiences.
Of interest to the forensic laboratory is the recovery and identification of post-blast residue and
intact recovered explosives. Law enforcement and other security agencies are interested in
detecting both trace and bulk amounts of explosives. Trace detection determines whether an
object or person has been in contact with explosives. Bulk detection is used to find large
amounts of concealed explosives before they are used illegally. The Military is interested in
detection of land mines so they can be safely removed. There is an interest in finding explosives
in the environment so that land and water can be remediated. The variety of audiences interested
in explosives detection results in the research being published in a wide variety of journals.

Some research is presented at symposia with only the abstracts being published, while other
proceedings may have full papers published. The 7th International Symposium on the Analysis
and Detection of Explosives was held in Edinburgh, Scotland from June 25-28, 2001, sponsored
by the Defence Evaluation and Research Agency (now known as Dstl – the Defence Science and
Technology Laboratory), an Agency of the United Kingdom Ministry of Defence. Forty papers
were presented in the area of Detection Methodology, Tagging and Vapour Detection, Analysis
of Post Detonation Samples, Studies of Environmental Contamination, Analytical Studies –
Mass Spectrometry, Thermal and other Analytical Methods, and a Poster Session.[1] This
symposium is held every 3 years, bringing together scientists from worldwide forensic
laboratories. A list of the papers 40 papers presented is included in Appendix A of this report.
The 3rd European Academy of Forensic Science Meeting was held in Istanbul, Turkey from
September 22-27, 2003. At the scientific session on fire and explosions, 6 papers were presented
on explosive analysis by researchers from the United Kingdom, Poland, Germany, Russia, and
India. Abstracts of these presentations were published in a supplemental issue of Forensic
Science International.[2] A list of these papers is included in Appendix B.

Various working groups have formed to work on areas of common interest in the area of
explosives. The Netherlands Forensic Institute and the Forensic Explosives Laboratory, Dstl,
United Kingdom founded the Forensic International Network for Explosives Investigation
(FINEX – pronounced Phoenix). This group was formerly known as NFEX. FINEX was formed
as a result of 38 laboratories surveyed expressing an interest in the formation of a forensic
explosives network. The Netherlands Forensic Institute proposed that FINEX be formed as an
Expert Working Group of the European Network of Forensic Science Institutes (ENFSI), and
this proposal has been adopted by ENSFI. The network is intended for Government agencies
active in the field of forensic explosives analysis including crime scene investigation,
examination of physical evidence, including improvised explosive devices and post explosion
debris, chemical analysis, and writing of expert reports and testifying in court as an expert
witness. While FINEX is open to members of ENFSI, it is also open for membership from non-
ENFSI institutes and non-European agencies, providing they are active in the field of explosives
investigation. The activities of FINEX are directed toward the exchange of information and
expertise, support on technical issues, promoting quality assurance, proficiency testing and
collaborative exercises, harmonization of crime scene guidelines, examination procedures, and
analytical methods, and co-operation in research and development projects. The 1st Conference
on the Forensic International Network for Explosives Investigation was held in the Netherlands
on the 14th – 16th of April 2004, with the theme of “Needs in Forensic Explosives Investigation.
During the conference, FINEX was officially founded and a Steering Committee appointed. The
symposium consisted of oral presentation and posters covering the topics of scene examination,
analytical methods and techniques, research and development, quality assurance, and interesting
cases. Copies of the proceedings are available by contacting Susan Phillips of Dstl.[3]

331
During the period of 2001 through 2004, the Forensic Explosives Laboratory of Dstl hosted a
number of meetings and symposia.[4] The International Workshop on the Forensic Aspects of
Peroxide Explosives was held at Dstl Fort Halstead on the 5th and 6th of December 2001.
Approximately 40 delegates from forensic and government agencies in twelve countries attended
the workshop, which aimed to compare types of devices incorporating peroxide explosives.
Methods for the safe handling of peroxides and methods for forensic analysis were discussed.
The International Seminar on the Recovery of Forensic Explosives Evidence was held at the
Thistle Hotel, Dartford, United Kingdom on the 3rd and 4th of September 2003. It was attended
by 65 delegates from forensic laboratories, police forces, and universities worldwide. The
seminar discussed best practices and procedures for the recovery of forensic explosives evidence
from pre- and post-blast scenes. The Network for Forensic Isotope Ratio Mass Spectrometry
(FIRMS) was formed in 2002 by the University of Reading and the Forensic Explosives
Laboratory, Dstl. The network is funded for three years by the United Kingdom Engineering
and Physical Sciences Research Council. The FIRMS network conference was held on the 16th
and 17th of September 2002 at the Thistle Hotel, Dartford, United Kingdom. The conference,
attended by over 50 delegates from forensic establishments, instrument manufacturers, police
forces, and academia, aimed to bring together IRMS researchers, end users, and instrument
manufacturers. The conference aimed to facilitate the exchange of information between
researchers and end users, to understand the statement of requirement for the development of the
use of IRMS in forensic science, and to begin to formulate a strategy for development. The
Proceedings are published in Science and Justice.[5] From the conference, three working groups
were formed, for drugs, explosives, and general forensic science.

In the United States, the Scientific Working Group for Fire and Explosions (SWGFEX), formed
in 1998 to make recommendations for nationally accepted guidelines for the forensic
examination of fire and explosive materials and residues, continues to have yearly symposia
presenting papers on fire and explosives research. A listing of presentations of Symposia held in
2002 and 2003 is included in Appendix C. In addition to the symposia, the group has produced
some documents. In the area of explosives analysis, they have produced an explosives analyst
job description and an explosives analyst’s training guide. The Guide for identification of intact
explosives is currently under discussion for public comment.[6]

Interest in gaining an understanding how best to collect and interpret evidence from large-scale
bombs led to a series of experiments conducting such tests by researchers from the Defence
Evaluation and Research Agency and Forensic Explosives Laboratory in Kent, UK.[7] The tests
were conducted at a range at the New Mexico Institute of Mining and Technology in Socorro,
New Mexico, USA. The three types of explosives used were ammonium nitrate/fuel oil, 2.4.6-
trinitrotoluene, and 2 different size charges of calcium carbonate ammonium nitrate/icing sugar.
The charges were surrounded by road signs and vehicles that served as witness materials to
provide both chemical and physical evidence. Nitrate was generally recovered in greater
quantities than ammonium. Levels of recovery decreased with increasing distance from the
charge. Damage to the witness materials was recorded, along with the velocities of detonation.

During this review period, 2 Ph.D. theses were published in the area of explosives. One dealt
with the forensic evaluation of explosive power and contamination issues[8], and the other with
latent fingerprint and trace explosive detection by photoluminescence and time-resolved
imaging[9]

332
SAMPLE PREPARATION AND ANALYSIS OF EXPLOSIVES

The literature over the past 3 years shows research interest on sample preparation, various
methods development for a variety of explosives, interest in analyzing the effects of explosives,
and analysis of explosives in the environment. Sample preparation research looked into
microextraction and solid phase extraction techniques. In the area of explosives analysis, stable
isotope mass spectrometry is being explored as a possible way to link explosives samples or
determine the source of explosives. Newer instrumental methods explored include capillary
electrophoresis and ion chromatography mass spectrometry. The illegal use of the improvised
peroxide explosives has generated method development for their analysis. Interest in
characterization and identification of propellants used in improvised explosives devices
continues. Mass spectrometry coupled with chromatographic separation continues to be of
interest for the analysis of high explosives. The environmental arena shows methods for either
detecting land mines or analysis of explosives for remediation efforts.

Sample Preparation

Researchers from the Technical University of Crete in Crete, Greece optimized a method for
solvent microextraction to the analysis of nitroaromatic explosives in water samples. Extraction
of 11 nitroaromatic compounds was achieved by suspending a 1 l drop of organic solvent into
a stirred sample. The organic sample was then analyzed by GC/MS.

Toluene was found to be the most successful solvent. Detection limits for a 15 minute exposure
were ~ 0.1 – 1.0 g/L. The technique proved to be a fast, simple and inexpensive tool for
preconcentration and matrix isolation of nitroaromatics on a microscale.[10] The same
researchers compared this single drop technique to solid-phase microextraction (SPME). While
the single-drop method was less expensive, it was also less sensitive and precise than SPME.[11]
Researchers from the Institute de Recherche Criminelle de la Genarmerie Nationale in France
reported on the exaction of high explosives from aqueous samples by SPME using GC/ECD.
The use of SPME eliminated most interfering compounds, making the identification easier.
SPME also provided a low detection limit. Direct injection of the SPME fiber on column
decreased degradations of the most sensitive molecules.[12] In the United States, researchers at
the University of Ohio studied using solid phase extraction (SPE) to extract trace amounts of
explosives from water followed by analysis using ion mobility spectrometry. Detection limits
for TNT, RDX, and HMX were at the part-per-trillion level.[13] Finally, researchers in South
Australia reported on ammonium nitrate and methyl-ammonium nitrate derivitized with
alkylchloroformates either in situ or on-fiber using SPME, and then analyzed using GC/MS.[14]
Researchers from Stockholm University in Stockholm, Sweden presented an analytical method
for determining nitroaromatic explosives in vapor phases. The samples were collected by
pumping air through glass fiber filters and polyurethane foam adsorbents, and extracted on-line
by supercritical fluid extraction prior to analysis by high performance liquid chromatography.
The fully automated system separates most nitroaromatic esters in 30 minutes. The method
shows promise for assessing whether areas are mined in landmine-clearing operations.[15] These
same researchers recently reported using solid-phase extraction cartridges to collect the analytes,
followed by a modified supercritical fluid extraction, followed by analysis using large-volume
injection gas chromatography with nitrogen/phosphorus detection. They applied the technique to
characterize the headspace composition above military grade trinotritoluene (TNT). Results
confirm that 2.4-dintrotoluene DNT) and 1.3-dintirbenzene (DNB) constitute the largest vapor
flux, but TNT, 2,6-DNT, and trinitrobenzene were also consistently detected in all the
samples.[16]

333
Analysis of Explosives

Research on the use of capillary electrophoresis in the detection of monomethylamine and

benzoate ions in post-blast residues was reported by the Bureau of Alcohol, Tobacco and
Firearms (ATF) laboratory in Rockville, Maryland. Monomethylamine is found in Tovex®, a
water gel explosive. Sodium benzoate is added to Pyrodex® as a fuel and burn rate
modifier.[17] Detection limits were about 1 ppm. A cyclodextrin-assisted capillary
electrophoresis (CD-EKC) method for the determination of cyclic nitramine explosives was
developed by researchers at the Biotechnology Research Institute, part of the National Research
Council Canada in Montreal, Quebec, Canada. The method was compared to analysis by high-
performance liquid chromatography (HPLC). The method was able to rapidly resolve and detect
2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaaza-isowurtzitane (CL-20), octahydor-1,3,5,7-
tetranitro-1,3,5,7 tetrazocine (HMX) and hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) and their
related degradation intermediates in environmental samples. The researchers concluded that
HPLC was more sensitive than CD-EKC, but the CD-EKC, being the faster of the two, facilitates
the real-time monitoring of experiments. They concluded that HPLC and CD-EKC are
complimentary to each other in the determination of cyclic nitramines and their degradation
products in environmental samples.[18] The stable isotope ratio for 37Cl was used to differentiate
chlorate and perchlorate samples from different sources by researchers at the University of
Reading in the United Kingdom. In addition, the manufacturing process was identified as a
fractionation event based on comparison of the isotope ratios for feedstock chlorine and the final
products.[19] Researchers from both the United States and United Kingdom reported on using
scanning electron microscopy and energy dispersive spectroscopy (SEM/EDS) to characterize
pyrotechnic residues. Common elements found were sodium, magnesium, aluminum, sulfur,
chlorine, potassium, copper, strontium, and barium.[20,21,22] Researchers at the National
Center for Forensic Science in Orlando, Florida developed a searchable library of oxidizers by
analyzing concentrated solution (1 mM) by direct introduction into the electrospray mass
spectrometer. Post-blast samples were analyzed and successfully matched to the library.[23]
Finally, ATF reported on the development of a method to identify ascorbic acid and its
degradations products in Black Powder substitutes. Samples were derivitized using a mixture of
acetonitrile and bis(trimethylsilyl)acetamide and analyzed by GC/MS.[24]

Use of peroxide based explosives by terrorist’s sparked interest in developing methods for their
identification. Researchers in the United Kingdom and Switzerland reported on the development
of LC/MS methods for both TATP and HMTD.[25,26] Researchers from the Netherlands and
Germany reported on a method using HPLC/diode array and fluorescence detectors to identify
TATP and HMTD.[27] McKay from the Dstl laboratory in the United Kingdom reported on their
laboratories extensive research to develop reliable chemical, explosive, and analytical data on
organic peroxide explosive. A systematic study was conducted on the physical and chemical
properties of these explosives along with methods for qualitative analysis and detection.
Analytical techniques including FTIR, TLC, GC/MS and LC/MS can be used for forensic
analysis and identification. They have also developed a low-hazard TATP training aid for the
United Kingdom Police explosive search dogs.[28] Researchers from Israel studied the effect of
water on the recovery of high explosives. The most retentive surfaces were glass, plastic and
aluminum. The most persistent explosives were PETN>Semite>RDS>TNT. RDX was found to
survive in ocean water for only minutes to hours. The upper limit for recovery was 1-2
weeks.[29] Capillary electrophoresis was also used to detect high explosives by researchers in
Australia. The Australians used artificial neural networks to optimize the separation of high
explosives. Almost full resolution of the EPA 8330 mixtures was obtained in less than 10
minutes.[30] Hopen reported on the contribution of Dr. Walter McCrone in using polarizing light
microscopy to characterize and identify explosives such as RDX and HMX.[31] Researchers

334
from the Peoples Republic of China published a paper outlining methods for the search and
identification of explosives, including new techniques and methods.[32]

Researchers a the Central Forensic Science Laboratory in Ramanthapur, Hyderbad, India studied
the thermal behavior of low explosives compositions containing potassium nitrate mixed with
ammonium chloride using Differential Scanning Calorimetry (DSC). The results provide
information about the ion exchange reaction between these two chemical substances and the
temperature region at which the formation of a cloud of salt particles of potassium chloride takes
place. The addition of ammonium chloride quenches the flame of deflagrating compositions and
causes the mixture to undergo explosive decomposition at relatively low temperatures.[33]

Because of its popularity as a filler for pipe bombs in the United States, the characterization and
identification of smokeless powder propellants generated a good deal of research in the United
States. Researchers at Ohio University, Athens, Ohio reported on an HPLC procedure for
smokeless powder comparisons.[34] They also reported on updating the HPLC method to
include ESI-MS detection in the positive ion mode. The method allowed for identification of
organic additives in various commercial powder samples and differentiation of intact
samples.[35] Researchers at the US National Institute of Standards and Technology in
Gaithersburg, Maryland published a series of papers looking at organic additives in smokeless
powders. The methods explored the possibility of using the organic additives to determine
handgun use, and possible association of known and unknown powders. The possibility of a
previously fired ammunition type contaminating the organic gun shot residue from subsequent
ammunition types was investigated. Only a trace of the stabilizer from an initial load of
ammunition was detected in the first shot of the second ammunition type. In addition, the type
of primer used (leaded vs. lead-free) did not affect the composition of the organic residue.[36] A
method to quantitatively extract and determine NG, DPA, and EC was developed. The method
used ultrasonic extraction in 1:3 2-butanol:methanol at room temperature followed by micellar
capillary electrophoresis.[37] The propellant (nitrocellulose and nitroglycerine) to stabilizer
(diphenylamine + ethyl centralite) ratio (P/S) was calculated for various intact smokeless
powders and their associated gun shot residues. Four of 7 ammunition types could be
differentiated based on this analysis, with all 7 differentiated when morphology was considered.
Using the P/S ratio to link unfired powder to their residues was successful in some cases.[38]
Qualitative identifications of smokeless powder components were compared from 19
laboratories. Identification of NG and major stabilizers posed no difficulty. Identification of
minor stabilizers and their degradation products was more problematic.[39] Quantitative
analyses of smokeless powder components were compared from 5 laboratories. The
determination of NG was the most susceptible to method bias. Furthermore, within-lab
uncertainty was 1 – 5%, while between lab uncertainty was 5 – 10%.[40]Work on using vacuum
collection of gunpowder (propellant) residues from clothing worn by shooting suspects was
reported by researchers from the Division of Identification and Forensic Science in Jerusalem,
Israel. The vacuum collected samples were analyzed by gas chromatography/thermal energy
analyzer (GC/TEA), ion mobility spectrometry (IMS), and gas chromatography/mass
spectrometry (GC/MS). The residues were collected on fiberglass and Teflon filters using the
portable vacuum supplies with the IMS. The filters were extracted with solvent, centrifuged, and
analyzed without any further sample clean-up. Based on the results of the study, an operational
method was introduced into casework without changing the current method of looking for
gunshot residue (GSR) first using double-sided adhesive tape, followed by vacuuming for
gunpowder residues. Both the GC/TEA and IMS provided sufficient sensitivity to detect and
identify gunpowder residues in real life samples.[41]

The use of ion mobility spectrometers (IMS) to screen air passengers sparked interest in this
technology. Workers in the United States reported two reviews on the use of ion mobility

335
spectrometry. Researchers at Idaho National Engineering and Environmental Laboratory in
Idaho and the Department of Chemistry and Biochemistry at New Mexico State University in
New Mexico summarized instrumental developments as well as IMS date for various high
explosives and taggants. They concluded that better knowledge of the complex gas phase ion-
molecule chemistry has resulted in better performance of the equipment. Sampling methodology
has become the main weakness in applications.[42] Researchers at Weber State University and
Brigham Young University in Utah provided an overview of IMS and it’s coupling with various
mass spectrometers. Among the applications discussed is the analysis of explosives.[43] A way
to resolve interferences in negative mode ion mobility spectrometry using selective reactant ion
chemistry was reported by researchers at Idaho National Engineering and Environmental
Laboratory, Idaho Falls, Idaho, USA, and the Department of Chemistry at Montana State
University in Bozeman, Montana, USA.[44] These researchers found that 2,4-
dichlorophenoxyacetic acid and 2,4-dichlorophenol had IMS responses which overlapped those
of 2,4,6-trinitrtoluene degradation products. The Cl- reaction ion chemistry, often used for
explosives analysis, was not always successful in resolving peak overlap of analytes and
interferents. The desired resolution of the analytes and interferences can sometimes be achieved
using only air for the formation of reactant ion, or at other times through the use of Br- as an
alternative to Cl- for producing reactant ions. Adduct stability could also be achieved by
lowering the IMS temperature.

Researchers at the University of Twente in the Netherlands reported on the “lab-on-a-chip”

technology. They cite this could be used for identification of explosives, along with a list of
other possible uses.[45]

The use of mass spectrometry, especially coupled with a chromatographic separation technique,
continues to be an area of methods development for explosives. Professor Yinon provided a
review of the forensic analysis of explosives by LC/MS. The article contains a review of the
instrumentation for LC/MS interfaces and ionization techniques. LC/MS with negative ion ESI
was found to be the most successful in the analysis of high explosives with detection limits in the
picogram range.[46] Researchers at the National Center for Forensic Science in Orlando,
Florida, USA published 5 papers on the use of chromatography and mass spectrometry in
studying explosives. Zhao and Yinon used LC/MS with atmospheric pressure chemical
ionization to study the by-products of industrial 2,4,6-trintirotoluene (TNT) in order to build a
profile for the characterization of TNT samples from various origins. By looking at the isomers
of trinitrotoluene, dinitrotoluene, trinitrobenzene and dinitrobenzene, which are by-products
originating from the manufacturing process of TNT, their combined profile is different for
samples from different manufacturing plants.[47] These same researchers evaluated methods for
the identification of nitrate ester explosives by liquid chromatography-electrospray ionizations
(ESI) and atmospheric pressure chemical ionization (APCI) mass spectrometry in the negative
ion mode.[48] They found that with post-column introduction of various additives, both LC-ESI-
MS and LC-APCI-MS demonstrated high specificity and sensitivity in the identification of
pentaerythritol tetranitrate (PETN), nitroglycerin (NG), and ethylene glycol dinitrate (EGDN),
and other nitrate esters though adduct ion formation. Identification of EGDN in LC-MS was not
possible without an additive. ESI was found to be more sensitive than APCI. The analysis of
three explosive samples of forensic interest, Booster DYNO, Semtex, and smokeless powder,
demonstrated the effectiveness of using post-column additives in the detection of nitrate ester
explosives. Zhao and Yinon looked at the identification of explosive oxidzers by electrospray
ionization mass spectrometry.[49] It was found that a series of cluster ions were predominant in
both positive- and negative-ion mode, allowing for the characterization of the investigated
oxidizers. The identity of the recorded cluster ions was further confirmed using some
isotopically labeled compounds and tandem mass spectrometry with collision-induced
dissociation. Three commercially available samples were analyzed. They were Powermite, a

336
commercially available slurry explosive, black powder, and “match heads”, a filler sometimes
found in pipe bombs. For qualitative purposes, ESI-MS is well suited for the characterization of
the major inorganic oxidizers in explosives and can be used as a complimentary method to ion
chromatography. The validity of this technique still needs to be investigated for the quantitative
analysis of trace inorganic explosive residues. Gapeev, Sigman, and Yinon reported on the
liquid chromatography/mass spectrometry of 1,3,5-trinitro-1,3,5-trazacyclohexane (RDX) by the
attachment of an anion to the analyte molecule as a way of producing characteristic ions under
ESI and APCI conditions.[50] They concluded this is a powerful technique for the analysis of
trace levels of RDX. Finally, Gapeev and Yinon demonstrated that electrospray mass
spectrometry, when used with spectral libraries, is a useful method for the rapid identification of
inorganic oxidizers commonly present in commercial and improved explosives.[51] ESI-MS of
oxidizers reveal a series of characteristic cluster ions. Such a set of cluster ions can be regarded
as a “fingerprint” of a particular oxidizer. With the aid of a spectral library, tentative
identification of an oxidizer becomes automated and easy to implement. Because it is not
necessary to separate the components before analysis, results become available in real time.
Little sample consumption and the ease of sample preparation are also advantages. Researchers
in Japan reported on developing a new detection system to detect military explosives.[52] The
system is based on a novel ion source for APCI. The direction of the sample gas flow introduced
into the ion source is opposite to that of the ion flow produced by the ion source. They call this
technique “counter-flow introduction: (CFI). The CFI ion source has high ionization efficiency
for nitro-compounds and is installed in an ion-trap mass spectrometer. Tests on various military
explosives show that the system is suitable for practical on-line explosive detection within a few
seconds without any pretreatment of the sample gases. Researchers at the Ion Cyclotron
Resonance Program at Florida State University in Tallahassee, Florida, USA reported on the
identification of explosives by Electrospray Ionization Fourier Transform Ion Cyclotorn
Resonance (ESI FTICR) Mass Spectrometry.[53] They demonstrated the potential of ESI
combined with FTCIR mass analysis for discrimination and possible identification of military
explosives. The unique value of high resolution mass analysis is that it can identify elemental
compositions of both active and nonactive ingredients of the explosives. For example, they were
able to correct prior misassignments of the most abundant negative ion species in RDX and
HMX. Characteristic ingredients can be detected from postblast explosive residues of each
explosive. Future work will focus on analysis of the sample explosive product from different
manufacturers to see whether the origin of an explosive can be determined by mass analysis.
Researchers from the State University of Campinas in Brazil and Purdue University in the
United States reported on using gas-phase reactions to improve the selective detection of TNT
and RDX. They found that using ethylvinyl ether in both electron and chemical ionization
modes yielded highly characteristic fragment ions.[54]

Post-blast signatures and Effects

Researchers at the University of Rhode Island in the United States reported on the correlation
between the small-scale explosivity device (SSED) and actual pipe bombs was evaluated. The
relative order of explosivity matched the fragmentation seen in the pipe bombs. Generally, the
restricted volume of the SSED increased the amount if intact explosive that was found in post-
blast chemical analysis.[55] These same researchers collaborated with scientists at the ATF
laboratory in Maryland to conduct a study on 56 pipe bombs. For identical devices, the overall
fragmentation pattern was surprisingly reproducible. The study demonstrated the possibility
that, even in circumstances where chemical residue cannot be found, sufficient evidence is
present in the pipe fragments to identify the nature of the energetic filler.[56] Researchers at the
New Mexico Institute of Mining and Technology in New Mexico determined that changes in the
microstructure, hardness and martensite content (in stainless steel) of metal pipe filled with high

337
and low explosives was studied post-blast. Microstructure damage, hardness and martensite
content all scaled with detonation velocity.[57]

Contamination/Explosives Background

Researchers from the United Kingdom reported on a background survey of inorganic ions and
sugars since they play an important role in the forensic investigation of an explosives related
incident. They found that sodium calcium chloride, sulfate, nitrate, and phosphate were the most
common and abundant. Chlorate was found at a low level in some external samplers.
Perchlorate and thiocyanide were not found. Ammonium was found in wall samples while
sugars were found in interior residential areas.[58] Workers from the United Kingdom and the
United States collaborated to study the recovery of explosives from hair. A method using
acetonitrile extraction followed by GC/ECD and GC/TEA was used to detect explosives in
persons exposed to the vapors of TNT, PETN, and RDX in an occupational setting. As little as
one hour was required to obtain detectable levels of explosive.[59] Researchers at the University
of Rhode Island in the United States reported on the potential for high explosives to contaminate
the laboratory environment after handling explosives. A few percent remained on surfaces from
original quantities (mg), < 0.1% was secondarily transferred, outside surfaces of improvised
explosive devices were estimated to contain ~0.01% of the total explosive weight.[60]
Researchers from the Defence Evaluation and Research Agency, Kent, United Kingdom,
reported on an environmental survey relating to improvised and emulsion/gel explosives.[61]
Since the detection and identification of traces of inorganic ions and sugars can play a major role
in the forensic investigations of explosives incidents, the survey investigated the background
levels of these substances in the general environment, both urban and rural, and in summer and
winter. Swabbings were extracted with water and analyzed for a range of inorganic ions and
sugars using ion chromatography. Most of the target anions were found to be common to all
locations, with chloride, sulphate, nitrate and phosphate being the most common and abundant.
Perchlorate and thiocyanate were not detected in any samples. Sodium and calcium were
detected in most samples, and potassium and magnesium in approximately half of the samples.
Ammonium was less common but detected in significant levels in wall samples. Glucose,
fructose, and sucrose were detected in the vacuum samples from the interior surfaces of houses,
hotels, and cars.

A study on the burning rates and ballistics of Low Vulnerable Ammunition (LOVA), propellants
used in military applications, containing fine RDX particles was conducted to determine the
particle size that would give the most stability to the propellants.[62] This was prompted by the
possibility of accidental explosions of these propellants in armored vehicles and reports that
RDX exhibits an unconventional burning behavior depending on the particle size of RDX in the
propellant. The evaluation was carried out by static firing using a closed vessel. The results
revealed that fine RDX of 4.5 to 6µm size may be the most suitable for LOVA gun propellant to
meet desired burning rates for satisfactory ballistics.

In 2001, researchers at the Forensic Explosive Laboratory of the Defence Evaluation and
Research Agency in Kent, United Kingdom, reported on a system of contamination prevention
procedures used to prevent contamination of standards and samples.[63] The system was
progressively improved over an 8-year period. Monitor samples taken weekly from surfaces
within the laboratory have, with few exceptions, revealed only low levels of contamination,
predominantly RDX. Analysis of 401 control swabs, processed alongside the monitor swabs,
has demonstrated that in this environment the risk of forensic sample contamination is extremely
small. The regime has also been valuable in a process of continuous improvement, allowing
sources of contamination transfer into the laboratory to be identified and eliminated.

338
In 2001, researchers at the Beijing Institute of Technology in Beijing, Peoples Republic of
China, reported on using raw TNT to make an industrial explosive using a new method of
manufacture. The detonation velocity was measured, and it was determined that the raw TNT
could be used to make a reliable explosive.[64]

Environmental Analysis

A group of researchers in Canada developed a method for detection of explosives and their
degradation products in soil environments.[65] The workers developed methods using
supercritical fluid extraction, solid-phase microextraction, and acetonitrile to extract explosives
and their degradation productions from water, soil, and plant tissue sample for analysis by
HPLC-UV, CE-UV, or GC-MS. Their extensive e study demonstrates that former explosives
manufacturing and training sites can have significant amounts of explosives. The detection of
explosives in different natural soil environments, including surface and subsurface soil,
groundwater and plant tissues, showed contamination by explosives is widespread and can reach
the water table and also accumulate in plants. Researchers from Ohio University in Athens,
Ohio, USA reported on using solid phase microextraction to concentrate explosives from water,
and subsequently analyze the samples with a commercially available ion mobility
spectrometer.[66] They found concentrations as low as one part per trillion could be detected.
Walsh from the US Army Cold Regions Research and Engineering Laboratory in Hanover, New
Hampshire, USA reported on the analyzing soils for nitroaromatic, nitramine, and nitrates ester
explosives in soil using gas chromatography and an electron capture detector.[67] Researchers
from the University of Rhode Island, USA, studied whether they could differentiate TNT from
land mine leakage and TNT from a post-blast detonation. Identification of microbial degradation
products of TNT, mainly 2-aminoninitrotoluene and 4-aminodinitrotoluene, can help
differentiate the source.[68] A study on the detection and decontamination of residual energetics
from ordnance and explosives scrap was conducted by researchers at the University of Idaho,
Idaho, USA.[69] Decommissioning and cleanup of these materials has also led to concerns
about the explosive hazards associated with residual energetics still present on the surfaces of
ordnance and explosives scrap. Typically, open burning or detonation is used to decontaminate
ordinance or explosive scrap. A method was developed to decontaminate these materials using a
bioslurry of anaerobic microbes. A portable ion mobility spectrometer was used for the
detection of residual explosive residues. The mixed microbial populations effectively
decontaminated both the scrap and the mortar round. Use of the IMS was a sensitive field
screening method that can be used by personnel with minimal training.

Unpublished/Internal Communications

Dr. Chris Lennard from the Forensic & Technical Services of the Australian Federal Police
reports that they purchased a GC-IRMS and CE-MS between February 2003 and February 2004.
Two members of the staff are undertaking part-time Ph.D. projects to develop procedures for the
application of these technologies in analyzing explosives residues. Other research completed
from 2002 to 2004 included an in-house validation/limits of detection studies on our equipment
and the development of CE protocols for residue analysis. These results were published in the
open literature.[70] Wendy Norman from the Royal Canadian Mounted Police, Forensic
Laboratory Services – Ottawa, Canada reports that their laboratory has been doing research that
has not been published on the “best swab” from all the instrumental backgrounds’ point of view,
milk and chlorine bottle bombs, TATP detection and characterization, and the characterization of
components of Pyrodex and Triple Seven by LC/MS.[71] Dr. Frantisek Zreck from the
Department of Chemistry of the Institute of Criminalistics in Prague, the Czech Republic, reports
they are development instrumental methods and ways of sample preparation for peroxide
explosives including TATP and HMTD. They also did research on the laboratory collection of

339
particle material from pieces of evidence for further examination on explosives trace. This work
was presented as a poster at the International Seminar on the Recovery of Forensic Explosives
Evidence organized by Dstl in 2003.[72]

Sean Doyle, the Head of Chemistry and Research at Dstl, Fort Halstead, Kent, United Kingdom
reported on both published and unpublished in the open literature (but published in internal
documents) on a wide variety of research done by their laboratory in the area of explosive
analysis over the last 3 years.[73] A complete listing of the internal Dstl reports is listed in
Appendix E.

DETECTION OF EXPLOSIVES

There is a great deal of interest and emphasis on developing technologies to find explosives, both
in trace amounts and bulk explosives, to prevent a terrorist attack. Finding traces of explosives
on a person or piece of their personal property may identify someone who has engaged in
making improvised explosive devices. The detection of bulk amounts of explosives is intended
to identify large amounts of explosives that may be hidden in luggage or large containers in
vehicles or ships. In addition, detection of explosives to find landmines and contaminated soil is
also an area of interest. A review of the literature on detection of explosives revealed several
conferences held periodically that may be of interest to those in the field of explosives.
Proceedings are published from the International Autumn Seminar on Propellants, Explosives
and Pyrotechnics that are held in the Peoples Republic of China in October of every other year
on odd numbered years. Proceedings of SPIE – The International Society for Optical
Engineering (Sensors and Command, Control, Communications and Intelligence) also contain
information on detection technologies. Proceedings from the American Institute of Physics
meetings contain information on detection technology using gamma resonance technology.

The types of technologies being used to develop explosive detectors include neutron, gamma
ray, radiation beam, sensors such microcantilevers with polymer films or immune sensors, ion
non-linear drift spectrometry, ion mobility spectrometry, quantum cascade transmitters,
chemiluminescence, microchip capillary electrophoresis, and microthermal analysis. The types
of targets of interest include finding landmines, soil remediation, looking for bulk explosives in
vehicles, large containers, vessels, and luggage, and trace amounts on individuals, including the
development of portal technologies. Research of particular interest is summarized below.
Citations for the rest of the research reported in this area are listed in Appendix D.

Several review papers were published on the topic of the detection of explosives. A review of
field detection and monitoring of explosives using mobile and hand-held detectors covered the
three classes of detectors: vapor and particle detectors; radiation detectors; and, biochemical
detectors.[74] The detection of explosives in situ is of importance in several applications:
finding hidden explosives in airport luggage and in the mail; screening of personnel for
concealed explosives; environmental monitoring of explosives contaminated sites; and the
detection of buried landmines. The principles of operation of the main detectors in use are based
on ionization and separation analysis of explosive vapors, pyrolysis and gas-phase reactions,
bulk detection by means of a reaction of an incident radiation with an element or elements of the
explosive compound, and detection of a product of a biochemical reaction with the explosive.
Another article covers the different types of detection technologies used in hand-held and mobile
devices, comparing them to “electronic noses”.[75] In 2001, researchers reported on the
scientific foundation and efficacy of suing canines for the detection of explosives, and compared
them to the advantages and disadvantages of electronic devices.[76] The study concluded that
overall, detector dogs still represent the fastest, most versatile, reliable real-time explosive
detection device available. While instrumental methods continue to improve, they generally

340
suffer from a lack of efficient sampling systems, selectivity problems in the presence of
interfering odor chemicals and limited mobility tracking ability. A second study published in
2003 compared the use of biological detectors (canines) and instrumental methods for the rapid
detection of ignitable liquid residues and high explosives.[77] Headspace solid phase
microextraction (SPME) was used as a sampling method, followed by ion trap mobility
spectrometry (IMS) for the identification of high explosives. The study focused on identifying
the volatile odor chemicals detected by canines so they could be used for instrumental detection
of explosives. Additional studies will focus on optimizing the SPME/IMS interface. In 2001,
Proceedings the Autumn Seminar on Propellants, Explosives and Pyrotechnics in Shaoxing,
China include a review article from the Bejing People’s Police College on the use of detectors to
find explosives.[78] The Institute of High Energy Physics in Beijing, Peoples Republic of China,
reported on a review of systems used to detect narcotics and explosives.[79]

One study reported looking at sampling from the human body for trace amounts of explosives
based on collecting particulates based on the thermal behavior of air surrounding the body.[80]
Experiments were conducted in a dispersal chamber to identify variables affecting the
detectibility of concealed RDX and TNT patches. Movement by human volunteers enhanced the
available explosive trace signal, while clothing blocked some of the movement generated signal.
The signals varied significantly from volunteer to volunteer. The information is being used to
design a practical, non-intrusive trace detection portal for aviation security screening and related
applications. Another portal was reported using an airline passenger personnel portal coupled to
a high-flow, high-resolution ion mobility spectrometer (IMS).[81] The modifications to the
traditional IMS enhanced both detectability and resolving power.

Patents

Six patent applications were filed with the United States Patent Office and 2 with the Russian
patent office for devices for detecting explosives. Two of the patents filed in the United States
deal with the use of thermal analysis, and include the ability to also detect other controlled
substances.[82,83] One patent uses chemiluminescence for the detection of explosives, narcotics,
and other chemical substances.[84] A detection system using an array of molecularly imprinted
polymer coated, bifurcated fiber optic cables is described in another patent.[85] Another patent
describes a sampling device with a test strip inserted into air aspirated from luggage interiors for
the detection of concealed explosives.[85] The last patent filed in the United States describes an
explosive detection system.[87] One of the patents filed in Russia uses nuclear quadrupole
resonance technology for the detection of both explosives and narcotics.[88] The second Russian
patent deals with a device that used emitting pulse neutron flow to detect explosives and
fissionable material, and is designed to be used for screening at airports and custom control
checkpoints.[89]

SUMMARY

The illegal use of explosives has generated much interest in developing new detection
technologies. Technology is moving towards more sensitive, reliable, inexpensive, and smaller
detection devices that can be more widely deployed in an effort to protect the public. Detection
remains a focus for the location of landmines and remediation of soil. Tracing explosives has
sparked interest in the use of stable isotope ratio analysis to see if samples of explosives can be
linked or to determine if it is possible to find an area of origin. In the laboratory analysis of
explosives, interest in the United States focuses more on low explosives, the filler of choice in
the most common type of explosives devices seen there, pipe bombs. The characterization and
analysis of peroxide based explosives is gaining attention as their more widespread use
increases.

341
Acknowledgements

I would like to acknowledge the assistance of Adiva Sotzky, librarian, for collecting references
over the past 3 years. I also want to acknowledge Dr. John Goodpaster of the ATF Forensic
Science Laboratory - Washington for his assistance in preparing this paper and reviewing the
literature, along with the help of Dr. Sam Howerton of the National Institute of Standards and
Technology. Finally, I wish to acknowledge the input provided by Chris Lennard with the
Chemical Criminalistics group of the Australian Federal Police, Wendy Norman from the Royal
Canadian Police Forensic Laboratory Services, Canada, Frantisek Zrcek from the Department of
Chemistry Institute of Criminalistics in Prague, the Czech Republic, and Sean Doyle, Head of
Chemistry and Research for The Forensic Explosives Laboratory, Dstl, United Kingdom.

342
 APPENDIX A

Papers from the Proceedings of the 7th International Symposium on the Analysis and
Detection of Explosives
June 25-28, 2001
Edinburgh, Scotland

DETECTION METHODOLOGY AND REPORTS

Warren R, Leggett J, Jupp I, Dermody, G. A CZT Detector Solution for the Detection of
Explosives in Baggage, using Anular Dispersive X-ray Diffraction. DERA, Fort Halstead,
Sevenoaks, Kent, UK.

Hanold KA Mass Spectrometry Based Personnel Screening Portal. Syagen Technology, Inc.
Tustin, CA

Annis M, Adler R. Tomography based on Nested High Voltage Generator. Annis Tech and
North Star Copration, respectively, USA.

Lareau RT, Chamberlain, RT, Hallowell, SF. MEMS/Nanotechnology based Trace Explsoives
Detection – is smaller better? US Federal Aviation Administration, Atlantic City International
Airport, NJ, USA.

Tarver EE, Jennings, RT, Stamps, JF. Improved Resolution for Explosives Dtection Using
External Second Gate Fouier Transform Ion Mobility Spectrometry. Sandia National
Laboratoryies, Livermore, CA, USA.

Fricano L, May L, Kuja F, Goledzinowski M, Nacson S. Walk-Through Portal for Trace

Detection of Explosives Vapors and Particles. Barringer Research Limited, Mississauga,
Ontario, Canada.

Fultz, ML, Albirght, WH Jr., Deel, LA, McCune LJ, Shater, DS, Strobel, RA. ATF Explosives
Detection Research and Development Efforts. Bureau of Alcohol, Tobacco and Firearms,
Washington, DC, USA.

Fisher, M, Cumming C. Detection of Trace Concentrations of Vapor Phase Nitroaromatic

Exploisves by Fluroescence Quenching of Novel Polymer Materials. Nomadics, Inc.,
Stillwaters, OK, USA.

TAGGING AND VAPOUR DETECTION

Lightfoot, PD, Fouchard RC, Jones DE. Marking of C-4 with Microencapsulated DMNB.
Canadian Explosives Research Laboratory, Ottawa, Ontario, Canada.

Chen T. Universal Interfaces for Sampling DMNB Vapors from Inside Luggage. U.S. Army
Tank-Automotive Commands Armaments Research Development and Engineering Command,
Picatinny Arsenal, NJ, USA.

343
ANALYSIS OF POST DETONATION SAMPLES

Waekfield JL.Analysis of Deglagraitng Explosive Residues. Forensic Explosive Laboratory,

DERA, Fort Halstead, Sevenoaks, Kent, UK.

Kuja F, Grigoriev A, Loveless A, Jackson R, James R, Nacson S. Applications of GC-

IONSCAN M400B for the Determination and Identification of Explosives in Post-Blast
Samples. Barringer Research Limited, Mississauga, Ontario, Canada.

Yeager K. Analysis of Post-Blast Residue from a Variety of Ammonium Nitrate Based

Improvised Explosives. FBI Explosives Unit, Washington, DC, USA.

Strobel R1, Noll 1, Kury J2. Nitromethane K-9 Dtection Limit. Bureau of Alcohol, Tobacco and
Firearms, Washington, DC, USA1, and Lawrence Livermore National Laboratory, Livermore,
CA, USA2.

Wakelin DH. Isotope Ration Analysis of Explosives – a New Type of Evidence. Forensic
Explosives Laboratory, DERA, Fort Halstead, Sevenoaks, Kent, UK.

Stancl M. Direct and Indirect Explosive Contamination of Surfaces. Research Institute of

Industrial Chemistry, Czech Republic.

Kuja F, Grigoriev A, Debono R, Nacson, S. Ion Mobility Spectrometry in the Detection of

Improvised Explosives. Barringer Research, Mississauga, Ontario, Canada.

Tamiri T, Abramovich-Bar S, Sonenfeld D, Glattstein B, Ashdat L. Division of Identification

and Forensic Science, Israel Police Headquarters, Jerusalem, Israel.

STUDIES OF ENVIRONMENTAL CONTAMINATION

Mount KH, Miller, ML. A Field Survey of Explosive Residue in the Environmnet: Part I-
Inorganic Analysis, Part II – Organic Analysis. FBI Laboratory, Washington, DC, USA.

Preis A1, Astratov M1, Levsen K1, Godejohann M2, Spraul M2, Neidig KP2. Application of the
NMR, LC/NMR and LC/NMR/MS Methods to the Analysis of Environmental Samples from
Ammunition Hazardous Waste Sites. 1Fraunhofer Institute fur Toxikologie un Aerosolforshung,
Pharmaforschun und Klinische Inhalation, Hannover, Germany, 2Bruker Analytick, Rheinstetten,
Germany.

Cummings A1, Volk F2, Mostak P3. Influence of Sampling Methology and Natural Attenuation
on Analysis of Explisves Content in Contaminated Sites. 1DERA, Forthalstead, UK, 2FICT,
Berghausen, Germany, 3ALIACEM, Pardubice Semtin, Czech Republic.

ANALTYICAL STUDIES – MASS SPECTROMETRY

Yinon J, Zhao X. Characterization and Origin Identification of Explosives by LC/MS. National

Center for Forensic Science, Orlando, FL, USA.

McGann WJ, Goedecke K, Becotte-Haigh P, Neves J, Jenkins, A. Simultaneous, Dual Mode

IMS Detection System for Contrabanc Detection and Identification. Ion Track Instruments,
Wilmington, MA, USA.

344
Dreifuss PA, Klonta, KM. Advances in Atmospheric Pressure Ionizaton (API) LC/MS and
GC/MS Methods for the Analysis and Detection of Explosives. Bureau of Alcohol, Tobacco and
Firearms, Rockville, MD, USA.

Takada Y, Kojima K, Suga M, Hashimoto Y, Yamada M, Sakairi M, Kakamura J1. Dectection

of Explosives by Atmospheric-pressure Chemical Ionization Ion-trap Mass Spectrometry with
‘Counter Flow Introduction’. Hitachi, Ltd, Tokyo, Japan, 1National Research Institute of Police
Science, Kashiwa Chiba, Japan.

Bender EC, Ferguson, M. The Analysis of Charcoal Extractables in Black Powder by GC/MS.
Bureau of Alcohol, Tobacco and Firearms Laboratory, Rockville, MD, USA, and Michigan State
University, East Lansing, Michigan, USA, respectively.

THERMAL AND OTHER ANALTYCIAL METHODS

Chen CC1, Bannister WW1, Furry J2, Slough G3. Micro-Fabrication Thermal Analysis Devices
1
for Detection of Energetic Materials. Department of Chemistry, University of
Massacheusettts/Lowell, Lowell, MA, USA, 2ProTechScientific, Kissimmee, FL, USA, 3TA
Instruments, Inc., New Castle, DE, USA.

Klapec D, Ferguson M. A Preliminary Study into the Feasiblity of Using Capillary

Electrophoresis (CE) in the Examination of Water Soluble Salts Found in Smokeless Powders.
Bureau of Alcohol, Tobacco and Firearms, Rockville, MD, USA.

Muller D., Abramovich-Bar S., Shelef R, Sonenfeld D, Levy A, Kimchi S., Tamiri T. Improved
Methods in the Post-Explosion Analysis of TATP. Division of Identification and Forensic
Science, Israel Police Headquarters, Jerusalem, Israel.

Bunte G. Heumann H, Krause H, Chromatographic Analysis of dintramide anions in the

presence of nitrate. Fraunhofer-Institute fűr Chemische Technologie, Pfinztal, Germany.

Kelly RL, Mothershead RF. Smokeless Powder Analysis: Interpretations and Complications
Part 1. FBI Laboratory, Washington, DC, USA.

Nakamura J, Arai H. The Analysis and Properties of New Type of Explosives in Japan.
National Research Institute of Police Science. Kashiwa, Chiba, Japan.

Heflinger D, Arusi-Parpar T, Lavi R. Remote detection of explosives by photodissociation

followed by laser-induced fluorescence. Non-Linear Optics Group, Soreq NRC, Yavne, Isarael.

Minet JJ, Vergnes F, Batonnier M. Trace Analysis of Explosives Using HPLC/TEA.

Département des Explosifs et des Incendies, Laboratoire Central de la Préfecture de Police,
Paris, France.

POSTERS

Minet JJ, Vergnes F, Batonnier M. Trace Analysis of Explosives Using HPLC/TEA.

Département des Explosifs et des Incendies, Laboratoire Central de la Préfecture de Police,
Paris, France.

Karelse JW, Jansen J, deBruyn PC. Detection equipment for high-explosives on the scene of
crime. Netherlands Forensic Institute, Rijswijk, The Netherlands.

345
Benson S, Royds D, Kwok B, Lennard C. Explsoive Residue Analysis within the Australian
Federal Police. Criminalistics Team, AFP Forensic Services, Australia.

Brandsma JE, de Bruyn PC. Cation chromatography of pyrotechnics. Netherlands Forensic

Institute, Rijswijk, The Netherlands.

Buechler S1, Barel S1, Nivon U1, Matsliah L1, Malotky L2, Shabray B3, Roth T3, Gal M3.
Explsoives Automated Sampling and Detection for Inspection of Bulk Cargo, Mail, Luggage.
1
RAY Dtection Technoloties, Holon, Israel, 2US-Federal Aviation Administration, Washington,
DC, USA, 3Israel Police, R&D Division and Bomb Disposal Division, Jerusalem, Israel.

Appendix B
rd
Proceedings of the 3 European Academy of Forensic Science Meeting
September 22-27, 2003
Istanbul, Turkey

Bagley J1, Brookes S1, Belanger C1, Coleman M2, Ader M2, Isaacs M2, Poswa A2, Beadah A3,
Doyle S3, Wakelin D3, Stroud M3. Stable Isotope Ration Analysis of Explsoives – A New Type
of Evidence. 1Iso-Analytical Ltd, Sandbach, Cheshire, United Kingdom, 2University of Reading,
Reading, United Kingdom, 3Dstl, Fort Halstead, Kent, United Kingdom.

Kronke K, Evaluation of Explosion Damages. Kiel, Germany.

Taubkin I. Classification of Substances and Materials by Explosive Properties. Importance for

Forensic Expertise Practice. Department of Fire and Explosion Investigations of Russian
Federation center of Forensic Expertise, Moscow, Russia.

Kartha KP, Babu ES, Karu S, Sharma DR. DSC Characterization of Explosive Compositions
Containing Various Types of TNT. Central Forensic Science Laboratory, Ramanthapur,
Hyderabad, India.

Kaushik, DK, At A, Sharma DR, Shukla SK. Two Dimensional Thin Layer Chromatography for
Identification of High Explosives. Central Forensic Science Laboratory, Ramanthapur,
Hyderabad, India.

Appendix C
Technical Working Group for Fire and Explosions
Sponsored by the National Center for Forensic Science
Orlando, Florida, USA
Annual Symposia

2002 Symposium, October 15-18, 2002

Cabral M. Overview of the History & Evolution of Terrorist Acts using Fire or Explosives as
Their Weapons. Los Angeles District Attorneys Office, Los Angeles, California, USA.
Seidel G. Incident Command System: The Roles of Investigators & Lab Personnel at the Scene.
Los Angeles City Fire Department, Los Angeles, California, USA.
346
Kelly R, Weiderhold R. Preparing to Collect & Preserve Evidence from Potential Terrorist
Incidents. FBI Laboratory Division, Washington, DC, USA.
Cooper B, May T. Bombing Case in Freemont California. Bureau of Alcohol, Tobacco and
Firearms, Forensic Science Laboratory – San Francisco, Walnut Creek, California, USA.
Bertoni J. How Can the Data I Collect be Used? Bureau of Alcohol, Tobacco and Firearms,
Arson and Explosives National Repository, Washington, DC, USA.
Rogers R. Forensic Applications of High Resolution FT-ICR Mass Spectrometry. National High
Magnetic Field Laboratory, Tallahassee, Florida, USA.
Jasper J. Forensic Application of Stable Isotopes. Molecular Isotope Technologies, Niantic,
Connecticut, USA.
Burmeister B. TWGFEX Explosives Protocols. FBI Laboratory Division, Washington, DC,
USA.
Madryzkowski D. Computational Fluid Dynamics of Fire Modeling. National Institute of
Standards and Technology, Gaithersburg, Maryland, USA.
Ehorn C. Chemical Warfare Agents by Chemical Ionization GC/MS. Varian, Inc., Palo Alto,
California, USA.
Sigman M. Thermal Desorption Sample Introduction for GC Analysis of Explosives. National
Center for Forensic Science, Orlando, Florida, USA.
Yinon J. Differentiation between nitroglycerine-based Medications and Explosives. National
Center for Forensic Science, Orlando, Florida, USA.
Lang T, Eynon T.A Case Review of Possible Fire Scene Contamination by Gasoline-Powered
Positive Pressure Ventilation Fans. The Centre of Forensic Sciences, University of Western
Australia, Crawley, Western Australia.
Evaluation of an Ignitable Liquid Mass Spectral Search System. State of Florida Fire Marshal
Office, Tallahassee, Florida, USA.

2003 Symposium, November 19-23, 2003.

Madryzkowski D. Fire Dynamics-How They Affect Investigations and Laboratory Analyses.
National Institute of Standards and Technology, Gaithersburg, Maryland, USA.
Mathias L. Polymers and Plastics Commonly Found in the Home. University of Southern
Mississippi, Hattiesburg, Mississippi, USA.
Chasteen, C. Collection, Preservation and Packaging of Fire Debris Evidence. State of Florida
Fire Marshal Office, Havana, Florida, USA.
Stauffer E. Interfering Products of Common Polymers Found in Fire Scenes. Applied Technical
Services, Inc., Marietta, Georgia, USA.
Doyle F. Collection, Preservation and Packaging of Evidence from Explosions. Frank Doyle &
Associates,
Lentini J.The View from the “Other Side”-Reviews of Cases with Serious Errors. Applied
Technical Services, Inc., Marietta, Georgia, USA.
Lennard C. World View – The Bali Bombing. Australian Federal Police, Canberra ACT,
Australia.
Cooper B1, Thurman T2., Crippin J3, McCardle R4. Explosives Devices Component Recognition
– Blurring the Line between the Scene and the Laboratory. 1Bureau of Alcohol, Tobacco,

347
Firearms and Explosives, Forensic Science Laboratory – San Francisco, Walnut Creek,
California, 2FBI Laboratory Division, Quantico, Virginia, 3 Western Forensic Law Enforcement
Training Center, Pueblo, Colorado.4State of Florida State Fire Marshal Office, Tallahassee,
Florida, USA.

Crippin J. Doing More than Hanging a Carbon Strip-Looking at the Evidence. Western Forensic
Law Enforcement Training Center, Pueblo, Colorado.
Chasteen, C. High Temperature Accelerants in Fires. State of Florida Fire Marshal Office,
Havana, Florida, USA.
Kennedy P. Investigating Dust Explosions. John A. Kennedy & Associates, Sarasota, Florida,
USA.
Dawn-Hewitt T. Technical Testimony by Laboratory Analysts. McKenna Hewitt, Denver,
Colorado, USA.
Hopkins R. NFPA 921-The Latest Revisions. Eastern Kentucky University, Richmond,
Kentucky, USA.
Kelleher J. Bomb Scene Investigations in Australia. Victoria Police Forensic Centre, Macleod,
Victoria, Australia.
Sigman M. Accelerants & Explosives Research at NCFS. National Center for Forensic Science,
Orlando, Florida, USA.
Oxley J, Shinde K. A New Source of Evidence: Explosive Traces in Hair. University of Rhode
Island, Kingston, Rhode Island, USA.
Broome S. Organic Peroxide Explosives in the UK Forensic Explosives Laboratory. Dstl, Ft.
Halstead, United Kingdom.
Oxley J, Buco R. Computer Searchable Database of Explosive Properties. University of Rhode
Island, Kingston, Rhode Island, USA.
DeHaan J. Volatile Organic Compounds from Combustion of Human and Animal Tissue. Fire-
Ex Forensics Inc., Vallejo, California, USA.
Garbutt D. Recovery of TATP During Post Blast Exercises. RCMP Forensic Laboratory,
Explosives Section, Ottawa, Canada.

Appendix D

Miscellaneous Citations for Explosives Detection Technology

2001-2004

Mostak P, Stanel M. Detection of SEMTEX Plastic Explosives. NATO Science Series, II:
Mathematics, Physics and Chemistry 2002; 66: 93-102.

Kolla P. Trace Detection of Components Emanating from Hidden Explosives. NATO Science
Series, II: Mathematics, Physics and Chemistry 2002; 66:77-81.

Kozlovsky S, Kyzyurov V, Laykin A, Olshansky Y. Development of a Combined Device for the

Detection of Unauthorized Transportation of Explosive, Fissionable and Radioactive Materials.
Nuclear Instruments & Methods in Physics Research, Section AA: Accelerators, Spectrometers,
Detectors, and Associated Equipment 2003; 505 (1-2): 478-481.
348
Vakhtin D, Evsenin A, Kuznetsov A, Osetrov O, Zubkov M. Decision-taking Procedure for
Explosive Detection by Nuclear Technique 2002; NATO Science Series, II: Mathematics,
Physics and Chemistry 2002; 66:59-67.

Krausa M, Massong H, Rabenecer P, Ziegler H. Chemical Methods for the Detection of Mines
and Explosives. NATO Science Series, II: Mathematics, Physics and Chemistry 2002; 66:1-19.

Kotel’nikov G, Yakovlev G. Potentials for Detection of Explosive Materials by Using Neutron

Irradiation and Simultaneous Recording of Nitrogen and Oxygen Gamma-Radiation.
Inzhenernaya Fizika 2001; (4): 69-70.

Chen L, Feng C, editors. On the Explosives Detection. Proceedings of the International Autumn
Seminar on Propellants, Explosives and Pyrotechnics 2001; 4th, Shaosing, China October 25-28,
2001: 751-755.

Vourvopoulos G, Womble P. Pulsed Fast/Thermal Neutron Analysis: A Technique for

Explosives Detection. Talanta 2001; 54 (3): 459-468.

Bagley I, Coleman M, Beadah A, Doyle S, Wakelin D, Stroud M et al. Stable Isotope Ratio
Analysis of Explosives- A New Type of Evidence. Forensic Science International 2003; Abstract
# FE 136 (Supplement 1): 140.

Jimenez A, Navas M. Chemiluminescence Detection Systems for the Analysis of Explosives.

Journal of Hazardous Materials 2003; 106 (1): 1-8.

Ivanov N, Novikov V, Shemaev A. Radiation Beam Technologies in Detection and Destruction

of Explosives. NATO Science Series, II: Mathematics, Physics and Chemistry 2002; 66:243-
246.

Pumera M, Wang J. Contactless conductivity detector for microchip capillary electrophoresis:

fast measurements of explosives and explosive residues. Journal for the Association of
Laboratory Automation 2002; 7 (4): 47-49.

Choi M, Bettermann A, van der Weide D. Potential for detection of explosive and biological
hazards with electronic terahertz systems. Philosophical Transactions of the Royal Society of
London, Seires A: Mathematical, Physical and Engineering Sciences 2004; 362 (1815): 337-
349.

Bulk

Kiraly B, Olah L, Csikai J. Neutron-based Techniques for Detection of Explosives and Drugs.
Radiation Physics and Chemistry 2001; 61 (3-6): 781-784.

Gavrish Y, Sidorov A, Gialkovskii A. Nondestructive Elemental Analysis in Searching for

Explosives and Fissioning Materials during Customs Inspection of Cargo. Atomic Energy 2003;
95 (1): 480-485.

Kiraly B, Sanami T, Doczi R, Csikai J. Detection of Explosives and Illicit Drugs Using
Neutrons. Nuclear Instruments & Methods in Physics Research, Section B: Beam Interactions
with Materials and Atoms 2003; 213 (Complete): 452-456.

349
Gamma Resonance Technology

Brondo J, Wielopolski L, Thieberger P, Alessi J, Vartsky D, Sredniawski J. Explosive Detection

Systems Using Gamma Resonance Technology. AIP Conference Proceedings 2003; 680:931-
934.

Wielopolski L, Thieberger P, Alessi J, Brondo J, Vartsky D, Sredniawski J. Gamma Resonance

Technology for Detection of Explosives, Revisited. AIP Conference Proceedings 2003; 680:919-
923.

Guardala N, Farrell J, Dudnikov V, Merkel G. Detection of Hidden Explosives Using Resonant

Gamma Rays from In-flight Annihilation of Fast Positrons. AIP Conference Proceedings 2003;
680: 905-908.

Vartsky D, Goldberg M, Engler G, Shor A, Goldschmidt A, Feldman G, Feldman G, et al.

Detectors for the gamma-ray resonant absorption (GRA) method of explosives detection in
cargo: a comparative study. Proceedings of SPIE – The International Society for Optical
Engineering 2004; 5198 (Hard X-Ray and Gamma-Ray Detector Physics V): 243-253.

Thermal Analysis

Chen C, Bannister W, Viswanathan A, Furry J, Slough G. Micro-Thermal Analysis for Airport

Detection of Energetic Materials. Proceedings NATAS Annual Conference on Thermal Analysis
Applications 1999; 27th: 67-72.

Sensors

Wang X, Lee S, Drew C, Senecal K, Kumar J, Samuelson L. Fluorescent Electrospun Polymer

Films for the Detection of Explosives. Polymer Preprints 2002; 43 (1): 130-131.

Houser E, Mlsna T, Nguyen V, Chung R, Mowery F, McGill A. Rational Materials Design of

Sorbent Coatings for Explosives: Applications with Chemical Sensors. Talanta 2001; 54 (3):
469-485.

Yang X, Du S, Shi J, Swanson B. Molecular Recognition and Self-Assembled Polymer Films for
Vapor Phase Detection of Explosives. Talanta 2001; 54 (3): 439-445.

Pinnaduwage L, Boiadjiev V, Hawk J, Thundat T. Sensitive Detection of Plastic Explosives with

Self-Assembled Monolayer-coated Microcantilevers. Applied Physics Letters 2003; 83 (7):
1471-1473.

Datskos P, Lavrik N, Sepaniak M. Detection of explosive compounds with the use of

microcantilevers with nanoporous coatings. Sensor Letters 2003; 1 (1): 25-32.

Holl, G. Characterization of Chemical Sensors for the Detection of Explosives – Development of

Standards. NATO Science Series, II: Mathematics, Physics and Chemistry 2002; 66: 133-136.

Muralidharan G, Wig A, Pinnaduwage L, Hedden D, Thundat T. Adsorption-desorption

Characteristics of Explosive Vapors Investigated with Microcantilevers. Ultramicroscopy 2003;
97 (1-4) 433-439.

350
Gozani T. Elsalim M, Ingle M, Phillips E. Gamma Ray Spectroscopy Features for Detection of
Small Explosives. Nuclear Instruments & Methods in Physics Research, Section AA:
Accelerators, Spectrometers, Detectors, and Associated Equipment 2003; 505 (1-2): 482-482.

Sohn H, Sailor M, Magde D, Trogler WC. Detection of Nitroarmoatic Explosives Based on

Photoluminescent Polymers Containing Metalloles. Journal of the American Chemical Society
2003; 125 (13): 3821-3830.

Luggage

Ostafin M, Nogaj B. Detection of Plastic Explosives in Luggage with 14N Nuclear Quadruple
Resonance Spectroscopy. Applied Magnetic Resonance 2000; 19 (3-4): 571-578.

Jupp I, Durrant P, Ramsden D, Carter T, Dermody G, Pleasants I, Burrows D. The Non-Invasive

Inspection of Baggage Using Coherent X-ray Scattering. IEEE Transaction in
Nuclear Science 2000; 47 (6, Part 2): 1987-1994.

Farsoni A, Mireshghi S. Design and Evaluation of a TNA explosive Detection System to Screen
Carry-on Luggage. Journal of Radioanalytical Nuclear Chemistry 2001; 248 (3): 695-697.

Soil

Simonson, R, Hance B, Schmitt R, Johnson M, Margis P. Remote Detection of Nitroaromatic

Explosives in Soil Using Distributed Sensor Particles. Proceedings of SPIE – The International
Society for Optical Engineering (Part 2, Detection and Remediation Technologies for Mines and
Minelike Targets VI 2001; 4394.

Walsh M. Determination of Nitroaromatic, Nitramine, and Nitrate Ester Explosives in Soil by

Gas Chromatography and an Electron Capture Detector. Talanta 2001; 54 (3): 427-438.

Landmines

Kuznetsov A. Concept of a Combined Mobile Device for Explosives and Landmine

Identification Based on Timed Neutron Source and Electromagnetic UHF Waves. NATO
Science Series, II: Mathematics, Physics and Chemistry 2002; 66:21-32.

Schubert H, Kuznetsov A, Editors. Detection of Explosives and Landmines: Methods and Field
Experience. NATO Science Series, II: Mathematics, Physics and Chemistry 2002; 66.

Jenkins T, Legget D, Miyares P, Walsh M, Ranney T, Cragin J, George V. Chemical Signatures

of TNT-Filled Land Mines. Talanta 2001; 54 (3): 501-513.

Trace

Buxton T, Harrington P. Rapid Multivariate Curve Resolution Applied to Identification of

Explosives by Ion Mobility Spectrometry. Analytica Chimica Acta 2001; 434 (2): 269-282.

Buryakov I, Kolomiets Y, Luppu B. Detection of Explosives Vapors in the Air Using Ion Drift
Nonlinearity Spectrometer. Journal of Analytical Chemistry 2001; 56 (4): 336-340.

351
James R, DeBono R, Kuja F, May L, Jackson R. Rapid Detection of Explosives, Chemical
Warfare Agents and Toxic Industrial Chemicals Using Ion Mobility Spectrometry. Annual
Meeting Proceedings of the Institute of Nuclear Materials Management 2002; 43rd: 272-278.

Schultz J, Taubman M, Harper W, Williams R, Myers T, Cannon B, et al. Quantum Cascade

Transmitters for Ultrasensitive Chemical Agent and Explosives Detection. Proceedings of SPIE
– The International Society for Optical Engineering 2003; 4999 (Quantum Sen.): 1-18.

Shriver-Lake L. Charles P, Kusterbeck A. Non-aerosol Detection of Explosives with Continuous

Flow Immunosensor. Analytical and Bioanalytical Chemistry 2003; 377 (3): 550-555.

Vetlicky B. Detection of Nanogram Amounts of Explosives. NATO Science Series, II:

Mathematics, Physics and Chemistry 2002; 66:33-37.

Buryakov I. Detection of Explosive Vapours in Ambient Air by Ion Non-linear Drift

Spectrometry Method. 2002; NATO Science Series, II: 2002; 66: 69-75

Appendix E

Dstl Internal Customer Reports on Explosives Analysis

2001-2004

Sanders K, Phillips S, Mountford S. Investigation into the deposition and recovery of explosives
traces from hair. Dstl customer report DSTL/CR09604, 2003.

Gray J. Recovery of explosives traces using the contact heater. Dstl customer report
DSTL/CR4109, 2004.

Salt I. Evaluation of the modified contact heater for the recovery of explosives traces. Dstl
customer report DSTL/CR09231, 2004.

Dear R. LC-MS analysis of HMX, RDX, Tetryl, NG, TNT and PETN. DERA customer report
DERA/CES/CS/CR000229, 2000.

Watson S. LC/MS development during the period July 2001-Auguts 2002. Dstl customer report
DSTL/CR04832, 2002.

Robertson C. LC-MS development during the period of September 2002 – August 2003. Dstl
customer report DSTL/CR08084, 2003.

Phillips S, Philp L, Watson S, Vaughan I. Recovery of peroxide explosives from soil. Part 1 –
Development of methods for the recovery and trace analysis of TATP. Dstl customer report
DSTL/CR04199, 2002.

Mountford S. Recovery of peroxide explosives from soil. Part 2 – Optimisation of recovery and
trace analysis of TATP. Dstl customer report DSTL/CR07551, 2003.

Phillips S. Review of the effectiveness of anti-contamination procedures for explosives trace

analysis. DERA customer report DERA/DSTL/CR00586, 2001.

352
Salt I. Survey of inorganic traces in the environment – final report. Dstl customer report
DSTL/CR08232, 2003.

Beardah A. Recovery of evidence from deflagrating explosive devices. Part 1 – Evaluation of

techniques currently employed at the Forensic Explosives Laboratory. Dstl customer report
dERA/DSTL/CR00919, 2001.

Phillips S. Recovery of evidence from deflagrating explosive devices. Part 2 - Detection of post
explosion spheroid residue particles by SEM/EDS. Dstl customer report DSTL/CR06612, 2003.

Phillips S. Recovery of evidence from deflagrating explosive devices. Part 3: Analysis using
variable pressure SEM and ATR-microspectroscopy. Dstl customer report DSTL/CR06612,
2003.

Ritchie K. Development of a rapid screening process for inorganic explosives. Dstl customer
report DERA/DSTL/CR01027, 2001.

Beardah M. Evaluation of a capillary zone electrophoresis method for the screening of inorganic
explosive traces. Dstl customer report DSTL/CR03936, 2002.

Prest J. Separation of small ions present in explosives residues using isotachophoresis. Progress
report January 2004, SCTL/ETD/FEL/205/1 Pt A.

King A. Investigation into the post-blast survivability of DNA. Dstl customer report
DSTL/CR04084, 2002.

Wakelin D. Isotope ratio analysis of explosive traces – a new type of evidence. DERA
customer report dERA/CES/CS/CR000294, 2000.

Beardah A. Stable isotope ratio mass spectrometry of explosives – a new type of evince. Part 3.
Dstl customer report DSTL/CR05104, 2002.

Zolnhofer N. HPLC of propellant stabilizers. Dstl customer report DSTL/CR02786, 2002.

Gibson A. The use of capillary electrophoresis with indirect UV detection in the analysis of
sugars. Dstl customer report DSTL.CR01350, 2001.

Walker A. Evaluation of the SensIR Technologies ‘TravelIR’ for use in forensic analysis at
scenes of crime. Dstl customer report DSTL/CR00984, 2001.

McKay G. Triacetone triperoxide (TATP) training aids for dogs. Dstl customer report
DERA/DSTL/CR00824, 2001.

Phillips S. Proceedings of the International Workshop on the Forensic Aspects of Peroxide

Explosives, 5th-6th December 2001. Dstl customer report DSTL/CR02638, 2002.

Phillips S, Philp L. Proceedings of the International Seminar on the Recovery of Forensic

Explosives Evidence, 3rd-4th September 2003. Dstl customer report DSTL/CR09424, 2004.

Phillips S., Doyle S. Mountford S. Proceedings of the Forensic Isotope Mass Spectrometry
(FIRMS) Workshop, 14th May 2003. Dstl technical report DSTL/TR07549, 2003.

353
Phillips S., Doyle S. Forensic Isotope Ratio Mass Spectrometry Network – Technical Strategy.
Dstl technical strategy DSTL/STR08207, 2003.

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Explosives: RDX Adduct Ions. Rapid Communications in Mass Spectrometry 2003; 17
(9): 943-948.
51 Gapeev A, Yinon J. Application of Spectral Libraries for Characterization of Oxidizers
by Electrospray Mass Spectrometry. Journal of Forensic Sciences 2004 March; 49(2):
227 - 237.
52 Takada Y, Nagano H, Suga M, Hashimoto Y, Yamada M, Sakairi M, Kusumoto K, Ota
T, Nakamura J. Detection of Military explosives by Atmospheric Pressure Chemical
Ionization Mass Spectrometry with Counter-Flow Introduction. Propellants, Explosives,
Pyrotechnics 2002; 27: 224-228.
53 Wu Z, Hendrickson C, Rodgers R, Marshall A. Composition of Explosives by
Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry
Analytical Chemistry 2002; 74: 1879 – 1883.
54 Meurer E, Chen H, Riter L, Cotte-Rodrigues I, Eberline M, Cooks R. Gas-phase
reactions for selective detection of the explosives TNT and RDX. Chemical
Communications 2004; (1): 40-41.
55 Oxley J, Smith J, Resende E. Determining explosivity Part II: Comparison of Small-scale
Cartridge Tests to Actual Pipe Bombs. Journal of Forensic Sciences 2001; 46 (5): 1070-
1075.

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56 Oxley J, Smith J, Resende E, Rogers E, Strobel R, Bender E. Improvised Explosive
Devices: Pipe Bombs. Journal Forensic Sciences 2001; 46 (3): 510-534.
57 Walsh G, Inal O, Romero V. A Potential Metallographic Technique for the Investigation
of Pipe Bombings. Journal of Forensic Sciences 2003 September; 48 (5): 945-960.
58 Walker C, Cullum H, Hiley R. An Environmental Survey Relating to Improvised and
Emulsion/Gel Explosives. Journal of Forensic Sciences 2001; 46 (2)” 254-267.
59 Sanders KP, Marshall M, Oxley JC, Smith JL, Egee L. Preliminary Investigation into the
Recovery of Explosives from Hair. Science and Justice 2002; 42 (3): 137-142.
60 Oxley J, Smith J, Resende E, Pearce E, Chamberlain T. Trends in Explosives
Contamination. Journal of Forensic Sciences 2003; 48 (2): 334-342.
61 Walker C, Cullum H, Hiley R. An Environmental Survey Relating to Improvised and
Emulsion/Gel Explosives. Journal of Forensic Sciences 2001; 46 (2)” 254-267.
62 Pillai A, Sanghavi R, Dayana C, Joshi M, Velapure S, Singh A. Studies on RDX Particle
Size in LOVA Gun Propellant Formulations. Propellants, Explosives, Pyrotechnics 2001;
26 (5): 226-228.
63 Crowson A, Hiley R, Clifford C. Quality Assurance Testing of an Explosive Trace
Analysis Laboratory. Journal of Forensic Sciences 2001 January; 46 (1): 53-56.
64 Song Y, Xu J, Xu G, He D. Investigation of Raw TNT Applicated in Industrial
Explosive. Huozhayao Xuebao 2001; 25 (1): 69-70.
65 Halasz A. Groom C, Zhou E, Paquet L, Beaulieu C, Deschamps S et al. Detection of
Explosives and their Degradation Products in Soil Environments. Journal of
Chromatography A 2002 July; 963 (1-2): 418-441.
66 Buxton T, Harrington P. Trace Explosives Detection in Aqueous Samples by Solid-Phase
Extraction Ion Mobility Spectrometry (SPEIMS). Applied Spectroscopy 2003; 57 (2):
223-232.
67 Walsh M. Determination of Nitroaromatic, Nitramine, and Nitrate Ester Explosives in
Soil by Gas Chromatography and an Electron Capture Detector. Talanta 2001; 54 (3):
427-438.
68 Oxley J, Smith J, Resende E, Pearce E. Quantification and Aging of the Post-blast
Residue of TNT Landmines. Journal of Forensic Sciences 2003 48 (4): 742-753.
69 Jung C, Newcombe D, Crawford D, Crawford R. Detection and Decontamination of
Residual Energetics from Ordnance and Explosives Scrap. Biodegradation 2004; 15 (1):
41-48.
70 Personal communication. Dr. Chris Lennard, Manager Operations Support, Forensic &
Technical Services, Australian Federal Police, GPO Box 401, Canberra, ACT 2601,
Australia.
71 Personal communication, Wendy W. Norman, Explosives Section Royal Canadian
Mounted Police, Forensic Laboratory Services – Ottawa, 1200 Vanier Parkway, PO Box
8885,Ottawa, Ontario K1G 3M8 Canada.
72 Dr. Frantisek Zrcek, Department of Chemistry, Institute of Criminalistics, Prgeu, POB
62/KUP, Strojnicka 27, 17089 Prague, the Czech Republic.
73 Personal communication, Sean Doyle, Head of Chemistry and Research, Dstl, Fort
Halstead, Seveoaks, Kent TN14 7BP, United Kingdom.
74 Yinon J. Field Detection and Monitoring of Explosives. TrAC, Trends in Analytical
Chemistry 2002; 21 (4): 292-301.
75 Yinon J. Detection of Explosives by Electronic Noses. Analytical Chemistry 2003; 75
(5): 99A-105A.
76 Furton K, Myers L. The Scientific Foundation and Efficacy of the Use of Canines as
Chemical Detectors for Explosives. Talanta 2001; 54 (3): 487-500.

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77 Furton K, Harper R, Perr J, Almirall J. Optimization of Biological and Instrumental
Detection of Explosives and Ignitable Liquid Residues including Canines, SPME/ITMS
and GC/MS. Proceedings of SPIE – The International Society for Optical Engineering
2003; 5071(Sensors and Command, Control, Communications and Intelligence): 183-
192.
78 Ruiping Z, On the explosives detection. Proceedings of the International Autumn
Seminar on Propellants, Explosives and Pyrotechnics 2001; 751-755.
79 Meng X. Explosives and Narcotic Detection Technologies. He Dianzixue Yu Tance Jishu
2003; 23 (4): 363, 371-379.
80 Gowadia H, Settles, G. The Natural Sampling of Airborne Trace Signals from Explosives
Concealed Upon the Human Body. Journal of Forensic Sciences 2001; 46 (6): 1324-
1331.
81 Wu C, Steiner W, Tornatore P, Matz L, Siems Watkinson D, et al. Construction and
Characterization of a High-flow High-resolution Ion Mobility Spectrometer for Detection
of Explosives after Personnel Portal Sampling. Talanta 2002, 57 (1): 123-134.
82 Bannister WW, Chen C, Curby W, Chen EB, Damour P, Morales A. Thermal Analysis
for Detection and Identification of Explosives and Other Controlled Substances. US
Patent 2002; US2000-491026.
83 Kuo C, Nagarajan R, Bannister W, Loder R, Furry J, Chen C. Detection of concealed
explosives and drugs by thermal analysis and thermal profiles of samples with
microsensors. US Patent 2004 2004027386 A2.
84 Nguyen D, Berry S, Gelewicz J, Courure G, Huynh P. Chemiluminescent detection of
explosives, narcotics, and other chemical substances. US Patent 2004: US20050053421
A1.
85 Schwartz P, Murray G, Uy O, LeBinh Q, Stott D, Lew A. Apparatus and Methods for
Detecting Explosives and other Substances. US Patent 2001 May; US14190 3.
86 Allen W, Ige L. Sampling device with test strip inserted into air aspirated from luggage
interior for detection of concealed explosives. US Patent 2004; US200435187.
87 Krasnobaev L, Persenkov V, Belyakov V, Kekukh V, Bunker S. Explosive Detection
System. US Patent 2003; US20030193338 A1.
88 Gartsev N, Semeikin N, Sharshin Y, Pomozov V, Trushkov V, Alekseev N, et al. Device
for detection of explosives and narcotics. Russian Patent Application: RU 2001-
118733.
89 Vorogushin M, Gavrish Y, Sidorov A, Gialkovskii A. Method for Detection of
Fissionable and Explosive Substances. Russian Patent 2001; RU1999-110873 26.

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 ENVIRONMENTAL CRIME

— A Review: 2001 to 2004 —

Jennifer A. Suggs, MS
Kenna R. Yarbrough, BS

Library assistance provided by:

Dorothy E. Biggs, NEIC

Barbara L. Wagner, Contractor (Vistronix)
Nancy B. Greer, Contractor (Vistronix)

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

OFFICE OF ENFORCEMENT AND COMPLIANCE ASSURANCE
OFFICE OF CRIMINAL ENFORCEMENT, FORENSICS AND TRAINING

Author to whom correspondence should be addressed:

Jennifer A. Suggs
EPA-NEIC
Bldg. 25, Denver Federal Center
Denver, CO 80225

NATIONAL ENFORCEMENT INVESTIGATIONS CENTER

Diana A. Love, Director
Denver, Colorado

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CONTENTS

List of acronyms

Introduction

Overview
Authors’ perspective

Environmental crime scene

Voluntary consensus standards and method standardization

Sampling guidance

Laboratory analysis of environmental samples

Recent books
General environmental chemistry books
General instrument techniques books
Method and technique specific books
Substance specific books
Instrumentation and techniques by topic

special topic–endocrine disrupting compounds

Methods for the identification of endocrine disruptors

Appendices

a) Major environmental laws of the united states environmental protection agency

(usepa)
b) USGS national water quality laboratory methods of analysis

References

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LIST OF ACRONYMS

µ-AED – micro-atomic emission detector

µ-ECD – micro-electron capture detector
AA – atomic absorption
AAS – atomic absorption spectrometry
AE – atomic emission
AED – atomic emission detection
AES – atomic emission spectrometry
AF – atomic fluorescence
ANSI – American National Standards Institute
AOCD – 9-(2-acridone)oxyethylcarbonylimidazole
APCI – atmospheric pressure chemical ionization (mode)
APEO – alkylphenol ethoxylate
ASE – accelerated solvent extraction
ATR – attenuated total reflectance
BFRs – brominated flame retardants
BTEX – benzene, toluene, ethylbenzene, and xylene
CAA – Clean Air Act
CAS – Chemical Abstracts Service (as in CAS #)
CDFMS – compact double-focusing mass spectrometer
CE – capillary electrophoresis
CERCLA – Comprehensive Environmental Response, Compensation, and Liability Act
CFR – US Code of Federal Regulations
CIT – cylindrical ion trap
CLU-IN – USEPA Technology Innovation Program. Hazardous Waste Clean-Up
Information
CMC – chromatomembrane cells
CRM – certified reference material
CWA – Clean Water Act
DFG – Deutsche Forschungsgemeinschaft (German Research Foundation)
ECD – electron capture detector
EDCs – endocrine disrupting compounds or endocrine disrupting chemicals
EDSP – Endocrine Disruptor Screening Program
EDXRF – energy dispersive X-ray fluorescence
EPCRA – Emergency Planning and Community Right-To-Know Act
ES – electrospray
ESA – Endangered Species Act
ESI – electrospray ionization (mode)
ETAAS – electrothermal atomic absorption spectrometry
ETV – electrothermal vaporization
FA – flow analysis
FAAS – flame atomic absorption spectrometry
FEM – USEPA Forum on Environmental Measurement
FFDCA –Federal Food, Drug and Cosmetic Act
FI – flow injection

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FID – flame ionization detector
FIFRA – Federal Insecticide, Fungicide, and Rodenticide Act
FIMS – fiber introduction mass spectrometry
FLD – fluorescence detection
FM – focused-microwave (irradiation)
FMASE – focused-microwave assisted Soxhlet extraction
FMOC – 9-fluorenylmethyl chloroformate
FPC – focal plane camera
FPD – flame photometric detection
FSL – fused-silica-lined
FT – Fourier transform
FTIR – Fourier transform infrared (spectrometry)
GC – gas chromatography
GC x GC – two-dimensional gas chromatography
GD – glow discharge
GPO – US Government Printing Office
HFs – hydraulic fluids
HG – hydride generation
HPLC – high performance liquid chromatography
HS – headspace
IC – ion chromatography
ICP – inductively coupled plasma
ICR – ion cyclotron resonance
IR – infrared
ISO – International Organization for Standardization
LC – liquid chromatography
LIF – laser induced fluorescence
LLLME – liquid-liquid-liquid microextraction
LPME – liquid-phase microextraction
LVI – large-volume injection
MAE – microwave assisted extraction
MC – multicollector
MEC – microwave enhanced chemistry
MIP – molecularly imprinted polymer
MS – mass spectrometry
MTBE – methyl t-butyl ether
MWFs – metalworking fluids
NCI – negative chemical ionization
NEIC – National Enforcement Investigations Center
NEPA – National Environmental Policy Act
NI – negative ion (mode)
NICI – negative ion chemical ionization
NIST – National Institute of Standards and Technology
NMR – nuclear magnetic resonance
NSAIDs – nonsteroidal anti-inflammatory drugs
NTIS – National Technical Information Service

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NTTAA – National Technology Transfer and Advancement Act
OCPs – organochlorine pesticides
OERR – USEPA Office of Emergency and Remedial Response
OES – optical emission spectrometry
OMB – US Office of Management and Budget
OPA – Oil Pollution Act
ORD – USEPA Office of Research and Development
OSWER – USEPA Office of Solid Waste and Emergency Response
OVAs – organic vapor analyzers
PAHs – polycyclic aromatic hydrocarbons or polynuclear aromatic hydrocarbons
PBDEs – polybrominated diphenyl ethers
PCBs – polychlorinated biphenyls
PCDDs – polychlorinated dibenzodioxins or polychlorinated dibenzo-p-dioxins
PCDFs – polychlorinated dibenzofurans
PFBBR – pentafluorobenzyl bromide
PFE – pressurized fluid extraction
PFPA – pentafluoropropionic acid
PI – positive ion (mode)
PID – photoionization detector
PIF – photochemically induced fluorimetry
PLE – pressurized liquid extraction
PM – particulate matter
PPA – Pollution Prevention Act
PPCPs – pharmaceuticals and personal care products
PXRF – portable X-ray fluorescence
PyGC – flash pyrolysis gas chromatography
RCRA – Resource Conservation and Recovery Act
RP – reversed-phase
SARA – Superfund Amendments and Reauthorization Act
SBSE – stir bar sorptive extraction
SCCPs – short-chain chlorinated paraffins
SDWA – Safe Drinking Water Act
SES – sequential extraction schemes
SF – sector field
SIA – sequential injection analysis
SIM – selected ion monitoring
SPE – solid phase extraction
SPME – solid-phase microextraction
SRMs – standard reference materials
SSPE – sequential solid-phase extraction
SVOCs – semi-volatile organic compounds
SW-846 – Test Methods for Evaluating Solid Waste: Physical/Chemical Methods
TBA – t-butyl alcohol
TBT – tributyltin
THMs – trihalomethanes
TIC – total ion chromatogram

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TLC – thin-layer chromatography
TMA – trimethylamine
TMSD – trimethylsilyldiazomethane
TMSI – N-trimethylsilylimidazole
TOF – time-of-flight
TSCA – Toxic Substances Control Act
TXRF – total reflection X-ray fluorescence
UE – ultrasonic extraction
US – United States
USEPA – United States Environmental Protection Agency
USGS – United States Geological Survey
VOCs – volatile organic compounds
WRI – USGS Water-Resources Investigations Report
WWTP – wastewater treatment plant
XRF – X-ray fluorescence
XRS – X-ray spectrometry

INTRODUCTION

OVERVIEW

This environmental crime review is a follow-up to the 2001 review paper prepared for the
13th International Forensic Science Symposium. 1 Some information presented earlier will
be repeated such as resources for sampling methods and the annual or biannual
instrumentation reviews regularly featured in some journals. Other topics within the paper
are new or in an expanded presentation such as consensus standards, environmental
measurements, sampling guidance, and endocrine disrupting compounds.

The paper will proceed in an order roughly resembling that taken during an environmental
crime investigation, as the previous review paper did. Information regarding the fieldwork
or work at the actual crime scene will be presented first then followed by a section on
analytical methods developed and published during the past 3 years. Reference
information has been gathered from books, websites, and journals.

AUTHORS’ PERSPECTIVE

The United States Environmental Protection Agency (USEPA) was established to protect
human health and the environment in the United States (US). Several environmental laws
provide the guidance for this mission (a list of major environmental laws is provided in
Appendix A). The National Enforcement Investigations Center (NEIC) is part of the
USEPA. 2 The NEIC investigates, develops, and assists in prosecuting environmental
crimes.

The Code of Federal Regulations (CFR) contains the guidance, requirements, and
boundaries for environmental crime investigations. 3 The USEPA is bound by these

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regulations for the prosecution of environmental crime cases. Many specific sampling and
testing methods are required by law for the prosecution of an environmental crime. Much
of the information presented here (for example, alternate methodologies) is not being used
in the prosecution of environmental crimes in the United States, but it is our hope that it
may be useful to other environmental protection entities.

While the USEPA NEIC is limited to enforcement, other sections of the agency are
involved in the research of new environmental issues, the development of methods for
identification and quantitation of hazardous substances, and the development of improved
ways of sampling and assessing sites, as well as improving the treatment or recovery of
these same sites. The Office of Research and Development (ORD) is the scientific
research arm of the USEPA. ORD has eight priority areas for scientific research: air,
drinking water, ecosystem assessment and restoration, global change, human health
protection, water quality, pollution prevention and new technologies, and endocrine
disrupting chemicals (EDCs). 4 Internationally, endocrine disrupting chemicals (or
endocrine disrupting compounds) and the affects of these chemicals on human and
environmental health are developing areas of concern. A brief section on EDCs and
analytical techniques for the identification and quantitation of EDCs has been included
after the laboratory methods section.

ENVIRONMENTAL CRIME SCENE

Decisions made by investigators regarding an environmental investigation must be

supported by facts obtained about the scene. If samples are taken and if laboratory analysis
occurs, all individuals gathering information and evidence need to maintain certain high
standards of care that will enable results to be accurate and reproducible. Several
organizations are involved in developing consistent, quality standards for sampling and
field measurements. The general agreements on what should be included in the quality
standards become consensus standards.

VOLUNTARY CONSENSUS STANDARDS AND METHOD STANDARDIZATION

Voluntary consensus standards are standards developed or adopted by voluntary consensus

standards bodies. These bodies must agree to make the standards available on a non-
discriminatory, royalty-free or reasonable royalty basis to all interested parties. Voluntary
standards are distinguished from mandatory standards, which are published standards that
are part of a code, rule or regulation and there is an obligation by certain parties to conform
to the standard. Some voluntary standards become de-facto mandatory standards when
they are referenced or required by a code, rule, or regulation.

In February 1998, the revised circular No. A-119 was published by the Office of
Management and Budget (OMB) concerning federal participation in the development and
use of voluntary consensus standards. 5 The circular directs US federal agencies to use
voluntary consensus standards in lieu of government-unique standards except where
inconsistent with law or otherwise impractical. This circular was developed due to the
approval of the 1995 National Technology Transfer and Advancement Act (NTTAA)

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which emphasized the use by federal agencies of standards developed by private,
consensus organizations. 6 A recent article in ASTM Standardization News makes the point
that regulators may be forced to change regulations to incorporate provisions of relevant
consensus standards. 7

The American National Standards Institute (ANSI) is a private, non-profit organization that
administers and coordinates the US voluntary standardization system. 8 It is the official
US representative to the world’s leading standards bodies, including the International
Organization for Standardization (ISO). ANSI has a membership of approximately 1000
companies, organizations, government agencies and others. Although ANSI doesn’t
develop standards, it provides interested parties a setting to come together, working toward
common agreements. A 1996 National Institute of Standards and Technology (NIST)
document reports that there are almost 700 standards producing bodies in the United
States, with more than 93,000 standards produced. 9 The NSSN is a product of ANSI, and
serves as a comprehensive data network on developing and approved national/international
standards and regulatory documents on the World Wide Web. 10 The NSSN routes
different users to both commercially available and regulatory technical documents that
they may need. NSSN has many helpful lists concerning consensus standards and the
bodies that develop them, for example, the acronym directory of US standards developers.
11
This list is updated regularly.

Environmental measurement related voluntary consensus standards are developed from

many different national and international organizations. The ISO produces the largest
number of international standards. 12 ISO has standards concerning environmental
measurements and sampling, particularly wastewater sampling, and these standards are
available for purchase on the organization’s webpage. 13 ASTM International is also one
of the largest voluntary consensus standard development organizations in the world. This
organization has many different committees and subcommittees on environmental
measurements. 14 The ASTM committee on Waste Sampling is designated as D-34. This
committee focuses on the promotion of knowledge, stimulation of research and
development of test methods, practices, etc. relating to the management of wastes,
especially as they relate to sampling of waste streams. Other ASTM International
committees concerning environmental measurements and sampling are D-18, Soil and
Rock; D-19, Water; and D-22, Sampling and Analysis of Atmospheres. Of additional
interest is Committee E-30, Forensic Sciences. The scope of this committee focuses on the
promotion of knowledge and development of standards for methods and standard reference
materials for the collection, preservation, scientific examination, preparation and reports
relating to physical evidence for forensic purposes and the general practice of forensic
science. Additional information concerning these committees and the standards available
for purchase is located on the organization’s webpage. 15

The USEPA has created a Forum on Environmental Measurement (FEM). 16 This

committee of senior USEPA managers was formed in order to enhance measurement
programs by agreeing on basic principles to promote consistency and consensus within the
agency on measurement issues. Some Agency-wide measurement issues that are being
worked on include:

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Validation of new USEPA measurement methods
Identifying and correcting problems with existing measurement methods
Ensuring and demonstrating the competency of USEPA laboratories
Consolidation USEPA supported measurement science conferences and
Use of performance approach in USEPA-mandated monitoring programs

The work being performed concerning validation of new USEPA measurement methods is
to help the FEM develop guidelines as to what represents the minimum level of method
validation and peer review before methods are issued by the Agency.

SAMPLING GUIDANCE

The USEPA publication, SW-846, titled Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods is the USEPA’s official compendium of analytical and
sampling methods that have been evaluated and approved for use in complying with the
USEPA’s waste regulations (Resource Conservation and Recovery Act or RCRA). 17 This
guidance publication has acceptable, through not required, methods for the
regulated/regulating communities to use for RCRA-related sampling and analysis
requirements. Chapters 9 and 10 of SW-846 concern developing sampling plans and
sample methodologies. The multi-volume publication changes over time as new
information and data are available. The current version is available on-line or an official
printed copy of SW-846 and most of its updates can be purchased from either the US
Government Printing Office (GPO) or the National Technical Information Service (NTIS).
18, 19
In October 2002, the USEPA made available a new draft guidance document for
public comment entitled "RCRA Waste Sampling Draft Technical Guidance.” This new
RCRA waste sampling guidance updates the information provided in Chapter 9 of SW-
846, which was last published in 1986, and is also available on-line.

Methods and Guidance for Analysis of Water is the USEPA’s primary resource for
sampling and analyses of water. This resource was most recently updated in 1999. 20 The
USEPA Office of Solid Waste and Emergency Response (OSWER) published a
groundwater forum issue paper in 2002 with the most up-to-date groundwater sampling
issues and guidelines. 21 Most air emission sampling and measurement methods for the US
EPA have been proposed or promulgated in the Federal Register and codified in the Code
of Federal Regulations (CFR). The methods are directly cited by specific regulations for
determining compliance under the air regulations in 40 CFR Parts 60, 61, and 63. 3

Within the USEPA Office of Emergency and Remedial Response (OERR) Superfund
program for cleaning up abandoned waste sites, there are several representative sampling
guidances for air, water, sediment/soil, biota, and waste. 22-26 These and other sampling
and environmental technologies are available through the USEPA Technology Innovation
program’s Hazardous Waste Clean-Up Information (CLU-IN) internet site. 27 The
USEPA’s Information Sources webpage lists hundreds of published reports and test
methods/sampling procedures and many are available for direct downloading. 28 Also, the
USEPA’s most comprehensive list of sampling, measurement, and analytical test methods
was developed by the Region 1 library staff. 29 The list is continually updated, currently

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contains about 1600 methods, and the majority of sources listed have live web links to the
actual method.

LABORATORY ANALYSIS OF ENVIRONMENTAL SAMPLES

Environmental analysis continues to be a growing field and while not all current areas of
study can be applied directly to environmental crime investigations, the research can
provide insights into the latent potential of new developments in instrumentation and
techniques.

RECENT BOOKS

General Environmental Chemistry Books

A few books published during the past three years provide introductions for the newcomer
into environmental chemistry. The Fundamentals of Environmental Chemistry textbook
has a fast, basic overview of environmental chemistry. The first third of the book consists
of a general chemistry primer with a touch of biochemistry. The rest of the book provides
a quick, clear foundation for learning about the environmental chemistry and pollution of
water, soil and the atmosphere. Topics in this section progress to include industrial
ecology, hazardous wastes, toxicological chemistry, analytical chemistry, and
environmental analysis. 30

Environmental Organic Chemistry is a textbook that progresses from the basic makeup of
organic compounds to the interaction of these compounds in environmental systems.
Major sections include the introduction to basic concepts in organic chemistry, the
equilibrium between the gas, liquid and solid phases, transformation processes of organic
compounds (chemical, photochemical and biological), transport phenomena (diffusion and
interaction between boundaries, for example, the air-water interface) and environmental
case studies combining the concepts presented throughout the book. One clear benefit to
the user of this book is the extensive bibliography allowing further follow-up for the
subjects covered in the book. 31

Soil and Environmental Analysis is an updated book on analytical techniques for the
analysis of environmental samples—primarily soil, but topics do include some water and
gas analyses. Each chapter provides a general background on techniques and addresses
several technique-specific concerns like sample preparation, sample introduction systems
and specific applications of the technique within environmental analysis. 32

Introduction to Environmental Forensics walks the reader through the early steps of an
environmental forensic investigation (witness statements, historical documents, and
photographic records) into the analytical measurements taken for forensic use. The
majority of the book deals with the measurements and includes topics such as chemical
fingerprinting of hydrocarbons, air dispersion modeling, particulate pattern recognition and
statistical methods. Each chapter provides a list of references or additional reading sources

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at the end and the appendices contain detailed chlorinated solvent information (history,
chemical names, commercial synonyms, and chemical properties). 33

General Instrument Technique Books

A history of mass spectrometry (MS) and its developments in sample introduction and
detection is given by de Laeter in the first portion of his book, Applications of Inorganic
Mass Spectrometry. The majority of the book contains an overview of the large number of
applications for the MS technique including a chapter on environmental science. de
Laeter’s book also has extensive references at the end of each chapter. 34

X-Ray Spectrometry: Recent Technological Advances is an up-to-date review of progress

in X-ray spectrometry (XRS); most of the references within this book are less than eight
years old. It does not revisit the fundamentals of analytical chemistry techniques based on
X-rays, but does include references to handbooks and text books that provide the basic
information. Early chapters include details on advances and improvements in X-ray
sources, optics and detector technology. Other sections are dedicated to special XRS
configurations, computerized advances and developments in specific fields. 35

According to one of the editors, R. Van Grieken, there has been a steady increase in the
amount of work published on the environmental applications of XRS analysis. A section
worth highlighting is the one titled “Portable Equipment for X-ray Fluorescence Analysis.”
The authors describe the form and function of energy-dispersive X-ray fluorescence
(EDXRF) equipment and the advances of internal construction—the miniatures and
lightweight solutions for X-ray tubes and detectors. The portable EDXRF systems rival
laboratory-sized spectrometers in analytical capability and have the advantage of providing
results “on the scene” for immediate decision-making.

Budde in Analytical Mass Spectrometry: Strategies for Environmental and Related

Applications presents gas chromatography coupled with mass spectrometry (GC/MS)
analyses as the “killer application” of mass spectrometry and the bulk of the book is
dedicated to GC/MS methods. The author limits his scope to those methods used by the
USEPA and the chapters separate into organic and semi-volatile organic compounds
amenable to gas chromatography (separate chapters), strategies to improve analytical
results, and compounds that are not amenable to GC. A brief mention of ICP/MS is near
the end of the book. 36

Method and Technique Specific Books

The “Air Analysis” group of the Deutsche Forschungsgemeinschaft (DFG), the German
Research Foundation, published a tidy, well-organized source of methods for the analysis
of hazardous materials in the air in several volumes. The most recent volume is #8 and
among the analytical methods included are ones for atrazine (herbicide), polychlorinated
biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and lacquer aerosols. A
brief method summary with a description of the substance (CAS #, structure, physical
properties and synonyms) and the data quality results (accuracy, recovery and limit of

370
quantitation) begins each method. Methods include extensive details on equipment,
chemicals and solutions, sample collection, operating conditions, sources of error and
references. At the back of the book, there is a list of the methods contained in volumes #1-
8. The list is in numerical order by the CAS # of the substance. 37

The US Geological Survey (USGS) National Water Quality Laboratory has published
several methods of analysis for contaminants in water samples or sediment samples in the
Water-Resources Investigations Report (WRI) series. Methods include both organic and
inorganic analyses. A list of the available methods and information on how to obtain these
reports is provided in Appendix B.

Crompton wrote an exceptional reference book on preconcentration techniques for the

analysis of organics, organometallics and inorganics (divided into cations and anions) for
water samples. Each major section ends with one or more summary tables for
preconcentration of specific types of compounds (hydrocarbons, PCBs, insecticides and
herbicides, etc.) or within certain matrices (non-saline water, sea water, surface water,
wastewater, etc.). Crompton provides references for every method and has organized this
book to be a master source of information on preconcentration techniques. 38

Substance Specific Books

Organometallic Compounds in the Environment provides analytical methods and

environmental details (toxicology, pathways, fate, etc.) for organometallic compounds
containing Hg, Sn, Pb, As, Sb, Si, Se, Tl, Bi, Cd, Te, Mn, Ge or Co. 39

A hefty two-volume set titled Handbook of Residue Analytical Methods for Agrochemicals
contains sections of compound classes and the analytical methods for each class. Some
method information is specific to one compound within the particular class. In addition to
the compound class section, volume two has “best practices in the generation and analyses
of residues in environmental samples” including water, soil, sediment, and air samples. 40,
41

If an environmental release of a petroleum product must be investigated, Analytical

Advances for Hydrocarbon Research contains a variety of techniques including gas
chromatography (GC), gas chromatography mass spectrometry (GC-MS), liquid
chromatography mass spectrometry (LC-MS), thin-layer chromatography (TLC), and X-
ray spectrometry (XRS) for the characterization of petroleum and fossil fuel samples. 42
ASTM International has published tables of test methods for products like aviation fuel,
automotive gasoline, fuel oxygenates, crude oils, and more. A brief quality assurance
section and a detailed sampling section (with diagrams) are included. 43

INSTRUMENTATION AND TECHNIQUES BY TOPIC

Environmental Analysis

371
Biennial review; developments in mass spectrometry as applied to environmental analysis;
primarily includes work published during 2002 and 2003 44
Annual review of atomic spectrometry as applied to environmental analysis; major sections
are divided by the matrix (air, water, soil and plant material, and geologic materials) 45
Biennial review; developments in environmental analytical chemistry from 2001 and 2002;
contents include sampling, extraction methods, detection techniques, analytes of interest
and emerging trends 46
Annual review; analysis of environmental samples by atomic spectroscopy; divided into
analysis categories of air, water, soils, and geologic materials 47
Review; covers developments in environmental mass spectrometry during 2000 and 2001
with emphasis on new and emerging contaminants and issues 48

Sampling, Sample Preservation, Sample Preparation

Review; addresses changes that may occur in water samples during storage and techniques
for water sample preservation 49
Reviews factors affecting stability of inorganic mercury and methylmercury during sample
storage, mechanisms for loss of mercury, and suggested treatments to decrease these losses
50

Review; methods of sample preparation for separation techniques; includes examples of

extraction and concentration of analytes from solid, liquid, and gas matrices 51
Sample pretreatment using chromatomembrane cells (CMC) for extraction and
preconcentration of pollutants (polycyclic aromatic hydrocarbons and extractable organic
halogens) from wastewater 52
Addresses sample handling and analysis for resin acids in water samples; provides tables
of analytical techniques (primarily gas chromatography and liquid chromatography, with
various detectors) 53

Extraction

Comprehensive review of sequential extraction schemes (SES) for metal fractionation of

environmental samples; massive applications tables of SES based on types of samples
(soils, sediments, sewage sludges, etc.) 54
Comparison of leaching tests on various soils and sediments for the extraction of Cd, Cr,
Cu, Ni, Pb, and Zn 55
Use of an ultrasound accelerated sequential extraction method for rapid metal partitioning
profiles; study compares results from conventional extraction and ultrasound extraction on
compost samples 56
Ultrasonic extraction (UE) as sample preparation technique for elemental analysis;
extracted standard reference materials and analyzed by inductively coupled plasma atomic
emission spectrometry (ICP-AES) 57
Comparison of ultrasound-assisted extraction to other techniques (Soxhlet, microwave-
assisted, and supercritical fluid extraction) 58
Chelating polymeric sorbent for metal ion extraction (Mn, Pb, Ni, Co, Cu, Cd and Zn);
method applied to sea water, well water, and tap water samples 59

372
Methods of extraction for isolating and preconcentrating organic analytes from
environmental matrices 60

Air Analysis

Study of recoveries and stabilities of volatile organic compounds (VOCs) stored in fused-
silica-lined (FSL) and SUMMA polished canisters; tables of recoveries under various
humidified conditions and over various time intervals at a set relative humidity 61
System for generating gas mixtures of volatile and semi-volatile organic compounds
(VOCs and SVOCs) for use as calibration standards prior to air sampling and analysis 62
Development of a solid-phase microextraction (SPME) technique for the analysis of
odorous gases (triethylamine, propionic and butyric acids, and sulfur compounds) 63
Method for the sampling and analysis of airborne particulate matter (PM) from an inhaler-
administered drug, spray insect repellant, and tailpipe diesel exhaust by SPME fibers and a
needle trap device; the designed devices proved useful for simple and inexpensive
screening and were robust enough for field sampling 64
Use of microwave heating for the preparation of gas standards containing mixtures of
VOCs and SVOCs; method uses a domestic microwave oven and 1 liter gas-sampling
bulbs 65

Water Analysis

Biennial review; developments in water analysis during 2001 and 2002; contents focus on
new, emerging contaminants and environmental issues 66
Methods of analysis of methyl tert-butyl ether (MTBE) and tert-butyl alcohol (TBA) in
ground and surface water samples; summarizes issues with direct aqueous injection,
headspace analysis, purge-and-trap, and solid-phase microextraction 67
Review; analysis for organic contaminants in sea water samples; includes table of analytes,
pre-treatment, analysis technique, and limit of detection 68
Brief review of methods for the determination of organochlorine compounds in wastewater
discharge samples 69
Fast, inexpensive screening method for heavy metal contamination in water samples 70
Sample screening method for benzene, toluene, ethylbenzene, and xylenes (BTEX) in
water using a headspace sampler with a mass spectrometer 71

Pesticides, Herbicides, Insecticides

Method for determining pesticides in environmental ground and surface water using solid-
phase extraction (SPE) with liquid chromatography (LC) electrospray (ESI) tandem mass
spectrometry (MS-MS) 72
Methods and instrumentation used to detect substituted urea compounds used as herbicides
and insecticides; techniques include gas chromatography, liquid chromatography (and
coupling of both to mass spectrometry detectors) and capillary electrophoresis (CE) 73
Solid-phase extraction of sulfonylurea herbicides in water and soil samples using a
molecularly imprinted polymer (MIP) 74

373
Study of pyrethroid insecticide tralomethrin and its transformation product, deltamethrin,
in gas chromatographic (GC) pesticide residue analysis; separation and identification of
compounds were possible using LC-MS 75
Determination of organophosphorus pesticides in aqueous samples by SPME and GC with
flame photometric detection (FPD) 76
Comparison of different SPME fiber coatings for the extraction and analysis of
organochlorine pesticides in groundwater; optimized methods for each fiber type were
applied to the analysis of polluted groundwater samples 77
Determination of residues of eight selected herbicides (trifluralin, butachlor, pretilachlor,
metolachlor, atrazine, acetochlor, alachlor, and fluroxypyr-meptyl) in groundwater samples
by SPME 78
Comparison of six organic solvents for the GC analysis of pesticides; study emphasized the
stability of selected pesticides in a given solvent 79

Polychlorinated & Polybrominated Compounds

Review of analytical methods for the determination of brominated flame retardants (BFRs)
with an emphasis on polybrominated diphenyl ethers (PBDEs); sample pre-treatment,
extraction, cleanup, chromatographic separation, detection methods, and quality control are
among the topics discussed 80
Application of SPME to the analysis of BFRs in water samples; method uses GC tandem
MS for quantification 81
Use of two-dimensional gas chromatography (GC x GC) to separate and identify the 209
PCBs 82
Study of the effects from solvent and temperature to the various extraction methods for
removing PCBs and polychlorinated dibenzodioxins (PCDDs) from fly ash 83
Method for the determination of polychlorinated dibenzo-p-dioxins (PCDDs),
dibenzofurans (PCDFs), and biphenyls (PCBs) using GC-MS; the use of different reagent
gases is studied 84
Speciation

Application of liquid chromatography (LC) coupled with inductively coupled plasma-mass

spectrometry (ICP-MS) in field of elemental speciation; a few key elements for speciation
(As, Se, Cd) are highlighted 85
Review of applications and instrumentation for speciation analysis; focus is on ICP-MS
and electrospray ionization mass spectrometry (ESI-MS) 86
As speciation using classical ion-exchange column chromatography; presents strategies for
separation and pre-concentration of arsenic species 87
Sb speciation problems and progress; table of Sb speciation from water, soil, and extracts
using high performance liquid chromatography (HPLC) separation 88
Review; trace metal speciation in environmental studies using sector field inductively
coupled plasma mass spectrometry (ICP-SFMS) and multicollector inductively coupled
plasma mass spectrometry (MC-ICP-MS) 89
Review of As speciation analysis using HPLC coupled to ICP-MS 90

374
Review of developments in GC-plasma interfaces for use in elemental speciation;
advantages and disadvantages of GC-plasma interfaces, types of plasmas and mass
spectrometers, and variants of plasma sources are discussed 91
Review of modern sample preparation techniques used in speciation analysis that reduce
waste generation and minimize environmental hazards 92
Comparison of extraction methods for arsenic speciation analysis; river sediment, sewage
sludge, and agricultural soil reference materials were used in the study; analyses were
completed by high-performance liquid chromatography-hydride generation-atomic
fluorescence spectroscopy 93

Field-Portable Techniques & Instrumentation

Portable capillary electrophoresis instrument prototype; basic instrument design and three
electrochemical detection methods are discussed 94
Use of portable X-ray fluorescence (PXRF) instrumentation in analysis of environmental
samples; includes tables comparing PXRF analysis of certified reference materials and
comparing performance of PXRF and laboratory ICP-AES results 95
Use of SPME for sampling environmental contaminants in air, water, and soil for analysis
by GC-MS in the field 96
Design test for the next generation of field-portable and low-cost GC-MS; the design
combined a small gas chromatograph with a compact double-focusing mass spectrometer
(CDFMS) as the detector 97
Comparison of organic vapor analyzers (OVAs) with either a flame ionization detector
(FID) or a photoionization detector (PID) to the analysis of soils contaminated with diesel
fuel 98
Development of a portable laser-induced plasma spectrometer; field results on steel-scrap
samples were compared to laboratory X-ray fluorescence (XRF) results 99
Report on prototype portable GC for use in the determination of complex vapor mixtures;
analysis was performed on a 30-vapor mixture and performance compared to indoor air
quality monitoring applications 100
Enhancement of selectivity in field-portable high-speed GC analysis for organic vapors
using a thicker film in the nonpolar column 101
Development of a battery-operated, miniature, cylindrical ion trap (CIT) mass spectrometer
that maintains laboratory-scale instrument functionality and performance 102
Use of a portable in-situ spectrophotometric analysis system for the measurement of
copper in coastal waters 103
Overview of field-portable GC-MS analytical systems and applications to environmental
and forensic analyses 104
Development of a fast gas chromatograph coupled to a time-of-flight mass spectrometer
(GC-TOFMS) for portable field use 105

Atomic Spectrometry

375
Annual review; atomic spectrometry update on chemical analysis of environmental
samples; extensive table summarizes applications by analyte, matrices (soils, plants,
sediments, etc.), and technique 106
Annual review; new developments in atomic emission (AE), atomic absorption (AA),
atomic fluorescence (AF), and related techniques 107
Annual review of novel developments and trends in atomic emission, atomic absorption,
and atomic fluorescence spectrometry 108
Annual review of trends and developments in atomic emission, absorption, and
fluorescence spectrometry 109
Review of advances in atomic emission, absorption, and fluorescence spectrometry and
related techniques 110
Biennial review of atomic spectroscopy developments published from January 2002 to
December 2003; includes AA, AF, AE, ICP-MS, and glow discharge (GD) 111
Biennial review of new developments in atomic absorption, atomic fluorescence, atomic
emission, glow discharge atomic spectrometry and inductively coupled plasma-mass
spectrometry from October 1999 to October 2001; primarily new applications and
methodology 112
Review of recent advances in the hydride-generation technique for analysis by atomic
emission spectrometry (AES) 113

Atomic Absorption Spectrometry (AAS)

Comparison of analytical performance of atom trapping systems and atomization

techniques for flame atomic absorption spectrometry (FAAS) 114
Review; developments and trends in sample pretreatment for electrothermal atomic
absorption spectrometry (ETAAS); coupling of flow injection (FI) for analyte separation
and preconcentration 115
Procedure for determining Cu, Ca, and Cr in interferents using pulsed peristaltic pumps
and Fourier transforms 116

Capillary Electrophoresis (CE)

Review of applications of capillary electrophoresis for detection and determination of

pesticides in formulations, environmental samples, and for chiral separations; includes
comparison table of detection limits for different detectors 117
Review for determining pesticide residues in environmental matrices; provides overview of
current developments and emerging techniques (CE-MS); includes analyte and sample
preparation methods table and provides comparison of CE to gas chromatography (GC)
and liquid chromatography (LC) pesticide-residue analysis techniques 118
Review; use of CE in the speciation of metal ions; includes table of metal ions and analysis
conditions 119
Developments in sample preparation for capillary electrophoresis including clean-up and
concentration methods 120
Reviews sensitivity enhancements for CE and gives several examples of water sample
analysis for both inorganic and organic analytes 121

376
Gas Chromatography (GC)

Biennial review of developments in gas chromatography including published work from

2002 and 2003, primarily; sections are divided into reviews and general interest, column
principles and technology, high-speed and portable GC, and detectors 122
Biennial review of developments in gas chromatography (articles from 2000 and 2001);
contents include high-speed and portable GC, detectors, column technology, and general
interest publications 123
Review of the use of GC in identification and quantification of environmental pollutants;
pollutant groups covered include volatile organic compounds (VOCs), polycyclic aromatic
hydrocarbons (PAHs), pesticides, and halogenated compounds 124
Two-dimensional gas chromatography (GC x GC) for separation and identification of
organic compounds in environmental samples 125
Two-dimensional gas chromatography (GC x GC) and recommended column
combinations for separating polychlorinated biphenyls (PCBs) 82
Use of two-dimensional GC coupled to time-of-flight mass spectrometry for the improved
analysis of polychlorinated biphenyl (PCB) congeners 126
Overview of the two-dimensional gas chromatographic technique 127
Data interpretation for two-dimensional gas chromatographic separations 128
Use of pressurized liquid extraction (PLE) and two-dimensional gas chromatography as a
broad screening method for PAHs in soil 129
Overview of fast GC with table of “speeding up” options and the practical aspects related
to the reduction in analysis time 130
Review; developments in coupled-column GC for the analysis of environmental toxins
such as dioxin, PCBs, and PAHs 131

Gas Chromatography-Atomic Emission Detection (GC-AED)

Brief overview of GC-AED technique including applications, performance issues, and

extended hyphenation options 132
Simultaneous determination of polychlorinated organic compounds using GC with micro-
electron capture detector (µ-ECD) and micro-atomic emission detector (µ-AED); mixtures
of organochlorine pesticides and PCBs were analyzed 133
Analysis of river sediments and sewage sludges by flash pyrolysis coupled with gas
chromatography and atomic emission detection (PyGC-AED); results from comparison
analyses made using flash pyrolysis coupled with gas chromatography and mass
spectrometry (PyGC-MS) are provided; river sediments were collected from rivers known
to be polluted by agricultural and industrial activities and sewage sludges were taken from
industrial and urban wastewater treatment plants and a lagoonal purification system 134

377
Use of GC-AED with a microwave-induced helium plasma for speciation of Hg, Sn, and
Pb compounds; includes large summary of GC-AES methods for determining inorganic
mercury and organomercury species in a variety of sample matrices 135

Gas Chromatography-Inductively Coupled Plasma-Mass Spectrometry (GC-ICP-

MS)

Review article; advances in gas chromatography (GC) coupled with inductively coupled
plasma mass spectrometry (ICP-MS) 136
Application note about the use of GC-ICP-MS for metal speciation in environmental
samples 137

Gas Chromatography-Mass Spectrometry (GC-MS)

Simultaneous determination of semi-volatile organic compounds (SVOCs) in air samples

by GC-MS; two combined disk-type filters used as adsorbents for air sampling 138
Analysis for PAHs and heavy metals in storm water and sediments using GC-MS 139
Study combining large-volume injection (LVI) to fast GC-MS in the analysis of 15
organochlorine pesticides (OCPs) in aqueous solutions; all analytes separated in less than 8
minutes 140
Review of analyses for metalworking fluids (MWFs) and hydraulic fluids (HFs) in oily
wastewater using GC/MS with “soft” ionization and two-dimensional GC techniques 141

High Performance Liquid Chromatography (HPLC), Liquid Chromatography (LC)

Review of developments in liquid chromatography equipment and instrumentation from

January 2000 through December 2001; topics include instrumentation, columns, detectors
(elemental, optical, luminescent, electrochemical, mass spectrometry, and others), and
computation 142
Glossary of terms used in HPLC 143
Determination of trimethylamine (TMA) in water samples by LC; the analyte was
derivatized in a precolumn using 9-fluorenylmethyl chloroformate (FMOC) 144
Analysis for phenols (from river and coke plant water) and herbicides (from soil samples)
by solid-phase extraction (SPE) and HPLC 145
Review of analysis for non-metals (carbon, sulfur, phosphorus, and halogens) using high
performance liquid chromatography coupled with inductively coupled plasma (HPLC-ICP)
146

Precolumn derivatization method for the determination of free amines in real water
samples (wastewater from different sampling sites) by HPLC with fluorescence detection;
the amide intermediate, 9-(2-acridone)oxyethylcarbonylimidazole (AOCD), formed from
the reaction of 9-(2-hydroxyethyl)acridone and N,N’-carbonyldiimidazole, reacts with free
amines in the presence of a base catalyst, 4-(dimethylamino)pyridine 147
Review of the use of HPLC in metal speciation (As, Se, Pb, Hg, Sn, and Cr); includes
sections on sample handling and different chromatographic modes 148

378
Ion Chromatography (IC)

Overview of use of ion chromatography (IC) for the determination of inorganic ions in
drinking water; includes table of regulatory methods and analytes 149
Basic principles, methods, and applications of ion chromatography 150
Comparison of IC detection techniques; includes table rating characteristics of each
technique 151
Approaches to sample pretreatment to overcome analysis problems from difficult matrices
152

Coupling ion chromatography with ICP-AES and ICP-MS; highlights advantages and
applications in sample preconcentration, elimination of interferences, and speciation
analysis 153

Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), Inductively

Coupled Plasma-Optical Emission Spectrometry (ICP-OES)

Review on matrix effects during ICP-AES sample analysis; addresses the effects from
easily ionized elements to the plasma and the analytical signal; includes a section on
correction methods 154
Preconcentration and determination of Cd, Hg, Ag, Ni, Co, Cu and Zn in water and
sediment samples using a chelating resin and ICP-AES 155
Determination of total metals with discrimination of chemical forms present in a sea water
matrix; use of solid-phase extraction for separation and preconcentration prior to ICP-AES
sample analysis 156
Method for studying long-term stability in ICP-AES 157

Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

Biennial review; developments in ICP-MS from October 2001 to October 2003; topics
include sample introduction, spectroscopic interferences, and isotope ratios 158
Biennial review; developments in ICP-MS from October 1999 to September 2001; several
tables with selected methods such as chemical vaporization, electrothermal vaporization
(ETV), and speciation are provided 159
Use of a modified Burgener parallel path nebulizer for vapor generation of noble and
transition metal species through reaction with tetrahydroborate 160
Comparison of on-line preconcentration columns in sequential injection analysis (SIA) for
the determination of metals in sea water (Al, As, Co, Cu, Mn, Mo, Ni, Pb and V) by ICP-
MS 161
Trace metal determination (Cr, Mn, Fe, Co, Ni and Cu) in saline water using a flow
injection on-line precipitation system coupled to ICP-MS 162
Overview of “practical aspects” of environmental analysis (measurement parameters and
analytical parameters) by ICP-MS 163
Determination of hexavalent chromium in ambient air with analysis using ICP-MS 164
Analysis for Sn in soil samples using potassium hydroxide fusion followed by continuous
hydride generation coupled to ICP-MS 165

379
Overview of the electrothermal vaporization (ETV) technique for ICP-MS 166

Infrared (IR) Spectrometry

Analytical technique for the simultaneous determination of Sb, As, and Sn in aqueous
samples; coupled flow analysis (FA) hydride generation (HG) and Fourier transform
infrared (FTIR) spectrometry system 167
Quantitative determination of various alkaline and alkaline earth metals in aqueous
solutions using Mid-FTIR spectroscopy 168
Quantitative method for the determination of ion concentrations of aqueous polyatomic
anions using attenuated total reflectance (ATR) FTIR spectroscopy 169

Liquid Chromatography-Mass Spectrometry (LC-MS)

Review of applications of liquid chromatography coupled with mass spectrometry (LC-

MS) using atmospheric pressure ionization in water analysis 170
Summary of problems using LC-MS for qualitative and quantitative analysis of organic
compounds in water 171
Determination of trace amounts of specific antibiotics in natural waters and wastewater
using SPE combined with high performance liquid chromatography-ion trap tandem mass
spectrometry (LC-MS-MS) 172
Method for the determination of halogenated and non-halogenated nonylphenols and
nonylphenol carboxylates using liquid chromatography tandem mass spectrometry in water
and sludge samples from a drinking water treatment plant 173
Summarizes sources of error in HPLC-MS analyses and suggests solutions 174
Analysis for emerging environmental contaminants using LC/TOF/MS 175
Analysis for fluorinated surfactants in spiked sludge samples using LC-MS-MS after
extraction and separation 176

Liquid-Phase Microextraction (LPME)

Developments in liquid-phase microextraction (LPME) based on disposable hollow fibers;

the technique principles, set-up, applications, and trends for the future are discussed 177
Use of LPME coupled to GC-MS to analyze for pesticides in soil samples 178
Developments in liquid-phase microextraction; includes details on some environmental
applications (polycyclic aromatic hydrocarbons, herbicides, pesticides, etc.) 179
Determination of trihalomethanes (THMs) such as chloroform, dichlorobromomethane,
chlorodibromomethane, and bromoform in drinking water samples (tap water and well
water) using headspace liquid-phase microextraction (HS-LPME) with gas
chromatography-electron capture detection (GC-ECD) 180

Microwave-Assisted Extraction (MAE) & Microwave-Enhanced Chemistry (MEC)

Overview of microwave-based devices used in solid sample pretreatment; includes both

closed and open, multi-mode and focused-microwave systems 181

380
Extraction and determination of selected endocrine disrupting chemicals (EDCs) in river
sediments by microwave-assisted extraction followed by gas chromatography mass
spectrometry (GC-MS) 182
Study of a microwave digestion technique for the analysis of metals (Ca, Mg, Fe, Mn, Zn,
Cr, Cd, Cu, Pb, and V) in sediments and soils; samples analyzed included standard
reference materials (SRMs) of sewage sludge, marine sediment, urban particulate matter,
and coal carbonization site soil 183
Review of sample extraction and digestion procedures using focused-microwave radiation;
includes tables of focused-microwave-assisted extractions of organic, inorganic, and
organometallic compounds and of focused-microwave-assisted digestions of organic and
inorganic samples 184
Use of focused-microwave (FM) irradiation to improve upon conventional Soxhlet
extraction; includes section on the use of FM-assisted Soxhlet extraction (FMASE) in the
analysis of environmental pollutants (polycyclic aromatic hydrocarbons, alkanes,
herbicides, metals, etc.) 185
Review of extraction and digestion procedures assisted by focused-microwave radiation;
applications presented include inorganic, organic, and organometallic analyses in a variety
of sample types 184
Comparison of microwave-assisted total digestion to aqua regia and nitric acid digestions
for the determination of heavy metal content in environmental samples (sediments, soils,
sludges, and plant materials) 186
Study of three microwave digestions for the determination of metals in sludge, soil, and
sediment samples; metals analysis performed by ICP-AES 187
Determination of 17 chlorophenolic compounds in ash samples obtained from different
incineration plants; a microwave system with closed extraction vessels was used in the
sample preparation 188
Digestion of organic samples using microwave-assisted sample combustion; cadmium and
copper were determined in the samples using electrothermal atomic absorption
spectrometry 189
Study of the thermal degradation of five carbamates (propoxur, thiuran, propham,
methiocarb, and chlorpropham) in microwave-assisted extraction followed by HPLC
analysis 190

Mass Spectrometry (MS)

Annual review of atomic mass spectrometry; review focuses on significant developments

in instrumentation and methodology and an improved understanding of the fundamental
phenomena of MS 191
Annual review of atomic mass spectrometry; developments in instrumentation and
methodology or fundamental principles of MS 192
Annual review of developments in atomic mass spectrometry 193
Structural and chemical characterization of compounds in complex environmental mixtures
using electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry
(ESI FT-ICR MS) 194
Brief comparison of GC-MS and LC-MS 195

381
Development of a mass spectrometer with simultaneous detection using a Faraday cup-
based detector called the focal plane camera (FPC) 196
Direct coupling of SPME with mass spectrometry to make a new analytical technique,
fiber introduction mass spectrometry (FIMS); analysis of VOCs, SVOCs, and two
herbicides using the new technique is discussed 197

Nuclear Magnetic Resonance Spectroscopy (NMR)

Use of high performance liquid chromatography coupled with nuclear magnetic resonance
spectroscopy (HPLC-NMR) in environmental analysis as a method of identifying
components of complex mixtures; references work using HPLC-NMR for the analysis of
environmental contaminants 198
Study of two techniques used for the analysis of perfluorinated surfactants in water
samples–19F NMR and LC-MS-MS; techniques complimented each other for sample
analysis and the methodology is applicable to other sample matrices 199
Use of NMR in hyphenated techniques with HPLC and MS with potential of separating
complex mixtures of pharmaceuticals or drug metabolites 200

Pressurized Fluid Extraction (PFE), Pressurized Liquid Extraction (PLE),

Accelerated Solvent Extraction (ASE)

Overview of the accelerated solvent extraction (ASE) technique for the extraction of
environmental pollutants from solid samples; presents basics of technique and comparison
to other extraction techniques 201
One-step cleanup and extraction method for the analysis of polycyclic aromatic
hydrocarbons (PAHs) using pressurized liquid extraction (PLE) 202
Study of efficiency of a pressurized liquid extraction (PLE) system for the isolation of
organic pesticides and polychlorinated biphenyls (PCBs) under varying pressure and
temperature conditions 203
Pressurized liquid extraction of veterinary antibacterial agents from soil samples followed
by SPE and LC-MS analysis 204

Solid-Phase Extraction (SPE)

Reviews use of solid-phase extraction for separation and sensitive determination of metal
ions (primarily in water samples); includes tables of on-line and off-line SPE applications
with details on matrix, trace elements, experimental conditions and methods 205
Innovative development of molecularly imprinted polymers (MIPs) for use in solid-phase
extraction (SPE) to selectively extract analytes from complicated matrices; addresses
analytes of environmental interest 206
Comparison of extraction techniques–solid-phase extraction (SPE) and solid-phase
microextraction (SPME)–in the analysis for short-chain chlorinated paraffins (SCCPs) in
tap and river water samples using GC coupled to negative chemical ionization mass
spectrometry (GC-NCI-MS) 207

382
Sample clean-up and separation by sequential solid-phase extraction (SSPE) for analysis of
polar pollutants in water samples; analyses of samples from wastewater treatment plants
(WWTPs), rivers, and streams were performed using LC-ESI-MS 208
Comparison of SPE materials for the removal of polar compounds from spiked water
samples; phenolic compounds and organochlorine pesticides were studied 209

Solid-Phase Microextraction (SPME)

General overview of SPME technique 210

Comparison of the extraction efficiencies of five different SPME fiber coatings in the
analysis of 52 pesticides and PCBs 211
Derivatization and SPME of organotin and organolead compounds in aqueous samples
with analysis by gas chromatography atomic emission detection (GC-AED); derivatization
is carried out in situ using sodium tetrapropylborate 212
Rapid procedure for determining butyltin species in sediments by SPME; analysis was
performed on a certified reference material (CRM-462) and coastal sediment samples 213
Direct headspace SPME method for the determination of polynuclear aromatic
hydrocarbons (PAHs) in atmospheric particulate matter; results showed potential for using
method as a screening tool 214
Simple and fast procedure for the analysis of aldehydes in water using SPME technique
with on-fiber derivatization; quality of results were evaluated using spiked bidistilled
water, chlorinated tap water, and well water 215
Determination of tributyltin (TBT) in water and sediment by automated in-tube SPME and
HPLC coupled to a quadropole mass spectrometer with electrospray ionization 216
Use of SPME and GC-MS to characterize odorant emissions from a landfill; demonstrated
use as an on-site analysis tool 217
Comparison of SPME with stir bar sorptive extraction (SBSE) in the extraction of semi-
volatile compounds (polycyclic aromatic hydrocarbons, organochlorines) in water; post-
extraction analysis was performed using GC-MS 218
Analysis for BTEX in water samples using headspace solid-phase microextraction (HS-
SPME) with GC-FID 219

X-ray Spectrometry (XRS)

Review of developments and improvements in X-ray spectrometry published during 2002

and 2003 220
Annual review of X-ray fluorescence (XRF); developments during 2002 and 2003 in
instrumentation and detectors, trends in analysis, and a range of applications including
environmental 221
Annual review of developments in instrumentation and applications of X-ray fluorescence
including environmental applications 222
Annual review; developments during 2000 and 2001 in X-ray fluorescence; contents
include instrumentation and detectors, optics, portable and mobile XRF, and applications
of XRF 223

383
Biennial review of developments in XRS and related fields (from late 1999 to the end of
2001); topics include those of detection, instrumentation and optics, and several
applications 224
On-line preconcentration flow system for the simultaneous determination of Co, Cu, Mn,
Ni, Pb and Zn by total reflection X-ray fluorescence (TXRF) spectrometry; improvements
in detection limits; system was applied to river water samples 225

SPECIAL TOPIC – ENDOCRINE DISRUPTING COMPOUNDS (EDCS)

Although not a consideration for the environmental crime field at this time, concern over
endocrine disrupting compounds (EDCs–also known as “endocrine disrupting chemicals”)
in the environment has been increasing. Endocrine disruptors have been defined as
“exogenous agents that interfere with the production, release, transport, metabolism,
binding, action, or elimination of the natural hormones in the body responsible for the
maintenance of homeostasis and the regulation of developmental processes.” 226 Research
to identify compounds that may interfere with hormonally-controlled body systems has
been increasing for both governmental and private research entities.

Currently, the USEPA is developing methods for the screening and testing of thousands of
contaminants with the potential to disrupt the endocrine system. 227 USEPA, as tasked by
the Federal Food, Drug and Cosmetic Act (FFDCA), developed the Endocrine Disruptor
Screening Program (EDSP) to “screen pesticide chemicals and environmental
contaminants for their potential to affect the endocrine systems of humans and wildlife.”
228
When complete, the EDSP will provide validated methods for screening drinking water
sources for EDCs.

Several other countries have taken steps to define the EDC problem and pursue solutions.
The United Kingdom Environment Agency has presented a position on phamaceuticals in
watercourses (prioritizing some of these pharmaceuticals for monitoring) and a strategy
paper on EDCs in the environment. 229, 230 Environment Canada also has a national
strategy regarding endocrine disruptors in the environment. 231

The Australian Government Department of the Environment and Heritage has made
available an EDC information paper wherein parties “agreed on the need to investigate, in
depth, the human, environmental and ecotoxicological aspects of endocrine disrupting
substances.” 232 Deustche Forschungsgemeinschaft (DFG) has established research
training group 546 for the “elimination of endocrine-disrupting substances from waste
water.” 233

The Japan Environment Agency has summarized on-line the plans for investigations,
research, testing, and method development for SPEED ’98–Strategic Programs on
Environmental Endocrine Disruptors ’98. 234 The Danish Environmental Protection
Agency has provided on-line an “Evaluation of Analytical Chemical Methods for the

384
Detection of Estrogens in the Environment.” This document provides environmental and
chemical properties of estrogens, analytical methods and applications to estrogens, and
recommendations. The document also contains active links to tables and numerous
references. 235

METHODS FOR THE IDENTIFICATION OF ENDOCRINE DISRUPTORS

Pharmaceutically Active Compounds

(antibiotics, anti-inflammatories, antibacterial agents, etc.)

Investigates the presence of sulfadimidine (sulfamethazine), an antibiotic used for animals,

in liquid manure and soil samples; surface water samples from river banks were extracted
and analyzed by LC–MS/MS for more than 20 antibiotics used in both animal and human
therapy 236
Review of pharmaceutical antibiotic compounds in soils with an extensive section on fate
studies 237
Analysis for the nonsteroidal anti-inflammatory drugs (NSAIDs) ibuprofen and 2-(4-
chlorophenoxy)-2-methylpropionic acid in wastewater; method used reversed-phase high
performance liquid chromatography (RP–HPLC) combined with a simple, fast, and
inexpensive two-step liquid-liquid-liquid microextraction (LLLME) 238
Analysis for NSAIDs in water samples using solid phase microextraction (SPME), on-fiber
silylation (derivatization), and GC/MS determination; the SPME method was compared to
the use of solid phase extraction (SPE) for analysis of ibuprofen and naproxen in the
influent and effluent from a sewage water treatment plant 239
Method for the determination of the fluoroquinolines ciprofloxacin and norfloxacin
(antibacterial agents) in sewage sludge and sludge-treated soil samples; samples were
extracted using accelerated solvent extraction (ASE); extracts were cleaned using SPE and
analyzed by liquid chromatography fluorescence detection (LC-FLD) 240
Extracts from sewage treatment plant wastewater and from surface water were analyzed for
carbamazepine (a drug used in the treatment of epilepsy, schizophrenia, bipolar disorders
and more) and five metabolites of carbamazepine using electrospray LC-MS/MS with
selected reaction monitoring 241
Determination of clofibric acid using acid and base/neutral liquid-liquid extraction,
derivatization with trimethylsilyldiazomethane (TMSD) and analysis by GC/MS 242
Analysis for polar pharmaceuticals by LC-MS without derivatization; samples of river
sediment were spiked with standards and prepared by ultrasonicated solvent extraction and
solid phase extraction (SPE) prior to analysis 243
Simultaneous determination of acidic and neutral pharmaceuticals in wastewater using
high-performance liquid chromatography photochemically induced fluorimetry (HPLC-
PIF) providing a clean, fast and inexpensive on-line post-column photoderivatization
procedure; SPE clean-up was used on the sewage water sample 244
Analysis for nine neutral pharmaceuticals in river water and wastewater samples (influent
and effluent from municipal sewage treatment plants) by liquid chromatography
electrospray tandem mass spectrometry (LC–ES–MS–MS) with SPE enrichment 245

385
Details six different analytical methods that (when totaled) allow for the analysis of nearly
80 pharmaceutical compounds and phenolic antiseptics 246
Brief report on proficiency test results for pharmaceuticals in river water and wastewater;
both GC/MS and LC-MS/MS methods were used by participants for the analyses 247

Pharmaceutical and Personal Care Products (PPCPs)

Study of the removal of selected pharmaceutical and personal care products (PPCPs)
through wastewater treatment processes; includes results from analyses of sewage
treatment works influent and effluent samples and the methodology used in analyzing for
five different groups of PPCPs 248
Method for detection of PPCPs that have a structure conducive to fluorescence using
capillary zone electrophoresis - laser induced fluorescence (CE-LIF); the determination of
salicylic acid in sewage effluent is presented 249
Review of investigations of musk residues in sewage, sewage sludge, surface water,
aquatic sediment, and biota 250

Steroid Hormones

Analysis for steroid hormones (gestagens, androgens, and estrogens) in drinking water and
groundwater; samples were extracted (SPE) and derivatized prior to GC/MS analysis in
selected ion monitoring (SIM) mode 251
Quantitation of estrogens in groundwater samples and swine lagoon samples; extracts were
derivatized with pentafluorobenzyl bromide (PFBBR) and N-trimethyl-silylimidazole
(TMSI) then analyzed using negative ion chemical ionization (NICI) gas chromatography
tandem mass spectrometry (GC-MS-MS) 252
Analysis for estrogens in surface water and wastewater treatment plant samples; samples
were extracted using SPE, derivatized using PFPA (pentafluoropropionic acid anhydride),
and analyzed by GC/MS 253
SPE-GC-MS method for the analysis of steroids and phenolic compounds in water
samples; changes in the method parameters were made to test the effects on the recovery of
the endocrine disrupting compounds (EDCs); parameters included different types of SPE
cartridges, elution solvent, salt concentration, pH, and humic acid concentration 254
Analysis of sewage treatment plant influent, effluent and river water for selected estrogens,
phytoestrogens, mycoestrogens and alkylphenols by LC-MS-MS; optimization of
instrument conditions for the EDC groups is detailed including results from electrospray
ionization (ESI) and atmospheric pressure chemical ionization (APCI) modes, negative ion
(NI) and positive ion (PI) modes, and mobile phase compositions 255
Determination of chlorinated and brominated derivatives of alkylphenol ethoxylate
(APEO) surfactants (industrial cleaning agents that mimic endogenous hormones) in
sludges, waters and sediments; extracts from samples were analyzed using reversed phase
LC/MS with a comparison of APCI and ESI interfaces 256
Analysis for steroid hormones in wastewater treatment plant (WWTP) effluent using liquid
chromatography tandem mass spectrometry (LC-MS-MS); samples were extracted by SPE
and cleaned with a liquid-liquid separation followed by a Florisil cartridge 257

386
Presents several methodologies for separation and analysis of steroid estrogens in sludge,
sediment, sewage effluent and surface water; details on the methods are summarized in a
flowchart and table; biological methods for determining the endocrine-disrupting activity
of a chemical are also discussed 258

General EDC Analytical Methods

Analysis of samples from 139 streams for pharmaceuticals, hormones, and other organic
wastewater contaminants using targeted methods and selected ion monitoring (SIM) for
improved sensitivity 259
Use of a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for
analysis of pharmaceuticals, steroids, and personal care products; method used one solid-
phase extraction (SPE) procedure and ESI (in positive and negative modes) and APCI (in
positive mode) 260
Comparison of separatory funnel liquid-liquid extraction to on-line continuous liquid-
liquid extraction in the analysis of several EDCs in water samples; data was collected in
both total ion chromatogram (TIC) mode and selective ion monitoring (SIM) mode of
GC/MS 261
Evaluation of matrix effects on 35 endocrine disrupting chemicals for the analysis of
environmental water samples by LC-ESI-MS/MS; efficient sample clean-up and the use of
internal standards showed reduced matrix effects regardless of the type of environmental
water sample (surface water, rain water, groundwater, channel water, wastewater treatment
plant effluents and industrial effluents) 262

387
 Appendix A

MAJOR ENVIRONMENTAL LAWS OF THE UNITED STATES

ENVIRONMENTAL PROTECTION AGENCY (USEPA)

Environmental Law Summary

Federal Food, Drug, and Set safety and quality requirements for food, cosmetics,
Cosmetic Act (FFDCA) drugs and therapeutic devices. Allows EPA to establish
safe tolerance levels for pesticide chemical residues
present in raw or processed foods. 263

Federal Insecticide, Provided federal control of pesticide distribution, sale,

Fungicide, and and use. EPA was given authority to study the results of
Rodenticide Act pesticide use and to require users to register when
(FIFRA) purchasing pesticides. 264,265

Federal Water Pollution Established the basic structure for regulating discharges
Control Act a.k.a. Clean of pollutants into the waters of the United States and set
Water Act (CWA) water quality standards for all contaminants in surface
waters. Gave EPA the authority to implement pollution
control programs. 266, 267

Clean Air Act (CAA) The comprehensive federal law that regulates air
emissions from area, stationary, and mobile sources.
EPA was authorized to establish National Ambient Air
Quality Standards to protect public health and the
environment. 268, 269

National Environmental Early environmental law that established a broad national

Policy Act (NEPA) framework for protecting our environment by requiring
that all branches of government consider the
environmental impact prior to undertaking any major
federal action that might significantly affect the
environment. Environmental Assessments and
Environmental Impact Statements are required when
airports, buildings, military complexes, highways, park
land purchases, and other federal activities are proposed.
270, 271

Safe Drinking Water Act Established to protect the quality of drinking water and
(SDWA) focused on all waters actually or potentially designed for
drinking use (above ground or underground sources). 272

Toxic Substances Gave EPA the ability to track the 75,000 industrial
Control Act (TSCA) chemicals currently produced or imported into the United
States. EPA repeatedly screens these chemicals, can

388
Environmental Law Summary
require reporting or testing of potentially hazardous
chemicals and can ban the manufacture and import of
chemicals that pose an unreasonable risk. Mechanisms
also exist to track newly developed chemicals with
unknown or dangerous characteristics. 273-275

Resource Conservation RCRA (pronounced "RICK-rah") gave EPA the authority

and Recovery Act to control hazardous waste from the "cradle-to-grave"
(RCRA) and included the generation, transportation, treatment,
storage, and disposal of hazardous waste. The tracking
of hazardous waste through this act only involves active
and future facilities. A framework for the management
of non-hazardous wastes was also established with this
act. 276, 277

Comprehensive CERCLA (pronounced “SIR-cla”) created a tax on

Environmental chemical and petroleum industries and provided broad
Response, Federal authority to respond directly to releases or
Compensation, and threatened releases of hazardous substances to the
Liability Act (CERCLA environment. The tax went to a trust fund, the
or Superfund) “Superfund,” for paying the costs of cleaning up
abandoned or uncontrolled hazardous waste sites as well
as accidents, spills and emergency releases of pollutants.
Through CERCLA, EPA was authorized to identify
parties responsible for any type of release and enjoin
their participation in the cleanup or recover costs
involved in the cleanup. 278-280

Superfund Amendments Amended CERCLA to increase State involvement,

and Reauthorization Act increase the size of the trust fund, increase focus on
(SARA) human health problems and revise the Hazard Ranking
System to accurately assess the relative degree of risk to
human health and the environment from uncontrolled
hazardous waste sites. 280-282

Emergency Planning As part of SARA, EPCRA was enacted to help local

and Community Right- communities protect public health, safety, and the
To-Know Act (EPCRA) environment from chemical hazards. Each state was
required to appoint a State Emergency Response
Commission, divide the states into Emergency Planning
Districts and name a Local Emergency Planning
Committee for each district. 283, 284

Pollution Prevention Act Focused industry, government, and public attention on

(PPA) reducing pollution through cost-effective changes in

389
Environmental Law Summary
production, operation, and raw materials use. Efforts to
reduce pollution prior to the need for treatment or
disposal are referred to as “source reduction.” Pollution
prevention also includes conservation and practices that
increase efficiency in the use of energy, water, or other
natural resources. 285, 286

Oil Pollution Act (OPA) Required oil storage facilities and vessels to submit plans
detailing how they will respond to large discharges,
established a tax on oil to finance a trust fund for spill
cleanup costs, and required the development of
contingency plans for oil spill response. EPA published
regulations dealing with above ground oil storage
facilities. 287, 288

Endangered Species Act Provided a program for the conservation of threatened

(ESA) and endangered plants and animals and their habitats.
EPA approval to register a pesticide is based in part on
the risk of adverse effects on endangered species and
habitats. Under FIFRA, EPA can issue emergency
suspensions of certain pesticides (cancel or restrict the
use) if an endangered species will be adversely affected.
289, 290

390
 Appendix B

USGS NATIONAL WATER QUALITY LABORATORY METHODS OF

ANALYSIS

Water-Resources Title
Investigations (WRI)
Report Number
2003-4293 Determination of Organochlorine Pesticides and
Polychlorinated Biphenyls in Bottom and Suspended
Sediment by Gas Chromatography with Electron-
Capture Detection 291

2003-4174 Evaluation of Alkaline Persulfate Digestion as an

Alternative to Kjeldahl Digestion for Determination
of Total and Dissolved Nitrogen and Phosphorus in
Water 292

2003-4139 Determination of Organophosphate Pesticides in

Whole Water by Continuous Liquid-Liquid
Extraction and Capillary-Column Gas
Chromatography with Flame Photometric Detection
293

2003-4079 Determination of Gasoline Oxygenates, Selected

Degradates, and BTEX in Water by Heated Purge
and Trap/Gas Chromatography/Mass Spectrometry
294

2002-4222 Determination of Organophosphate Pesticides in

Bottom Sediment by Gas Chromatography with
Flame Photometric Detection 295

2002-4144 Arsenic Speciation in Natural-Water Samples Using

Laboratory and Field Methods 296

2002-4071 Determination of Organophosphate Pesticides in

Filtered Water by Gas Chromatography with Flame
Photometric Detection 297

2001-4186 Determination of Wastewater Compounds by

Polystyrene-Divinylbenzene Solid-Phase Extraction
and Capillary-Column Gas Chromatography/Mass
Spectrometry 298

2001-4134 Determination of Pesticides in Water by Graphitized

391
Water-Resources Title
Investigations (WRI)
Report Number
Carbon-Based Solid-Phase Extraction and High-
Performance Liquid Chromatography/Mass
299
Spectrometry

2001-4132 Determination of Organic Plus Inorganic Mercury in

Filtered and Unfiltered Natural Water with Cold
Vapor–Atomic Fluorescence Spectrometry 300

2001-4098 Determination of Moderate-Use Pesticides and

Selected Degradates in Water by C-18 Solid-Phase
Extraction and Gas Chromatography/Mass
Spectrometry 301

Methods can be purchased from the USGS through the “Publications Warehouse”
on the USGS website. 302

392
MEDIA EVIDENCE

393
 QUESTIONED DOCUMENTS

— A Review: 2001 to 2004 —

Nils Angstrom
Statens kriminaltekniska laboratorium/Swedish National Laboratory of Forensic
Science
Dokumentenheten/Document Department
SE-581 94 Linkoping
Sweden

Phone: +46 13 241440

Fax +46 13 241822
dok@skl.police.se

394
INTRODUCTION:

This review is about what has been published in different journals and proceedings
during 2001-2003 in the field of document examinations.

The review is based upon

1. articles published in some major forensic science journals and on a number of

papers presented at different meetings regarding handwriting and document
examinations.

2. a questionnaire sent out by e-mail to laboratories active within the ENFSI

subgroup EDEWG. The same questionnaire has also been distributed through
INTERPOL to the member countries. See annex.

The frequency of response to the questionnaire has been quite low. Answers came above
all from European laboratories. Therefore the review is based mainly upon what has been
found in the journals and in proceedings from different meetings.

The following INTERPOL Member States provided information via the questionnaire:

Colombia, Czech Republic, Denmark, Estonia, Finland, France, Germany, Georgia,

Hungary, Israel, Japan, Latvia, Lithuania, Mexico, the Netherlands, Norway, Northern
Ireland, Poland, Scotland, Slovakia, Spain, Sweden, Switzerland (various services) and
Turkey.

Sources of references

As noted by Dr Pfefferli in the previous review there are not many forensic science
journals of today which regularly publish articles on questioned document examinations.
The regular printed sources today seems only to be two:

Journal of the American Society of Questioned Document Examiners (in English), and
Mannheimer Hefte für Schriftvergleichung (in German). Both publications cover
handwriting as well as questioned documents.

In Journal of Forensic Science, Science & Justice and Forensic Science International
occasional articles are published. The University of Wrocław publishes a series called
DOCUMENT – Various Specifications where some articles on questioned document
examinations can be found.

Document examiners interested in security printing and related topics can find much
information in e.g. Intergraphs journal Infosecura and in Keesing´s new magazine Journal
of Documents.

395
Otherwise the main sources regarding questioned document examinations are reports
presented at different meetings such as

The Annual ASQDE Meeting (American Society of Questioned Document Examiners)

The Biennial GFS Conference (Gesellschaft für Shriftvergleichung)
The Triennial EAFS Conference (European Academy of Forensic Science)
The Biennial Conferences organised by the University of Wrocław
The Triennial IAFS Conference (International Association of Forensic Science)
The Annual EDEWG meetings (European Document Experts Working Group)

Of great interest for document examiners are the Interpol conferences every 5th year on
Currency Counterfeiting and Fraudulent Travel Documents and the IFC (International
Fraud Conference). Also conferences organised by various organisations of the security
printing industry are of interest to the document examiner. One example is the
conferences organised by Intergraf every 18th month.

Document examinations

The review shows that the ongoing research and development within the field of
document examinations is done more or less individually and not on internationally
organised bases. Organisations like ASQDE and the different working groups of ENFSI
could form such a basis and be able to co-ordinate efforts in research in topics such as
classifying modern printers, age determination of ball point pen inks, the sequence of
crossing lines etc. Areas where no definite techniques have been established yet.

In the following individually performed studies are discussed. The categories listed below
are considered:

• Improvement in technical equipment

• Ink analysis
• Documents produced by office machines
• Determining the sequence of crossing lines
• Security printing and security documents

Improvement in technical equipment dedicated to document examination

The findings in a document examination are very much dependent upon advanced
equipment mainly from the optics industry since most of the examinations have to be
non-destructive. The following paragraphs are based on company brochures and on
information found on different web-sites.

Video spectral comparators

During the years 2001-2003 the different producers of equipment for optical
examinations have introduced more and more advanced models partly due to the sharp
competition between the makers, partly because of the introduction of new types of

396
security features in security documents. To be mentioned is the introduction of so called
anti-stoke inks and inks fluorescing under middle range UV light (313nm).

The three main producers of video spectral comparators are Foster & Freeman in UK,
Projectina and CES in Switzerland. There are of course other brands but not so well
known. All three have computerised their different optical instrumentation in order to
facilitate examinations and to extend the examining possibilities. This means they are
moving from analogue to digital imaging with increased resolution and that the soft
wares offered are dedicated to document examinations. It also means that it is possible
for certain of the more advanced models to automate routine examinations. The software
is a mixture of image processing and database handling programmes. Of course it is also
possible to run commercial standard programmes like Photoshop. The prices are in the
range of up to about 100000 Euro which means that small laboratories and organisations
with limited resources will have difficulty in affording this kind of expensive equipment.

Drexler and Smith (25) propose a simple piece of equipment with an affordable price.
The equipment is based upon a standard home camcorder as sensor and a slide projector
as light source together with some appropriate optical filters. This simple arrangement
can execute some of the tasks performed by much more expensive equipment.

Microscopes

In general stereo microscopes are gradually optically improved with reduced distortion,
enhanced viewing due to improved lens coatings, longer zoom ranges etc. Relatively new
on the market is the Leica MZ FL III stereo microscope for imaging visible UV-
fluorescence. The microscope has third beam path for the exitation light which becomes
coaxial through the zoom optics. With this construction the viewing is undisturbed by the
excitation light.

Electrostatic development

Electrostatical development of indented writing still is an important technique for the

document examiner both for screening and closer inspection of indented writing. The
ESDA from Foster & Freeman has been upgraded and now accepts A3 format and is now
called ESDA². The traditional methods of applying the toner can still be used. As a
compliment F&F has introduced a small pad containing the toner which is wiped over the
plastic surface giving cleaner operation of the equipment.

Ink analysis

Compositional analyses

Ink analysis can be performed chemically or optically. Many articles deal with chemical
methods which are destructive. With the introduction of Raman spectroscopy the number
of articles on optical analysis have increased. Non-destructive techniques are preferable.

397
Hand written documents are often stored under different light conditions which will
affect the ballpoint pen ink.

Andrasko (3) describes a method for comparing ink entries on documents stored under
different light conditions. The inks were analysed with high pressure liquid
chromatography (HPLC) and it was demonstrated that significant compositional changes
in the inks occurred on exposure to light. Andrasko (4) also demonstrated with HPLC
similar compositional changes for inks stored in darkness.

With an imaging system consisting of liquid crystal tunable filters and a forensic light
source Ibrahim (45) could differentiate seven inks that could not be discriminated easily
and effectively using conventional spectral imaging means. Chemical analysis afterwards
corroborated the result.

Grim et al (38) shows that the composition of an ink can be determined at molecular level
by fast atom bombardment and laser desorption mass spectrometry (LDMS). The results
also indicated that LDMS can be used to determine the relative age of ink.

Some years ago Foster & Freeman introduced Raman spectroscopy to document
examiners. It is an in-situ non-destructive technique for ink comparison. Background
fluorescence is posing a problem because it can obliterate the weak scattered light signals
from a sample. White (122) reports that the use of poly(L-lysine) and a colloid enhances
(SERRS) the spectra and is virtually non-destructive. Fabiañska (31) has studied the
influence of the paper when examining ballpoint pen inks with Raman spectroscopy.

Raman spectroscopy is particularly valuable in examinations of antiquities where it is an

absolute demand that the examination is non-destructive. Chaplin et al (19) have
examined Hawaiian Missionary Stamps kept at the British Library and compared them
with stamps reproduced in 1985. They conclude that Raman spectrometry is useful for
discriminating between authentic material and contemporary forgeries and reproductions.

Martin and Lyter (71) have tested microspectrometry in examining 8 black gel inks over
the full spectral range and also 2 blue gel inks. The results of these examinations indicate
the ability to differentiate, to varying degrees, the black gel inks, and consistency exists
between those inks of common manufacture (blue and black).

Jones and Wolstenholme (51) conclude that the introduction of gel inks which are not
extractable, precludes the use of TLC and dispersive IR. Instead infrared attenuated total
reflectance (IR-ATR), Raman and surface enhanced resonance Raman spectroscopy
(SERRS) were used to examine a number of black and blue ballpoint pen inks and gel
pen inks. The spectra obtained by IR-ATR, Raman and SERRS show that each technique
provides a viable method of differentiation by non-destructive means.

Dating of inks

398
In forensic examinations of documents the legitimacy of the age of an ink entry is often
an essential problem.

In a paper Lindblom (63) discusses the problems of the relative dating of inks and gives
consideration for example to inconsistent application of testing techniques and the
inappropriate use of methodology. He presents several cases where for instance the result
is contradicted by factual information.

Weyermann et al (120) have used Matrix Assisted Laser Desorption Ionisation (MALDI)
and Laser Desorption Ionisation (LDI)-MS) to study the ageing process of ballpoint pen
inks of various types. The ageing experiments show a strong correlation of dye
degradation to the duration of light exposure, which is not observed for exposure to heat.
For natural ageing, differences are observed depending on paper location, seasons and
days due to the fact of different light influences. Ink solvents vaporized rapidly at room
temperature and can´t be detected anymore after a relative short time. The authors
conclude that the state of the art of dye and solvent analysis allows to determine the
approximate age of an ink entry, if both the exact storage and the initial composition of
the ink are known and if the ageing process is still going on.

Lociciro et al (65) have studied the ageing dynamic of some inks with the aim of
knowing if it is truly possible or not to date them. They end up with opposite conclusion
compared to Weyermann et al. The selected approach measures the disappearance of the
volatile component (phenoxyethanol) as a function of time. Ink degradation is a result of
a complex superposition of various processes. The natural ageing of paper has its
importance as well as the ink composition and its capacity to produce chemical reactions
with the vehicle. The chemical reactions are strongly influenced by the environment and
the conditions of conservation which most often are not known. The results obtained
according to the definite protocol are such, according to the group, “that it is impossible
for us to date ballpoint pen inks in view of its application in documents casework”.

Contrary to Lociciro et al Andrasko (5) considers it possible to use the content of

phenoxyethanol as an indicator of the age of an ink but one must be aware of storage
conditions, contamination from fresh ink and so forth.

The debate and the research regarding the possibilities to accurately date ballpoint pen
ink entries will surely continue and new ideas will be tested. To this author ink dating
should be avoided in routine case work.

In the field of document examination it has been assumed that ink does not age whilst
inside a pen cartridge. A study by Grim et al (40) shows that this assumption may not be
entirely true

Documents produced by office machines

Dr Pfefferli in the review for 13th Symposium stated that ”the proliferating market of
modern business technology such as copiers, fax machines and printers reduces a

399
systematic approach.”. This statement still holds and one can even say that it is more
appropriate today than three years ago. However, a number of projects are reported in
different fields.

The different fields listed by Dr Pfefferli are with some exceptions still valid and some
deserves to be repeated here:

• Detection of laser printer and ink-jet printer defects for printer identification
• Evidential value from ink-jet printers and inks
• Identifying photocopying toners using different analysis techniques
• Classification of ink-jet printers and ink
• Classification of and identification of laser printers and copiers
• Examination of faxed documents
• Classification of full colour copiers
• Counterfeit Protection System codes of laser colour copiers
• Dot patterns of colour ink-jet printers

Szymanski (107) reports that the Haas Typewriter Atlas and Bouffard´s Typewriter
Classification program now are available on CD.

Lindblom et al (64) reports in a study that considerable changes in size were observed
between originals and faxed copies, between separate pages of multi page facsimile
transmissions and within individual faxed documents. Document examiners should be
aware of these facts when inspecting faxed documents. But it must be remembered that
certain fax machines have a function which automatically reduces the size of the
transmitted document. This function can be turned off.

In a case report by Parker (91) regarding anonymous letters it is described how it was
possible to attribute print flaws in the letters to a certain inkjet printer which had a
mechanical fault which caused smearing of the ink.

Gramatyka and Brodziak (37) describes the sources of individual identification features
of different types of printers connected to computers.

In a set of three articles Merrill and colleagues (76,29,28) at the FBI Counterterrorism
and Forensic Science Research Unit in Quantico reports about the building up of an
infrared spectral library of toners for printers and copiers. The library contains 807 toner
samples and can be used for screening purposes. As a test 20 photocopied documents,
each of which was paired to a test document, were compared in order to determine
whether the pair could have been produced by the same copier or not. The results
obtained were 100% correct. Tests on 30 samples using the spectral library generated
90% first hits for the correct group. Different statistical tests were performed on the
material.

According to Chopra and Sehgal (22) energy dispersive X-ray (EDXA) analysis has
proved to offer a high degree of discrimination. Together with FTIR EDXA can be

400
recommended as a means of providing reliable identification of inorganic elements and
polymers in toners. Lyter (66) also works with X-rays but with the purpose to determine
the age. He uses X-ray photoelectron Spectroscopy for the characterization of toners.
There is difference between carbon in graphite and carbon contained in polymeric
materials. He reports some success and promises a more comprehensive study.

Having studied more than 200 ink samples for ink-jet printers with micro-raman and UV-
vis spectrophotometry, Savioli et al (99) concludes that with two techniques it is possible
to differentiate and identify printer models and ink cartridges. The study will be enlarged
with the aim of building a database of ink-jet inks.

Determining the sequence of crossed lines

Determining the sequence between entries on a document is often crucial to an

investigation and much effort has been put in to do so and to find methods which are
reliable and simple to use.

Setz et al (102) have found that it is possible to determine the sequence between
electrostatically produced lines and lines from ballpoint pen inks even when there are no
line crossings. They assume the fact that laser printers to a greater or lesser extent scatter
toner particles all over the substrate. In some instances toner particles are found in the ink
lines and with bright field microscopy it was possible to determine if a toner particle was
on top of the ink line or if it was beneath it.

Aginsky (2) reports about a case where it was possible to determine the sequence
between laser print and ballpoint pen script in a document using the technique outlined by
Setz et al.

Although not a standard instrument for document examiners Kasas et al (54) have in a
study investigated the feasibility of using a particular type of scanning probe microscope,
the atomic force microscope (AFM) to examine line crossings. The results indicate that
AFM images provide the same qualitative information as scanning electron microscopy
(SEM).

Light microscopy and SEM are common techniques to determine the sequence of
crossing lines. Berx (10) and together with De Kinder (11) shows that measuring the
topographpy of the surface with a laser profilometer can provide additional information
about the sequence and that laser profilometry seems to be a promising technique. Micro-
Raman spectroscopy is reported by Savioli et al (100) as a new tool for the examination
of crossing lines. In this aspect this adds one more tool to the document examiner´s
toolbox. The Giles (35) confirms the findings concerning the use of Raman spectroscopy.

Security printing and security documents

Document laboratories involved in security printing and security documents do not find
much of interest in the forensic science journals or in the few journals specialising in

401
publishing articles on document examination. To be able to follow what is going on
regarding security documents there has not until recently been much published. However
last year a new journal, Journal of Documents, from the Dutch publishing house Keesing
was introduced. The journal deals with all aspects of document security, presents trends
and novelties regarding document security. Often articles in Journal of Documents
present new types of security features, new documents, new production techniques etc.
For instance reports van Renesse (93) in No 2, 2003, on laser technology to protect
passport photographs. Schell (101) reports about security foils on banknotes, passports,
visas etc and discusses the bonding between foil and paper and how the foil is applied to
paper.

In one of the forensic journals Ware (117) discusses a new thermochromic ink and its use
as an easy controllable security feature on for instance checks.

Another source is Infosecura published by the security printers´s organisation Intergraf.

In ”How Secure are Modern Passport Personalisation Techniques?” in Infosecura

Angstrom and Mattsson (6) discusses the relatively recent use of techniques for passport
issuance which is easily simulated by forgers. There is a trend in the industry and among
passport authorities to use laser and ink-jet printer technology for the personalization of
passports. Although protected by different types of transparent foils it does not prevent
the forger to use the same printing technique using simple office equipment. The result of
the forgery will be as good as the genuine result.

The production of security documents is not completely homogenous. There will always
be small variations within an edition and between editions of a certain document whether
it is a banknote, a passport or some other printed matter. There is “grey zone” which the
document examiner must be aware of when authenticating a document. Ross (95)
reminds us that this grey area includes quality-control issues in the production and that it
is important to understand and identify these issues when authenticating documents.

Since much of what the security printing industry does is not apt for publication, it is
necessary to take part in different conferences aimed at security printing. To be named
are the conferences organised by Intergraf every 18th month and the Pyrabelisk
conferences. When it comes to fraud of identity documents the International Fraud
Conference is of interest like the great conference on counterfeited banknotes and
fraudulent documents organised by Interpol every 5th year with intermediate smaller
conferences on the same topics. What is said at those conferences are normally not
published because of the confidential nature of the material.

Miscellaneous

Examinations using electrostatical development still attracts many writers. In a study

devised by Kullman et al (58) it is reported that it is possible to discriminate between
original impressions and traced impressions. Small misalignments occur in the traced
impressions.

402
Barton and Walker (7) discusses the question how to differentiate secondary impressions
from indentations in ESDA examinations. Although rare, document examiners should be
aware of them.

La Porte (60) discusses the possibilities to use the ESDA for identification of class
characteristics of different printers and copiers.

Electrostatic development of indented writing is not always successful. The reason for
this can be for instance the wrong type of paper. A novel technique is presented by
Koeijer (56). The method presented uses black gelatine lifter slabs that are normally used
to lift fingerprints.

ESDA films are often blurred and difficult to evaluate. With the use of the digital
enhancement possibilities offered in computer programmes like Photoshop Sperry and
Tolliver (104) performed a study which showed that legibility and decipherment of
impressions developed on the ESDA films could be significantly improved in this way.

Many document examiners work for long times with the ESDA and the equivalent
machine from Projectina, both producing ozone. A study by Cameron (16) shows that
under certain conditions the ozone levels can raise above what is permitted by health
administrations. He also points out that it is relatively simple to reduce the exposure to
ozone.

With a view to polish legislation Zienkiewicz (125) discusses the question what can be
considered a valid document under different regulations.

Quality assurance and networking

Very few questioned document laboratories, mainly European, report that they are part of
accredited services along the guidelines set out in ISO 17025. Some laboratories are
preparing their organisations in order to get accreditation. One problem will be to find
assessors because the documentation is in the national language. Instead most
laboratories work with internal quality assurance activities and regulations. There is a
common agreement that quality management is important and that the importance is
increasing. Quality management is time consuming and costs money but managed in the
right way it is worth the expenses because it gives stability to the routines within the
laboratory.

One way of checking quality is to take part in different proficiency testing programmes
commercially available like those from CTS (Collaborative Testing Service, USA). Many
laboratories report that they subscribe to tests from CTS. Most members of EDEWG
participate in proficiency tests constructed by group members and these tests cover all
aspects of document examination and are monitored by the steering committee of
EDEWG. EDEWG is also working on producing a best practice manual for document
laboratories.

403
From the answers to the questionnaire one can conclude that most laboratories are
members of one network or another, national or international. In Europe it is natural to be
a member of the ENFSI subgroup EDEWG. In the US ASQDE is natural common forum.
There are local networks like the Baltic Network of the Forensic Science Institutions. In
Japan we find the Japanese Association of Science and Technology for Identification and
on the southern hemisphere there is the Australian and New Zealand network.

A look into the future

Document examination is an ever changing subject where new fields of examination

appears continuously due to changes in office equipment, writing instruments, new
instruments for examination, new products and so forth. With introduction and
proliferation of computers and related equipment it is today easy for virtually anyone to
produce fake documents of very high quality. Gottesman et al (36) points out that with
affordable computers, photocopiers, and digital cameras, as well as high quality scanners
and printers, detecting forgeries and manipulations is no longer simple even for the fully-
trained document examiner. For the foreseeable future one can also predict closer and
closer co-operation between document examiners and computer specialists. It will be
necessary for the document examiner to acquire deep knowledge of the software as well
as the hardware in order to be able to draw the right conclusions regarding questioned
documents. Some areas of investigation will disappear. One example is examinations of
script from mechanical typewriters.

Abbreviations:
ABC Analytical and Bioanalytical Chemistry
DVS Document Various Specification
FSI Forensic Science International
FSS Forensic Science Service Reports
IS Infosecura
JA Journal of the American Society of Questioned Document Examiners
JD Journal of Documents
JFS Journal of Forensic Science
JIST Journal of Imaging Science and Technology
LAW Law Enforcement Technology
MH Mannheimer Hefte für Shriftvergleichung
PA59 Proceedings of American Society of Questioned Documents Examiners 59th
Annual Conference
PA60 Proceedings of American Society of Questioned Documents Examiners 60th
Annual Conference
PA61 Proceedings of American Society of Questioned Documents Examiners 61st
Annual Conference
PEAFS Proceedings of the 3rd European Academy of Forensic Science in FSI, Vol
136/SUPPL. 1, 2003
PGFS5 Proceedings of the 5th International Congress of Gesellschaft für
Schriftvergleichung (GFS)

404
SJ Science & Justice
Z Z-Zagadnien-Nauk-Sadowych

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 Digital Evidence

— A Review: 2001 to 2004 —

412
 Prepared by:

Anthony DiClemente, BS
Chief, Digital Evidence Section
Mary F. Horvath, MFS
Digital Evidence Support Unit
Mark M. Pollitt, MS
Joint Council on Information Age Crime

Federal Bureau of Investigation

Quantico, Virginia, USA

(703) 632-6450
adiclemente@fbi.gov

PART I - SUMMARY REPORT

INTRODUCTION

As defined by the Scientific Working Group on Digital Evidence (SWGDE) in 1998,

"Digital Evidence is information of probative value that is either stored or transmitted in
a binary form. " For the purposes of this report, we will identify four sub-disciplines:
Computer Forensics, Digital Video, Digital Audio and Digital Images . Each of these
sub-disciplines operates with slightly different processes and purposes, but share the
digital nature of the types of evidence examined. Digital Evidence has been recognized
and its status reported to this symposium since 1995.

This report will address the current status of digital evidence as practiced in the forensic
science community, how the disciple has evolved since our last report and some new

413
initiatives which have developed since the October, 2001 report. It is an understatement
to suggest that much progress has been made in this arena. For the last three symposia
we have reported on the infancy of digital evidence. Today, I believe we can announce
its adolescence.

CURRENT PRACTICE OF DIGITAL EVIDENCE

Volume:

The increasing use of digital technology in virtually every aspect of our daily lives is
producing a concomitant increase in evidence stored or transmitted in digital form. It is
difficult to measure the amount of digital forensic work that is being performed across
agency, national and international boundaries due to the use of non-standard terms and
definitions. As a result, empirical numbers are not available. However, to demonstrate
the relative increase in volume, we offer the following table which summarizes the
number of cases and the volume of digital evidence examined (by storage capacity)
within the FBI’s Computer Analysis Response Team (CART):

In FY 2003 Regional Computer Forensic Laboratories (RCFL’s) processed 82.3 TB of

data. This data represents FBI CART, and RCFL examiners, operating in the United
States and only conducting criminal and national security examinations of (generally) a
single type of evidence: computers. But to put this into context, in 2001, the Library of
Congress estimated that in 1980, the first year that they accepted digital submissions,
their entire collection was somewhere between 10 and 20 terabytes of information. The
CART and RCFLs are processing amounts of information that are hundreds of times the
amount of information stored in this national reference library every year and the volume
is increasing exponentially.

Organizational Issues:

Digital forensics continues to be practiced in a variety of ways by different organizations

and institutions. In fact, the largest trend is an increase in the number of practitioners
operating in each of the practice modalities. Digital forensic examinations are being
conducted by law enforcement officers and civilian employees in the field, within
investigative units and task forces as well as in dedicated units within traditional forensic
laboratories. This report will not further describe the various practice models; however,
will focus on the practice of digital evidence within traditional forensic laboratories.
One relatively recent development is the establishment of a network of single purpose
computer forensic laboratories known as RCFL’s. These facilities are partnerships
between local, state and federal law enforcement agencies and crime laboratories. Since
the establishment of the first such laboratory in San Diego, California, twelve new
laboratories have either been established or are under construction .

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The forensic examination of digital evidence has traditionally been the realm of
government agencies. That too is changing. Within the last several years, numerous
commercial organizations have begun to examine digital evidence, not only for
governmental agencies, but in connection with civil matters such as employment,
intellectual property, and product liability lawsuits. The term often used for this practice
is electronic discovery . In fact, according to one established firm, electronic discovery is
their largest area of growth within their forensic practice.

Tools and Methods:

Digital forensic practitioners have long shared a common approach to conducting

examinations. Over the last several years, there have even been attempts to codify these
approaches into frameworks . While there are at least six different frameworks, it is
noted that they are all similar in approach and in the words of one framework author,
Brian Carrier, "anyone of them could be mapped to any other. " It is clear that the
methods of examination have evolved into a generally accepted methodology.

Digital forensic tools have made great strides in the last three years. There are a number
of proprietary commercial and government software which have become standard tools in
the examination of digital media. Some of these tools are capable of utilizing multiple
processors and operating over networks. One recent trend is the development of tools
and methodologies to examine computers in an operational state.

With the tremendous increase in volume, forensic examiners have been adapting
technology to assist in making the process more efficient. One example of this is the
North Texas Regional Computer Forensic Laboratory’s use of storage area networks
(SAN’s) coupled with fiber channel networks to accelerate the acquisition of images,
aggregate images for examination and to provide network review capability for
investigators . This combination of hardware and methodology has proven so successful
that it is being adopted by the CART and the RCFL’s.

New tools and methodologies are also being developed to support the increasing number
of "smart" devices which include the functionality of multiple devices, such as
telephones, personal digital assistants (PDA’s), cameras, and e-mail devices.

Accreditation and Certification:

Accreditation is the recognition, by an accreditation organization, that a unit or laboratory

is competent to perform forensic examinations in a quality fashion. Certification, in
contrast, is the recognition by an organization or body, that an individual is competent to
perform specific duties.

In the United States, the American Society of Crime Laboratory Directors – Laboratory
Accreditation Board (ASCLD-LAB) has been the de facto standard for laboratory
accreditation. In February, 2003 ASCLD-LAB recognized digital evidence, along with

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its sub-disciplines of digital audio, digital video, digital imaging and computer forensics,
as a recognized discipline, subject to accreditation .

No time was wasted in developing an inspection process, and by the end of 2004 at least
three laboratories will have completed ASCLD-LAB inspection, and likely received
accreditation.

With recent recommendations by SWGDE and the Scientific Working Group on Imaging
Technology (SWGIT) to the ASCLD/LAB, the field will expand beyond the commonly
recognized "digital" media evidence types, but will now incorporate numerous other
physical item types such as analog tape, printed photographic material etc., - basically
anything that can ultimately be forensically examined under the computer, audio, image
and video sub-disciplines.

Recognition of these disciplines, by a recognized laboratory accreditation board, is a

significant landmark in the maturation of digital evidence. It recognizes digital evidence
as a forensic science, not merely an investigative tool utilized for lead purposes.
Accredited forensic laboratories have established Educational and Training Programs,
Standard Operating Procedures, Quality Assurance Guidelines, Test and Validation
Criteria, and Proficiency Examinations which collectively demonstrate a quality process.

The International Organization for Standardization (ISO) has developed a standard for
accrediting forensic laboratories under ISO 17025. The European Network of Forensic
Science Institutes (ENFSI) and the International Organization on Computer Evidence
(IOCE) have worked together to develop accreditation standards for digital evidence
within that standard . It should be noted that the ASCLD-LAB has decided to adopt the
ISO 17025 framework and has begun to transition to these new standards. The work
already undertaken by ENFSI’s Forensic Information Technology Working Group and
IOCE will ease that transition measurably.

Certification is another matter. At this time, virtually all forensic laboratories conduct
internal certification of practitioners. This may, in part, be due to a lack of a recognized
professional certification in the digital evidence disciplines. In the spring of this year, the
National Center for Forensic Science , at the University of Central Florida, hosted an
initial roundtable discussion on this issue. Attendance at this meeting included a number
of bodies currently offering certification in information security, training and education in
computer forensics, and agencies employing forensic practitioners. The consensus was
that there was a need for a multilevel certification program that would be recognized
across the forensic, law enforcement and private sector communities. We hope to be able
to report more fully on this initiative at the next INTERPOL Forensic Science
Symposium.

Research and Academic Programs

One of the unique aspects of digital forensics has been that it evolved in exactly the
reverse order from traditional forensic sciences such as DNA. Rather than apply an

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existing science to forensic use, digital forensics was driven from the law enforcement
end-user perspective. While this served to demonstrate its value, it created difficulty in
judicial and scientific acceptance. But that is rapidly changing.

Digital Forensic Working Group:

In approximately 2002, a number of universities began to explore the possibility of

developing and teaching digital forensic curricula. Given the paucity of information
available, they needed a forum to share ideas and to get input. In cooperation with the
law enforcement community, the Computer Forensic Educator’s Working Group was
established in early 2003. This group is now comprised of approximately 40 colleges and
universities and has been renamed the Digital Forensic Working Group. This group has
been instrumental in helping educational institutions develop academic programs in
digital evidence at the junior college, baccalaureate and graduate level. There are
currently several dozen schools that offer tuition in this area as either coursework,
concentrations, majors or degrees. Interestingly, included in the schools offering digital
forensics, there are traditional forensic programs, such as Duquesne and Marshall
Universities as well as traditional computer science, engineering and information
technology schools such as the University of Tulsa and Johns Hopkins University. In
addition to developing academic programs, this group is also focusing on research in the
digital forensic area.

International Federation for Information Processing (IFIP):

At their 2004 World Congress held in August, the International Federation for
Information Processing, one of the oldest and largest international bodies in the
information technology field, voted to establish a Working Group on Digital Forensics.
This is particularly significant, as this body is recognized for its four main purposes:
foster international cooperation, stimulate research and development, encourage
education and disseminate information . We hope to be able to report on this group’s
activities in our next report.

Digital Forensic Research Workshop (DFRWS):

A third development in the research area is that of the Digital Forensic Workshop
(DFRWS) . This venue, sponsored by the United States Air Force Research Laboratory,
began in 2001 and has sponsored a workshop each year since. The 2004 workshop
featured presentations of papers and workshops involving researchers and practitioners
from Brazil, Canada, China, Italy, the United Kingdom, the United States, and Uganda.
Much fundamental work was presented and this venue has added much to the
professionalization of this field.

PART II- DIGITAL EVIDENCE FORENSIC WORKING GROUPS

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European Network of Forensic Science Institutes - Forensic Information
Technology Working Group (FIT-WG)

The FIT-WG was established in September 1998, to promote the discipline of

information technology forensics in Europe, cultivate cooperation among its members,
establish quality in IT forensics and cultivate relationships with significant technical
organizations. In October 2003, the FIT-WG issued a best practices manual titled,
"Guidelines for Best Practices in the Forensic Examination of Digital Technology".

European Network of Forensic Science Institutes – Digital Imaging Working Group

(DIWG)

The DIWG was established in June 2003 with a focused mission of working together on
the use of digital imaging technology in forensic investigations. The primary members
are investigators and scientists from ENFSI institutes and are actively involved areas such
as crime scene photography, photogrammetry, 3d-reconstruction, computer modeling,
animation and simulation, face comparison, investigation of integrity and authenticity of
images and video analysis. Focused efforts have been on sharing information about
methods, operating procedures, guidelines, and current technical issues seen in casework.

European Network of Forensic Science Institutes – Forensic Speech and Audio

Analysis Working Group (FSAAWG)

The FSAAWG focuses its attention on issues related to speech, speech recognition, audio
analysis and authentication issues. Its current activities focus on proficiency testing,
collective exercises and database development efforts. The results of the first proficiency
test concerning authentication of analog tape recordings are currently being evaluated and
will be presented at the 2004 conference. Numerous efforts of building reference
database materials are underway for information such as magnetic pictures and events,
and speech data for use in automatic speaker recognition capabilities.

High Tech Crime Sub-Group of the G-8

In December 1997, the High-Tech subgroup of the G-8's Senior Experts on Transnational
Organized Crime and Home Affairs Ministers adopted principles and a 10 point action
plan. The principles and action plan, while not completely related to digital evidence,
recognized the need for coordination, training, preservation of evidence and the
establishment of standards. The G8 Government/Industry Conference on High Tech
Crime met in Tokyo in May 2001 and covered data retention, data preservation, threat
assessment and prevention, protection of electronic commerce, user authentication and
training.

International Organization on Computer Evidence (IOCE)

IOCE began in 1995 after the 2nd International Conference on Computer Evidence was
held. Its purpose was to provide an international forum for law enforcement agencies to

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exchange information concerning computer investigation and computer forensic issues.
At the request of the G8, IOCE developed and the G8 adopted six initial principles
written specifically for digital evidence as well as four definitions. Since that time IOCE
has held four International Conferences and published numerous guidelines and papers
relating to all aspects of the field of digital evidence such as examination, training,
laboratory management and quality assurance.

Since its inception, numerous other internationally related organizations have begun and
have now taken the field much farther than IOCE could have imagined. IOCE is re-
evaluating its impact and value on the community at large. It is unknown at this time
where and how it will continue its efforts.

National Institute of Justice (NIJ), United States - Department of Justice

The NIJ is the research, development and evaluation agency of the United States
Department of Justice. The NIJ sponsors Technical Working Groups (TWG) comprised
of law enforcement, forensic science and legal practitioners and research personnel
whose purpose is to improve investigative techniques. NIJ funded an initiative to
produce guides for the local law enforcement officers who were dealing with digital
evidence in their daily routines but did not have access to costly training programs and
courses. Technical Working Groups are established for each of the guides’ area of
concentration and consist of members with the relevant technical expertise. Seven of
these guides have been planned and three have been published.

In July 2004, the NIJ, Technical Working Group for the Examination of Digital Evidence
(TWGEDE) issued the third guide titled, "Forensic Examination of Digital Evidence: A
Guide for Law Enforcement Personnel". The report represents a consensus of
recommendations based upon the experiences and personal views of the TWGEDE
members. NIJ guides are not legal mandates or policy directives.

Scientific Working Group on Digital Evidence (SWGDE)

The mission of the SWGDE is to bring together organizations actively engaged in the
field of digital evidence to foster communication, and to ensure quality and consistency
within the forensic community. This groups’ membership includes representatives from
federal, state and local crime laboratories and law enforcement agencies in the United
States as well as associate members from Australia and Canada.

The SWGDE was formed as a result of the similarities and overlap in the disciplines of
audio analysis, video analysis, image analysis, and computer forensics. The SWGDE is
focused on the practice of digital evidence primarily in the forensic laboratory setting.
The SWGDE drafted a document titled, "Digital Evidence: Standards and Principles" and
presented at the International Hi-Tech Crime and Forensics Conference in London,
United Kingdom in October 1999.

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During 2004, SWGDE released "Best Practices for Digital Evidence Laboratory
Programs (Version 1.0 Approved 4/9/2004)" and "SWGDE Recommended Guidelines
for Validation Testing (Final Version-Approved 4/15/2004)".

SWGDE and SWGIT co-released drafts of a Standard Operating Procedure (SOP)

document, a Proficiency Test document, and a Digital Evidence Training Document
during August and September, 2004. ASCLD/LAB consults SWGDE for
recommendations and feedback concerning standards for the Digital Evidence discipline.

Scientific Working Group on Imaging Technology (SWGIT)

The goal of the SWGIT is to engage the entire law enforcement imaging community in
the development of guidelines.

The SWGIT was established to provide leadership to the law enforcement community by
developing guidelines for good practices for the use of imaging technologies within the
criminal justice system. The SWGIT released "Definitions and Guidelines for the Use of
Imaging Technologies in the Criminal Justice System in 1999, revised based on input
received in 2001 and was subsequently updated for release in June 2002 (Version 2.3).
The SWGIT released "Recommendations and Guidelines for the Use of Digital Image
Processing in the Criminal Justice System" as a draft in 2001 and was revised based upon
feedback. The final version was published in January 2003. The SWGIT released three
additional documents in final form. They include, " Definitions, Recommendation, and
Guidelines for the use of Forensic Video Processing in the Criminal Justice System,"
General Guidelines for Photographing Footware Impressions" and "General Guidelines
for Photographing Tire Impressions."

In July 2004, SWGDE and SWGIT jointly released, "SWGDE/SWGIT Proficiency Test
Program Guidelines (Version Draft), "SWGDE/SWGIT Recommended Guidelines for
Developing Standard Operating Procedures (Version Draft) and finally
"SWGDE/SWGIT Guidelines & Recommendations for Training in Digital & Multimedia
Evidence (Version Draft).

National Institute of Standards and Technology (NIST)

NIST is a non-regulatory federal agency within the U.S. Commerce Department's

Technology Administration. Its mission is to develop and promote measurement,
standards, and technology to enhance productivity, facilitate trade, and improve the
quality of life. In 2001, the FBI approached NIST with two project proposals, which are
now fully recognized and supported projects of NIST. A Steering Committee has been
established to oversee the operations of both projects and consists of representatives from
various US federal agencies including NIST, NIJ, DOJ, FBI, USSS, and US DoD.

The first project is the National Software Reference Library (NSRL), which grew out of
the FBI’s Advanced Computer Examination Support (ACES) Program. The NSRL is
now an internationally recognized effort which produces validated hash sets of

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commercially available programs for use in the data reduction process of digital forensic
examinations. The NSRL hash sets are publicly available are and recognized as standard
world-wide.

The second project is the Computer Forensic Tool Testing (CFTT) Project whose goal is
to perform validation and verification testing of forensic utilities that are commonly used
in the law enforcement community. Numerous reports are publicly produced for
comment and review along the entire test process to include test methodologies, test
plans, and test results. In addition, these reports are shared with the tools’ vendors to not
only allow for comment, but in hopes of providing the vendor areas of enhancement for
its utilities.

Forensic Computing Group - Association of Chief Police Officers (ACPO)

The Forensic Computing Group consisted of digital forensic practitioners in the United
Kingdom and was sponsored by the Association of Chief Police Officers. They produced
a "Good Practice Guide for Computer Based Electronic Evidence" in June of 1999 and
published by the ACPO Crime Committee. The Forensic Computing Group has since
disbanded.

United Kingdom’s National High-Tech Crime Unit (NHTCU)

The mission of the NHTCU is to combat national and transnational hi-tech crime within,
or which impacts upon the United Kingdom. It was set up as part of the national high-
tech crime strategy announced by the Home Secretary in November 2000 and was
launched in April 2001. The national high-tech crime strategy was drawn up in response
to the work of the ACPO Crime Committee, Computer Crime Working Group and a
published strategic threat assessment by the National Criminal Intelligence Service
(NCIS). The Unit is the lynch-pin to the UK’s coordinated response to cybercrime
working in partnership with other law enforcement agencies, business and the IT world. `
The NHTCU worked in conjunction with ACPO and produced new version of the Good
Practice Guide.

CONCLUSION

Since the last INTERPOL Forensic Science Symposium, the forensic discipline of digital
media has come a long way. Its process is more mature. Quality management of the
discipline is becoming the norm. The groups and organizations mentioned in this report
have fostered a healthy exchange of scientific knowledge and operational experience.
Given the rapidly increasing demand for these examinations, coupled with the integration
of technology in our daily lives, it is certain to continue in its dramatic development.

PART III - APPENDICES

Appendix A SWGDE Best Practices

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Appendix B SWGDE Recommended Guidelines for Validation Testing

Appendix C SWGDE Guidelines and Recommendations for Training in Digital

Evidence

Appendix D SWGDE/ SWGIT SOP

Appendix E SWGDE/ SWGIT Proficiency

Appendix F SWGIT Letter

Appendix G SWGIT Guidelines for Field Applications of Imaging Technologies in the

Criminal Justice System

Appendix H SWGIT Considerations for Managers

Appendix I SWGIT General Guidelines for Capturing Latent Impressions Using a

Digital Camera

Appendix J SWGIT Guidelines and Recommendations for Training in Imaging

Technologies in the Criminal Justice System

Appendix K SWGIT Recommendations and Guidelines for the Use of Digital Image
Processing in the Criminal Justice System

Appendix L SWGIT Definitions, Recommendations, and Guidelines for the Use of

Forensic Video Processing in the Criminal Justice System

Appendix M SWGIT General Guidelines for Photographing Footwear Impressions

Appendix N SWGIT General Guidelines for Photographing Tire Impressions

Appendix O SWGIT Recommendations and Guidelines Relating to the Use of Closed

Circuit Television Systems in Commercial Establishments

APPENDIX A–SWGDE BEST PRACTICES

Version 1.1
Drafted July 26, 2001
Revised October 2002, January 31, 2003
Revised February 2004
Approved for Comment February 4, 2004
Reformatted February 24, 2004

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Disclaimer:
As a condition to the use of this document and the information contained therein, the
SWGDE requests notification by e-mail before or contemporaneous to the introduction of
this document, or any portion thereof, as a marked exhibit offered for or moved into
evidence in any judicial, administrative, legislative or adjudicatory hearing or other
proceeding (including discovery proceedings) in the United States or any Foreign
country. Such notification shall include: 1) The formal name of the proceeding,
including docket number or similar identifier; 2) the name and location of the body
conducting the hearing or proceeding; 3) subsequent to the use of this document in a
formal proceeding please notify SWGDE as to its use and outcome; 4) the name, mailing
address (if available) and contact information of the party offering or moving the
document into evidence. Notifications should be sent to: execcmte@swgde.org.

Redistribution Policy:

SWGDE grants permission for redistribution and use of all publicly posted documents
created by SWGDE, provided that the following conditions are met:

1. Redistributions of documents, or parts of documents, must retain the SWGDE

cover page containing the disclaimer.

2. Neither the name of SWGDE, nor the names of its contributors, may be used
to endorse or promote products derived from its documents.

3. Any reference or quote from a SWGDE document must include the version
number (or create date) of the document and mention if the document is in a draft
status.

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BEST PRACTICES FOR DIGITAL EVIDENCE LABORATORY PROGRAMS

PART 1: Recommendations for Education and Training

SECTION 1: INTRODUCTION

1.1 Recommendations listed below are intended to apply to any examiner who:

Forensically examines and analyzes digital evidence or related materials, or

directs such examinations to be done.

As a consequence of such examinations, signs reports for legal and administrative

proceedings and provides testimony as required.

SECTION 2: MINIMUM RECOMMENDATIONS FOR EDUCATIONAL

REQUIREMENTS (for a further explanation of personnel/duties see section 7)

2.1 TECHNICIAN/ASSISTANT

Have education, skills, and abilities commensurate with their responsibilities.

2.1.2 Have on-the-job training specific to their position.

2.2 EXAMINER

An examiner should have at least a baccalaureate degree with science courses. An

examiner without a baccalaureate degree, should meet one of the following conditions:

Sixty semester hours of college level study to include course work with science courses;

OR

A minimum of two (2) years practical experience in the area of digital evidence
examination, and have demonstrated competency following the completion of a formal,
documented training program.

2.3 TECHNICAL MANAGER/LEADER

Meet all the requirements of an examiner.

Have a minimum of two (2) years of experience as an examiner in the forensic analysis of
digital evidence.

Exhibit knowledge necessary to evaluate results and conclusions.

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SECTION 3: CONTINUING PROFESSIONAL DEVELOPMENT

3.1 All personnel have an ongoing responsibility to remain current in their field. In
addition, agencies should provide support and opportunities for continuing professional
development. The recommended minimum continuing professional development
requirements for personnel are:

Forty annual hours of training relevant to the examiner’s responsibilities. All training,
once completed, must be documented. The training can be provided from a variety of
sources, including but not limited to:

Courses taught at the post-secondary educational level

Courses taught by vendors

In-service training conducted by the employer

In-service training taught by external provider

Attendance at workshops and participation in relevant scientific meetings or conferences.

To maintain membership in a field related professional organization.

SECTION 4: MINIMUM RECOMMENDATIONS FOR TRAINING PROGRAMS

Agencies should set their training programs to meet their needs as they relate to the types
of casework encountered, equipment available, and the level of competency of trainees.

A written training program, approved by the agency’s management, focusing on the

development of the theoretical and practical knowledge, skills and abilities necessary to
perform duties assigned, includes:

A training syllabus including descriptions of the knowledge and skills required by an

examiner (specific topic areas), milestones of achievement, and methods of testing or
evaluating competency.

Documented standards of performance and a plan for assessing theoretical and practical
competency against these standards (e.g. written and/or oral examinations, critical
reviews, mock casework, etc., per topic area).

A period of supervised casework that is representative of the type of casework required to

be performed.

Documentation verifying that the trainee has achieved the desired competence per
specific topic area.

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4.2 Topic areas in the training program should include, as a minimum, the following:

4.2.1 Relevant background information on digital evidence, such as:

4.2.1.1 Hardware

4.2.1.2 Software

4.2.1.3 Operating systems

4.2.1.4 Relevant applications

4.2.1.5 File identification

4.2.1.6 Relevant media (digital/analog)

4.2.1.7 File systems

4.2.2 Techniques, methodologies and equipment utilized in the examination of

digital evidence and related materials, such as:

4.2.2.1 Forensic analysis procedures

4.2.2.2 Best practices (technical procedures)

4.2.2.3 Standard operating procedures

4.2.3 Quality assurance, such as:

4.2.3.1 Quality assurance (for consistency within the forensic community)

4.2.3.2 Technical writing (for concise, clear reports)

4.2.3.3 Presentation skills (for the explanation of information)

4.2.3.4 General forensic principles and practices (for base of knowledge)

4.2.4 Expert/Court testimony and legal requirements, such as:

4.2.4.1 Public speaking (to build confidence in speaking situations)

4.2.4.2 Testimony skills (to establish a comfort level for testimony)

4.2.4.3 Admissibility (Daubert) Hearing Testimony (for issue awareness)

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 4.2.4.4 General criminal justice (to understand authority and result of
examinations)

4.2.4.5 Basic crime scene management (to understand scene and evidence
complexity)

4.2.5 Agency policies and procedures as they relate to the examination of digital
evidence and related materials, such as:

4.2.5.1 Safety (for the purpose of risk management and personal safety)

4.2.5.2 Security (to preserve chain of custody)

4.2.5.3 Ethics (to conform to a standard of integrity)

4.2.5.4 Evidence handling (to preserve integrity of evidence)

4.2.5.5 Training documentation (to demonstrate compliance)

An individual providing training must have the knowledge, skills, and abilities in the
subject area for which they are providing instruction.

SECTION 5: MINIMUM DOCUMENTATION/REFERENCE MATERIAL

AVAILABLE TO AN AGENCY PERFORMING DIGITAL EVIDENCE
EXAMINATIONS

Documentation/reference resources should be available and accessible to examiners in

hard copy or electronic form, such as:

College/university level textbooks as references to theory and practice in key subject

areas, e.g. hardware, software, and operating systems.

Reference literature pertaining to digital evidence.

Operation and maintenance manuals for all hardware and software available for use by
the examiner.

Relevant publications and periodicals.

Agency quality manual and standard operating procedures.

Relevant jurisdictional legislation (e.g., statutes and case law relating to digital evidence,
etc.).

Internet access.

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PART 2: Recommendations for Quality Assurance Guidelines

SECTION 6: INTRODUCTION

A digital evidence program should incorporate quality assurance. It is the goal of these
guidelines to provide a framework of quality management in the processing of digital
evidence, including evidence handling, management practices, analyses, and reporting.
6.1 QUALITY MANAGEMENT SYSTEM
A documented quality management system must be established and maintained.

The personnel responsible must be clearly designated and shall have access to
management responsible for organizational policy

6.1.2 The quality management system must cover all procedures and reports associated
with evidence

SECTION 7: PERSONNEL

7.1 JOB DESCRIPTION

The job descriptions for all personnel should include responsibilities and duties.

7.2 DESIGNATED PERSONNEL AND RESPONSIBILITIES

An individual (however titled) may be responsible for more than one of the following
duties:
Quality Assurance Manager: A designated person who is responsible for maintaining the
quality management system (including an annual review of the program) and who
monitors compliance with the program.

Health & Safety Manager: A designated person who is responsible for maintaining a
Health and Safety program (including an annual review of the program) and who
monitors compliance with the program.

Operational Manager: A designated person who has the overall responsibility and
authority for the operations of the unit.

Technical Manager/Leader: A designated person who has the overall responsibility and
authority for protocols and analytical methodologies.

Examiner: A designated person who:

Examines and analyzes digital evidence or related materials, or directs such examinations
to be done.

Signs reports for legal and administrative proceedings.

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Technician/Assistant: A person who works with evidence, but typically does not issue
reports for court purposes.

7.3 QUALIFICATIONS/EDUCATION
The agency should articulate its minimum qualifications, training and education
requirements consistent with those stipulated in Part 1 of this guide.

7.4 TRAINING
The agency must establish and document a training program and qualifying procedure for
all technical personnel. A written training program, approved by management, should
focus on the development of the theoretical and practical knowledge, skills and abilities
necessary to examine digital evidence and related materials as enumerated in Part 1 of
this guide.

7.5 MAINTAINING QUALIFICATIONS

The agency must establish and document the minimum continuing professional
development requirements for all technical personnel as enumerated in Part 1 of this
guide.

SECTION 8: PHYSICAL PLANT

FACILITY REQUIREMENTS
8.1.1 The facility shall provide adequate safety and security for personnel and
operations.
8.1.2 The facility must meet required health and safety standards.
8.1.3 The facility must contain adequate space to perform required analytical functions
and prevent alteration/damage to evidence.
A fume hood may be needed when the physical evidence poses a health and/or safety
hazard to the examiner (e.g., for digital evidence that was seized in a clandestine drug
lab, a crime scene containing biological materials, or other potentially hazardous
environments). It must be properly maintained and monitored according to an
established schedule.
8.1.5 A facility should maintain general cleanliness.
8.1.6 Facilities must be designed to ensure the proper safekeeping of evidence, data,
and records to protect from loss, cross-transfer, contamination and/or deleterious change.
Appropriate precautions should be taken with regard to electrostatic discharge, electrical
and magnetic fields to ensure the integrity of the digital evidence.
Appropriately secured storage areas must be provided.

SECTION 9: EVIDENCE CONTROL

The unit shall have and follow a documented evidence control system to ensure the
integrity of physical and digital evidence.

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9.1 RECEIVING AND IDENTIFYING EVIDENCE
The unit must maintain records of requests for service and of the respective items of
evidence. A unique identifier must be assigned to each case file or record. This file or
record must include at least the following:
9.1.1 The request for service document or a copy thereof.
9.1.2 The identity of the party requesting the service and the date of the request.
9.1.3 A description of items of evidence submitted with each having a unique item
identifier.
9.1.4 The identity of the person who delivers the evidence, along with the date of
submission. For evidence not delivered in person, descriptive information regarding the
mode of delivery and tracking information.
9.1.5 The chain of custody record.
9.1.6 Documentation of communication with the submitter.

9.2 INTEGRITY OF EVIDENCE

Evidence must be properly secured and labeled in accordance with the agency’s digital
evidence handling policy. Appropriate storage conditions shall ensure that the digital
evidence is not altered or lost. All actions taken with regard to the digital evidence will be
documented. A description of the evidence shall be compared to documentation prior to
examination. Any irregularities should be identified at this time, documented in the case
file and the submitter promptly informed.

9.3 STORAGE OF EVIDENCE

Access to the evidence storage area must be granted only to persons with authorization.
Access shall be controlled.

9.4 DISPOSITION OF EVIDENCE

Records must be kept regarding the disposition of all items of evidence.

9.5 DOCUMENTATION PROCEDURES

All records, such as results of examinations, measurements, notes, calibrations, spectra
and reports, shall be retained in a secure fashion.

SECTION 10: EXAMINATION PROCEDURES

10.1 PROCEDURES FOR DIGITAL EVIDENCE EXAMINATION

10.1.1 The unit shall have and follow written examination procedures.
10.1.2 Work practices shall be established to prevent contamination of evidence during
examination procedures.
10.1.3 The unit shall monitor the examination procedures using appropriate controls and
traceable standards.
Examination procedures must be validated in compliance with Section 14.

10.2 QUALIFICATION OF REFERENCE MATERIALS

10.2.1 The credibility of reference material should be confirmed prior to their first use.

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10.2.2 Unconfirmed reference materials must be qualified prior to use.
10.2.3 All qualifications must be documented to include the name of the individual who
performed the qualification and the date of qualification.

SECTION 11: EQUIPMENT PERFORMANCE

“Equipment” in this section refers to the non-evidentiary hardware and software the
examiner utilizes in the course of an examination.
11.1 Equipment must be monitored and documented to ensure proper performance is
maintained.
11.2 Only suitable and properly operating equipment shall be employed.
11.3 The manufacturer's operation manual and other relevant documentation for each
piece of equipment should be readily available.

SECTION 12: DOCUMENTATION, REPORTS, AND REVIEW

DOCUMENTATION
12.1.1 Examination documentation must contain sufficient detail to allow a peer to
reproduce the results obtained by the original examiner.
12.1.2 Evidence handling documentation should include: chain of custody, the initial
count of evidence to be examined, information regarding the packaging and condition of
the evidence upon receipt by the examiner, a description of the evidence, and
communications regarding the case.
12.1.3 Examination documentation should include items such as: observations,
examination processes and results, and supporting charts, graphs, and spectra generated
during an examination.
12.1.4 Documentation must be preserved according to written agency policy.

12.2 REPORTS
12.2.1 Reports issued by the unit must address the requests of the submitter.

Reports should include:

12.2.2.1 Identity of the reporting agency

12.2.2.2 Case identifier or submission number

12.2.2.3 Identity of the contributor

12.2.2.4 Date of receipt

12.2.2.5 Date of report

12.2.2.6 Descriptive list of submitted evidence

12.2.2.7 Identity of examiner

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12.2.2.8 Results/Conclusions

12.2.3 Written procedures for the release of case report information should be
established.

12.3 REVIEW

12.3.1 The agency must have a written policy establishing the protocols for technical and
administrative review.
The agency must have a written policy to determine the course of action should an
examiner and reviewer fails to agree.

SECTION 13: COMPETENCY AND PROFICIENCY TESTING

Each agency should participate in at least an annual proficiency-testing program and

should have written protocols for testing the competency and proficiency of its
examiners.

13.1 COMPETENCY TESTING

13.1.1 Units will monitor and document the competency of their examiner trainees and
technical support personnel prior to assumption of casework responsibilities.
13.1.2 Competency testing samples should be representative of the unit's normal
casework.
13.1.3 Competency testing must comply with the unit’s standard operating procedures
and other protocols.

PROFICIENCY TESTING - INTERNAL

13.2.1 Each examiner shall be proficiency tested annually in each sub-discipline in
which casework is performed.
13.2.2 The proficiency testing samples should be representative of the examiner's normal
casework.
13.2.3 The test examination must comply with the unit’s standard operating procedures.

PROFICIENCY TESTING - EXTERNAL

13.3.1 Each unit shall be proficiency tested annually in order to verify the unit's
performance.
13.3.2 The proficiency testing samples should be representative of the unit's normal
casework.
13.3.3 The test examination should follow the unit’s standard operating procedures.
The proficiency tests shall be obtained from approved test providers where available.

SECTION 14: VALIDATION

14.1 Validation is required to demonstrate the examination procedures and tools are
suitable for their intended purpose.

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14.1.1 Minimum acceptability criteria should be described along with means for
demonstrating compliance.
14.1.2 Validation documentation is required.

SECTION 15: INTERNAL AUDITS

15.1 Audits should be conducted at least once a year.

15.2 Records of each audit must be maintained and should include the scope, date of
the audit, name of the person(s) conducting the audit, findings, and corrective actions
taken, if necessary.

SECTION 16: DEVIATIONS AND DEFICIENCIES

In the course of examining digital evidence and related materials, the unit may experience
results that are anomalous in some manner. Each unit must have a written policy to deal
with deviations and deficiencies.
16.1 As used in this guide, a deficiency is any erroneous examination result or
interpretation, or any unapproved deviation from an established policy or procedure in an
examination.

16.2 As used in this guide, a deviation is a departure from the established policies and
procedures.

Comment: In developing policy the following may be considered: a requirement for

immediate cessation of the activity or work of the individual or tool involved, if
warranted by the seriousness of the deficiency, as defined in the written policy; a
requirement for administrative review of the activity or work of the individual involved; a
requirement for evaluation of the impact this deficiency may have had on other activities
of the individual or other examiners; a requirement for documentation of the follow-up
action taken as a result of the review; a requirement for communication to appropriate
employees of any confirmed deficiency which may have implications for their work.

SECTION 17: HEALTH AND SAFETY

The agency must have a documented health and safety program in place to meet the
needs of the unit.

17.1 HEALTH AND SAFETY REQUIREMENTS

17.1.1 All personnel should receive appropriate health and safety training.
17.1.2 The digital evidence unit shall operate in accordance with agency policy and
comply with any relevant statutory regulations.
17.1.3 Health and safety manual(s) shall be readily available to all personnel.

SECTION 18: DOCUMENTATION

In addition to casework documentation the unit should maintain documentation on the
following topics:

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18.1.1 Quality manual

18.1.2 Standard operating procedures

18.1.3 Training

18.1.4 Validation of tools

18.1.5 Physical workspace

18.1.6 Equipment maintenance/calibration

18.1.7 Health and safety

18.1.8 Evidence handling tracking system

18.1.9 Annual assessment of the quality management system

18.1.10 Proficiency testing

18.1.11 Report of findings

18.1.12 Court testimony monitoring

18.1.13 Competency testing

18.1.14 Evidence seized

18.1.15 Audits

18.1.16 Corrective action policy/procedures

18.1.17 Complaints and conflict resolution

18.1.18 Reference materials (including source and qualification).

18.1.19 Equipment inventory (e.g. manufacturer, model, serial number, acquisition

date).

SECTION 19: QUALITY MANUAL

19.1 The agency’s quality system policies and objectives shall be defined in a Quality
Manual. A comprehensive Quality Manual must contain or reference the documents or
policies/procedures pertaining to the following:

19.1.1 A quality policy statement including objectives and commitments by management

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19.1.2 The organization and management structure of the unit, its place in any parent
organization, and relevant organizational charts

19.1.3 The relationships and responsibilities of management, technical operations, and

support services in implementing the quality system

19.1.4 Job descriptions, education, and up-to-date training records of unit staff

19.1.5 Control and maintenance of documentation of case records and procedure

manuals

19.1.6 The unit’s procedures for ensuring that measurements are traceable to appropriate
standards, where available

19.1.7 The type and extent of examinations conducted by the unit

19.1.8 Validation of test procedures used

19.1.9 Handling evidence

19.1.10 The use of standards and controls in unit procedures

19.1.11 Calibration and maintenance of equipment

19.1.12 Practices for ensuring continued competence of examiners including

proficiency testing programs, and internal quality control schemes (e.g., technical review)

19.1.13 Gaining feedback and taking corrective action whenever discrepancies are
detected

19.1.14 Monitoring court testimony to ensure the reporting of scientific findings in

an unbiased and effective manner

19.1.15 Unit protocol permitting departures from documented policies and

procedures

19.1.16 Dealing with complaints

19.1.17 Disclosure of information

19.1.18 Audits and quality system review

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PART 3: Recommended Procedures for Digital Forensic Examinations

The following information is provided as guidance for the development of agency

Standard Operating Procedures (SOP). The SOP should address each of the following
elements:

SECTION 19: REVIEW THE REQUEST FOR SERVICE/EXAMINATION

Ascertain legal authority to perform the requested examination. The examiner will be
provided with the legal authority that allows him/her to examine digital evidence.
Examples of such authority include: consent to search by owner, subpoena, search
warrant, or other legal authority.

Review documentation provided by the requestor to determine the processes necessary to

complete the examination.

SECTION 20: RECEIPT OF EVIDENCE PROTOCOL

Maintain chain of custody per established agency standard operating procedures for
handling digital evidence.

Coordinate with the investigator and/or other forensic examiners when other forensic
examinations may be required. Specifically, the order in which these forensic
examinations will be conducted should be determined prior to any examination. (e.g.
latent print analysis, DNA analysis, hair fiber analysis)

SECTION 21: CONDUCT PHYSICAL INSPECTION OF ITEMS

PRESENTED FOR DIGITAL EXAMINATION

Inspect and document the evidence received. Note condition of items received and any
exceptions between the inventory of items received and the evidence reviewed by the
examiner.

Assess the power needs for devices with volatile memory. Follow agency policy for the
handling of these devices.

SECTION 22: PREPARATION FOR EXAMINATION

The examiner should maintain evidence integrity and document any exceptions.
Establish conditions to prevent the possibility of data contamination.

SECTION 23: CONDUCT EXAMINATION

Document evidentiary settings and configurations, if possible.

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Extract digital information necessary to meet requirements of the examination.

Analyze and/or interpret the extracted digital information.

SECTION 24: DOCUMENT THE EXAMINATION

The documentation must contain a sufficient level of detail such that another competent
examiner could reproduce the same extracted results.

Report(s) issued must meet the requirements of the agency.

SECTION 25: QUALITY CONTROL

Adhere to the agency’s quality control procedures which should include:

Technical/Peer review.

Administrative review.

SECTION 26: ISSUE REPORT

The report must be signed and dated by the examiner. The signature may be electronic or
physical as per agency standards.

SECTION 27: DISPOSITION OF EVIDENCE

Adhere to organization’s evidence disposition policy.

GLOSSARY

Administrative Review
A procedure used to check for consistency with laboratory policy and for editorial
practice. (ASCLD/LAB)

Audit
A review conducted to compare the various aspects of a laboratory’s performance with a
standard for that performance. (ASCLD/LAB)

Digital Evidence
Information of probative value stored or transmitted in binary form. (SWGDE)

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Digital Evidence Examiner (Examiner)
An individual responsible for the duplication, extraction and/or analysis of information
from digital evidence, generation of work product, writing reports, and testifying in legal
and administrative proceedings. (SWGDE)

Qualification Testing
Process to provide sufficient confidence that reference materials utilized are valid.

Quality Assurance
Those planned and systematic actions necessary to provide sufficient confidence that a
laboratory’s product or service will satisfy given requirements for quality.
(ASCLD/LAB)

Reference Materials
As used in this document, this refers to items such as published literature, hardware and
software documentation, hash sets, header sets, etc. (SWGDE)

Technical/Peer Review
An evaluation of reports, notes, data, and other documents to ensure an appropriate and
sufficient basis for the scientific conclusions. This review is conducted by a second
qualified individual. (In accordance with ASCLD/LAB)

Validation
The process of performing a set of experiments that establish the efficacy and reliability
of a technique or procedure or modification thereof. (ASCLD/LAB)

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 APPENDIX B - SWGDE RECOMMENDED GUIDELINES FOR VALIDATION
TESTING

Version 1--Draft Approved for Public Comment

Drafted by Research: August 20, 2003
Revised by Research: February 3, 2004
Approved for Public Comment by SWGDE: February 4, 2004
Reformatted February 24, 2004
Revised March 1, 2004 (based on voter feedback)
Final version approved by SWGDE for publication: April 15, 2004

Disclaimer:

As a condition to the use of this document and the information contained therein, the
SWGDE requests notification by e-mail before or contemporaneous to the introduction of
this document, or any portion thereof, as a marked exhibit offered for or moved into
evidence in any judicial, administrative, legislative or adjudicatory hearing or other
proceeding (including discovery proceedings) in the United States or any Foreign
country. Such notification shall include: 1) The formal name of the proceeding,
including docket number or similar identifier; 2) the name and location of the body
conducting the hearing or proceeding; 3) subsequent to the use of this document in a
formal proceeding please notify SWGDE as to its use and outcome; 4) the name, mailing
address (if available) and contact information of the party offering or moving the
document into evidence. Notifications should be sent to: execcmte@swgde.org.

Redistribution Policy:

SWGDE grants permission for redistribution and use of all publicly

posted documents created by SWGDE, provided that the following
conditions are met:

1. Redistributions of documents, or parts of documents, must retain the

SWGDE cover page containing the disclaimer.

2. Neither the name of SWGDE, nor the names of its contributors, may be used to
endorse or promote products derived from its documents.

3. Any reference or quote from a SWGDE document must include the version
number (or create date) of the document and mention if the document is in a draft status.

Introduction:

Validation testing is critical to the outcome of the entire examination process. Validation,
based on sound scientific principles, is required to demonstrate that examination tools
(hardware and software), techniques and procedures are suitable for their intended
purpose. Tools, techniques and procedures should be validated prior to initial use in

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digital forensic processes. Failure to implement a validation program can have
detrimental effects.

Target Audience:

All organizations performing digital forensic examinations.

Definition of Validation Testing:

An evaluation to determine if a tool, technique or procedure functions correctly and as

intended.

Scope of Testing:

Validation testing should be applied to all tools, techniques and procedures utilized in the
performance of digital forensics.

Special note of consideration: Tools, techniques and procedures, which by virtue of

their widespread use, duration of use, and acceptability by the larger information
technology community are generally acknowledged as reliable and trustworthy.
Consideration may be given to the general acceptance of a tool, technique or procedure in
its determination of whether validation is required.

When:

Validation testing should be performed whenever new, revised, or reconfigured tools,

techniques or procedures are introduced into the forensic process. While media and
operating systems are not generally considered tools for the purposes of this document,
these may exhibit characteristics that might not remain consistent when used with
different tools, techniques, and procedures. These situations may require additional
testing. Editorial changes or changes made for clarification purposes only will not
require revalidation.

Why:

To ensure the integrity of the components utilized in the forensic process.

Process:

Develop and document test plan before testing begins. The test plan should contain the
following:

Purpose and scope

Requirements to be tested – what does the tool have to do?

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Methodology – how to test? (Identify support tools required to assist in evaluation of
results when applicable)

Test scenarios

Condition or environment required for test scenario

Actions to perform during utilization of the tool, technique or procedure

Expected results - determine pass/fail criteria

One test may be sufficient depending on the tool, technique or procedure being tested.
The number of test scenarios should be sufficient to cover the various environments
encountered – for example, different file systems, media sizes, platforms, device types,
etc.

Different options may need to be tested such as user configurable option settings, switch
settings, etc., in accordance with purpose and scope

Test data to fulfill conditions of test scenarios – can the existing reference data set be
used? (Identify support tools required to assist in the development of test data when
applicable)

Document test data used

Note: Be sure each requirement is assigned to at least one test scenario.

Perform test scenario(s) and document results in test report

Use media and/or other sample materials that are in a known state or condition

Use test equipment with known configuration which corresponds to your examination
environment

If anomaly occurs then:

Attempt to identify conditions causing anomaly

Attempt to independently verify conditions causing anomaly

If feasible, implement alternative procedure and re-test

If re-tests are performed, results of all tests must be documented

Be sure pass/fail status for each requirement is annotated in test report

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Ensure to annotate all testers and dates assigned to test scenario

Individual test scenario(s) must be documented separately, but a summary report should
be written which states the overall pass/fail status of the tool, technique or procedure,
along with any recommendations, concerns, etc.

Validation of results: comparison between actual and expected results must be

performed and discrepancies between the two must be documented

Test Plan Template

The validation testing process shall be documented in detail to enable independent

replication and shall be written before testing begins. There is no standard format or title
for this document, but a typical format might include:

Purpose and scope

Requirements: what does the tool have to do?

Description of methodology: how to test?

Expected results: global view of pass/fail

Test Scenarios for each:

Conditions: test environment (hardware/software configurations, etc.)

Actions: specific actions

Assigned requirements

Expected results: specific pass/fail

Description of test data

Test Scenario Report Template

Individual test scenario(s) must be documented and a summary report should be written
which states the overall pass/fail status of the tool, technique or procedure along with any
recommendations, concerns, etc.

There is no standard format or title for a Test Scenario Report, but a typical format might
include:

Test number/identification: Each test should have a unique identifier for referral,
indexing, etc.

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Test title

Test date

Test person

Test designer/reviewer when applicable: Test reviewer should be independent of the

designer and the tester

Test description

Test result (overall pass/fail result)

Configuration of test platform: Document both hardware and software configurations as

well as any preference or option settings when test is performed

Tool being tested

Title

Manufacturer

Version or date

Notes regarding test data set

Test notes

Notes of tool or test being performed

Procedures

Procedures should be written granular enough to allow exact replication by independent

party

Document options or switches used if applicable

Observations

Results

Expected results

Actual results

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Validation results – comparison between actual and expected results must be performed
and discrepancies between the two must be documented

The Summary Report should state the overall pass/fail status of the tool, technique or
procedure along with any recommendations, concerns, etc. There is no standard format
or title for this report, but a typical format might include:

Test report title and number/identification

Test date

Test description

Title, manufacturer and version/date of tool, technique or procedure tested

Test result (overall pass/fail result)

List each requirement and its result

Observations, concerns, limitations

Recommendations (optional)

Note regarding included samples: The attached samples are in an abbreviated form and
are included for demonstration purposes only. Actual documentation of these types may
include steps not delineated here.

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Sample Test Plan

Test Number: SWWB -04-01

Test Title: Software Write-Block (Software WB)

Purpose and Scope:

This test plan will test the ability of the Software WB to write-protect supported hard
disks attached to a system during operational usage. The plan will consist of four test
scenarios.

Requirements:

The Software WB forensic tool should allow normal operation to unprotected disks (i.e.,
the system drive).

The Software WB forensic tool should block all modifications to protected disks.

The before-test and after-test md5sums should match for the protected disks.

The Software WB forensic tool should provide feedback to the user as to the status of the
tool and the disks that the tool can affect.

Description of Methodology:

Various supported hard drives will be attached to standard forensic computer

configuration and system will be booted. The Software WB utility must protect all non-
system devices and not allow modifications from taking place. Modifications shall be
attempted by executing functions that should write to protected and unprotected drives.

Expected Results:

The Software WB forensic tool allows normal operation to unprotected disks (i.e., the
system drive)

The Software WB forensic tool should block all modifications to protected disks

The before-test and after-test md5sums match on protected disks

The Software WB forensic tool provides feedback to the user as to the status of the tool
and the disks that the tool can affect

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Test Scenarios:

Test Environment: Actions: Assigned Expected Results:

Number Reqt’s:
04-01-01 ATA drive, primary Copy/create/edit All No modification to
slave / protected disks
SCSI drive, ID0 erase file
04-01-02 ATA drive, Copy/create/edit All No modification to
secondary / protected disks
erase file
04-01-03 SCSI drive, ID0 Copy/create/edit All No modification to
/ protected disks
erase file
04-01-04 SCSI drive, ID1 Copy/create/edit All No modification to
/ protected disk
erase file

Test Data Description:

Test Data Set:

Maxtor 541DX Model 2B010H1 (ATA)

Md5sum: d0aeab1c1ace0234ee50b6b2f65791a7
Seagate Barracuda Model ST318437LW 18.4 GB (SCSI)
Md5sum: ecdb8df03e39e11ab67e8cd1dc235387

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Sample Test Scenario Report

Test Number: SWWB -04-01-01 (a similar report will be created for all test
scenarios)
Test Title: Software Write-Block during Operational Testing
Test Date: 8/07/2003
Tester: John Doe

Test Description:

This test procedure will test the ability of the Software WB to write-protect an ATA hard
drive and a SCSI hard drive attached to a system during operational usage. The procedure
will consist of one case. The case consists of attaching a wiped ATA hard drive as a
primary drive and attaching the SCSI hard drive on a SCSI chain. The system will then
be booted, the system status confirmed and then shutdown.

Test Result:

Passed. The Software WB write-protected the SCSI and the ATA hard drives.

Hardware:
Test System:
OS Name & Version: Microsoft Windows 2000 Professional
5.0.2195 Service Pack 2 Build 2195
System Manufacturer: Dell
System Model: Precision Workstation 530MT
Processors: x86 Family 15 Model 2 GenuineIntel ~37202 Mhz (as indicated by
System Information)
x86 Family 15 Model 2 GenuineIntel ~37202 Mhz (as indicated by System
Information)
BIOS Version: 2/25/2002
SCSI Adapter: Adaptec 2940

Forensic Tool:

Title: Software WB
Manufacturer: Umpty-phrat Technologies Inc.
Version: Version 4.10.00

Test Data Notes:

Test Data Set: Maxtor 541DX Model 2B010H1

Md5sum: d0aeab1c1ace0234ee50b6b2f65791a7
Seagate Barracuda Model ST318437LW 18.4 GB
Md5sum: ecdb8df03e39e11ab67e8cd1dc235387

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Test Notes:

Since the Software WB is a Windows 2000 application, the hard drive is unprotected
until the application starts during initial boot up

The Software WB application is loaded on the test system before the procedure is run.
Automatically lock local and Network drives was selected during the Software WB
install

The test system boot sequence is 1) Hard-disk drive c:, 2) IDE CD-ROM device, and 3)
Diskette drive

The ATA test hard drive is attached to the test system as the primary slave. The SCSI is
attached to the test system via a SCSI chain with ID0

A Linux bootable CD-ROM, version 3.99, is utilized to perform the validation tests

Procedures:

The test system is shutdown

Press the “On/Off” switch on the test system

Step Result: The system boots up

Double-click the “SoftwareWB” icon

Step Result: The Software WB application opens with the Media tab having focus. The
following table is on the tab:

Physical Media: Partitions: Write Blocked:

System Partition C No
FloppyDrive0 A Yes
CDRomDrive0 E Yes
HardDrive0 C No
HardDrive1 D, I, J Yes
HardDrive2 F, G, H Yes

Close the Software WB window

Step Result: The Software WB window closes

Press the “Start” button and select “Settings”, “Control Panel”

Step Result: The “Control Panel” window opens

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Double-click “Administrative Tools”

Step Result: The “Administrative Tools” window opens

Double-click “Computer Management” button

Step Result: An independent “Computer Management” window opens

Select “Disk Management”

Step Result: The right side panel changes to display the attached drives information

Device Partition
Disk 0 C:
Disk 1 D:
I:
J:
Healthy
Unallocated
Disk 2 F:
G:
H:
Healthy
CDROM0 E

Close the “Computer Management” window

Step Result: The window closes

Close the “Administrative Tools” window

Step Result: The window closes

11. Launch “Windows Explorer”

Step Result: The “Windows Explorer” window opens

12. Select text file “Test.txt” from system drive C:

13. Right-Click on file and choose “Copy” option

14. Select D: drive (Disk 1, first partition)

15. Right-Click and choose “Paste” option

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Step Result: Dialog box appears with message “Unable to copy the file ‘test.txt’. The
media is write-protected”

16. Press “OK” to close the dialogue box

Step result: The dialogue box closes

17. In “Windows Explorer” window, highlight text file “Dataset.doc” from Disk 1, first
partition path D:\

18. Press delete key

Step Result: Dialog box appears with message “Are you sure you want to delete
‘Dataset.doc’?”

19. Press “Yes” at dialog box

Step Result: Dialog box appears with message “Unable to delete the file ‘Dataset.doc’.
The media is write-protected”

20. Press “OK” to close the dialogue box

Step result: The dialogue box closes

21. Close the “Windows Explorer” window

Step result: The window closes

System Shutdown:

Click the “Start” button and select “Shutdown”

Step Result: The Windows shutdown dialog box opens

Select “Shutdown” and press the “OK” button

Step Result: The test system shuts down

Remove the test hard drives from the test system

Expected/Actual Results:

Expected:

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1. The Software WB forensic tools should allow normal operation to unprotected
disks (i.e., the system drive)

2. The Software WB forensic tools should block all modifications to protected disks

The before-test and after-test md5sums should match

The Software WB forensic tool should provide feedback to the user as to the status of the
tool and the disks that the tool can affect

Actual:

The actual results were the expected results

Validation Results:

Connect an Acard to the ATA test drive and boot test machine with a Linux bootable CD-
ROM. Run the md5sum utility to produce an md5sum for the test drive. The following
command should be used:

tty1:/# md5sum /dev/hda

Step Result: The md5sum before and after test md5sums match

Test Drive md5sum

Maxtor 541DX Model 2B010H1 (ATA) d0aeab1c1ace0234ee50b6b2f65791a7

Connect an Acard to the SCSI test drive and boot test machine with a Linux bootable
CD-ROM. Run the md5sum utility to produce an md5sum for the test drive. The
following command should be used:

tty1:/# md5sum /dev/sda

Step Result: The md5sum matches the before test md5sum.

Test Drive md5sum

Seagate Barracuda Model ecdb8df03e39e11ab67e8cd1dc235387
ST318437LW 18.4 GB (SCSI)

This test procedure validated the test criteria for the Software WB. The criteria and a
validation statement are given below:

The Software WB forensic tool shall not block any requests to unprotected disks

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The system was able to boot from the unprotected system drive and the system drive was
used throughout the procedure

Following the installation of the Software WB forensic tool, all attempts to write to the
write-protected ATA hard drive shall be unsuccessful

The unchanged before-test and after-test md5sums show that the ATA and the SCSI hard
drive was not changed by the execution of the procedure

The Software WB forensic tool shall provide feedback to the user as to the status of the
tool and the disks that the tool can affect

Throughout the procedure, the Software WB application provided the status of the tool
relative to the disk the tool could affect

The unchanged before-test and after-test md5sums show that the ATA and the SCSI hard
drive was not changed by the execution of these procedures

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Sample Summary Report

Test Number: SWWB -04-01

Test Title: Software Write-Block (Software WB)
Test Date: 8/07/2003 – 08/16/2003

Test Description:

This documents the results of testing the ability of the Software WB to write-protect
supported hard disks attached to a system during operational usage. The test plan consists
of four test scenarios including ATA and SCSI hard disks.

Forensic Tool:

Title: Software WB
Manufacturer: Umpty-phrat Technologies Inc.
Version: Version 4.10.00

Test Results:

Test Environment Req’t Req’t Req’t Req’t

Number 1 2 3 4
04-01-01 ATA drive, primary Pass Pass Pass Pass
SCSI drive, ID0
04-01-02 ATA drive, secondary Pass Fail Fail Pass
04-01-03 SCSI drive, ID0 Pass Pass Pass Pass
04-01-04 SCSI drive, ID1 Pass Pass Pass Pass

Requirements:

The Software WB forensic tool should allow normal operation to unprotected disks (i.e.,
the system drive).

The Software WB forensic tool should block all modifications to protected disks.

The before-test and after-test md5sums should match for the protected disks.

The Software WB forensic tool should provide feedback to the user as to the status of the
tool and the disks that the tool can affect.

Observations/Concerns:

N/A

Limitations:

452
Not to be used with ATA drive attached to secondary IDE channel.

Recommendations:

To be used with SCSI drives, and ATA drives connected to primary IDE channel only.

453
History: SWGDE Recommended Guidelines for Validation Testing

Revision Issue Date Section History

Draft document created

08/20/2004 All`
Changed “Test Report Template” (original document, p. 4) to
Approved
1 p. 4 “Test Scenario Report Template”
02/04/2004
Added “Note Regarding Included Samples” after No. 7
Approved
2 p. 5 (“Recommendations (optional)”)
02/04/2004
Changed (under “Test Scenarios, Test Number 04-01-01,
Approved Environment:) “ATA drive, primary” to “ATA drive,
3 p. 6
02/04/2004 primary slave, SCSI Drive, 100”

Changed (under “Sample Test Scenario Report, Test Number):

Approved “SWWB –04-01” to “SWWB –04-01-01 (a similar report
4 p. 8
02/04/2004 will be created for all test scenarios”)

Added (under “Test Notes”) No. 5 (“A Linux bootable CD-

Approved ROM, version 3.99, is utilized to perform the validation
5 p. 9
02/04/2004 tests”)

Revised the table under “Procedures,” No. 3: “HardDrive

1/D,I,J/Yes” changed to “HardDrive0 /C/No”;
Approved “HardDrive2/K/Yes” changed to “HardDrive1/D,I,J/Yes”;
6 p. 9
02/04/2004 “HardDrive3/F,G,H/Yes” changed to
“HardDrive2/FGH/Yes”

Revised the table under “Procedures”, No. 8: “Disk 2/K”

Approved changed to “Disk 2/F:, G:, H:, Healthy”; replaced “Disk
7 p. 9
02/04/2004 3/F:” with “CDROM0/E”

Added, under “Procedures,” No. 10: Procedures Nos. 11-13

Approved
8 p. 9 14-19, 20-21
02/04/2004
Under “Validation Results,” No. 1: changed “Connect the
ATA test drive to a Linux system (using an Acard) and use
the md5sum utility to produce an md5sum for the test
Approved drive” to “Connect an Acard to the ATA test drive and
9 p. 10
02/04/2004 boot test machine with a Linux bootable CD-ROM. Run
the md5sum utility to produce an md5sum for the test
drive”

10 Approved p. 10 Under “Validation Results,” No. 1: changed content of table

454
 02/04/2004 under “Test Drive” – added “(ATA)” after Maxtor reference
(p.

Under “Validation Results,” No. 2: changed “Connect the

SCSI test drive to a Linux system and use the md5sum
utility to produce an md5sum for the test drive” to
Approved
11 p.10 “Connect an Acard to the SCSI test drive and boot test
02/04/2004
machine with a Linux bootable CD-ROM. Run the
md5sum utility to produce an md5sum for the test drive”

Under “Validation Results,” No. 2: changed content of table

Approved under “Test Drive” – added “(SCSI)” after Seagate Barracuda
12 p. 10
02/04/2004 Model reference

Under “This test procedure validated the test criteria”:

No. 1: deleted; replaced by No. 2
Approved No. 2: deleted; replaced by new No. 2
13 p. 11
02/04/2004 No. 3: retained
No. 4: new

Approved
14 All Reformatted entire document (jb)
02/04/2004
pp. 7, 9, Removed highlights from sections modified at the Feb. 2004
15 03/01/2004
10-15 meeting
Added the following final three (3) sentences to paragraph
16 04/14/2004 p. 2
under “When”
Under “Process,” deleted “Develop and document test
plan”; replaced with “Develop and document test plan
17 04/15/2004 p. 4
before testing begins. The test plan should contain the
following”:
Under “Process,” deleted old 1.a (“Shall be written before
testing begins”); replaced with new 1.a (“Purpose and
18 04/15/2004 p. 4
scope”).

Under “Process”, replaced old 1.b (“Document’s purpose

and scope”) with new bullet: “Requirements to be tested –
19 04/15/2004 p. 4
what does the tool have to do?”

Under “Process”, replaced old 1.c (“Develop and document

requirements to be tested – what does the tool have to
do?”) with new bullet: “Methodology – how to test?
20 04/15/2004 p. 4
(Identify support tools required to assist with evaluation
results when applicable)”

Under “Process”, replaced old 1.d (“Describe and document

21 04/15/2004 p. 4
methodology . . .”) with new bullet: “Test scenarios”

455
 Under “Process”, replaced old 1.e (“Identify and document
test scenarios”) with new bullet: “Test data to fulfill
conditions of test scenarios – can existing reference set data
22 04/15/2004 p. 4
be used? (Identify support tools required to assist with
developing test data when applicable)”

Under “Process”, replaced old 1.f (“Develop or identify test

23 04/15/2004 p. 4
data . . .”) with new bullet: “Document test data utilized”

Added boxed note

24 04/15/2004 p. 4
Under “Process”, replaced 2.a (“use media that is in a
known state”) with new bullet: “Use media and/or other
25 04/15/2004 p. 4
sample materials that are in a known state or condition”

Under “Process”, deleted “workaround” under Bullet 2.c

26 04/15/2004 p. 5 and added “alternative procedure”

pp. 10 - Added “SAMPLE” to all “Sample Test Plan” pages

27 05/12/2004
17
Revised footer to read “Final Version – Approved
28 05/12/2004 All 04/15/2004”

Revised cover page of document

29 05/12/2004 p. 1

456
 APPENDIX C - SWGDE GUIDELINES AND RECOMMENDATIONS FOR
TRAINING IN DIGITAL EVIDENCE

Version: 2.0
Drafted by Training: August 20, 2003
Revised by Training: February 3, 2004
Revised by Membership: February 4, 2004
Reformatted February 24, 2004
Revised March 1, 2004 (based on voter feedback)
Revised by Training: April 14, 2004
Membership: Send draft document to SWGIT (April 15, 2004)

Disclaimer:
As a condition to the use of this document and the information contained therein, the
SWGDE requests notification by e-mail before or contemporaneous to the introduction of
this document, or any portion thereof, as a marked exhibit offered for or moved into
evidence in any judicial, administrative, legislative or adjudicatory hearing or other
proceeding (including discovery proceedings) in the United States or any Foreign
country. Such notification shall include: 1) The formal name of the proceeding,
including docket number or similar identifier; 2) the name and location of the body
conducting the hearing or proceeding; 3) subsequent to the use of this document in a
formal proceeding please notify SWGDE as to its use and outcome; 4) the name, mailing
address (if available) and contact information of the party offering or moving the
document into evidence. Notifications should be sent to: execcmte@swgde.org.

Redistribution Policy:
SWGDE grants permission for redistribution and use of all publicly posted documents
created by SWGDE, provided that the following conditions are met:

1. Redistributions of documents, or parts of documents, must retain the

SWGDE cover page containing the disclaimer.

2. Neither the name of SWGDE, nor the names of its contributors, may be used to
endorse or promote products derived from its documents.

3. Any reference or quote from a SWGDE document must include the version number
(or create date) of the document and mention if the document is in a draft status.

There are many topics to include in digital forensic training for your workforce. There
are also many vehicles to provide training, such as in-service and out-service training and
distance learning. The recommendations for your training agenda are to provide your
employees and other workforce members with the information needed for them to do
their jobs within their discipline. The purpose of this document is to provide guidelines
and recommendations for such training.

457
It should be recognized that some agencies might choose to provide training other than
what is recommended in this section. In such circumstances, those agencies should
demonstrate and document that the training selected is adequate to meet their anticipated
needs.

Introduction

Personnel that encounter digital evidence must be aware of the capabilities and
limitations of specific technologies. Those engaged in the digital evidence process should
be aware of the procedures commonly followed within the forensics community and
should strive to meet or exceed these recommendations. They should also endeavor to
maintain awareness of new developments.

In support of these goals, the following recommendations are offered to personnel

engaged in forensics:

Define and employ quality assurance programs to ensure the implementation of valid and
reliable procedures for the task.

Maintain proficiency by pursuing continuing education courses in digital evidence

technology.

Maintain awareness of legal developments relating to digital evidence.

Maintain awareness of technological advancements.

Definitions of Categories

Several categories of digital evidence training relevant to those who encounter digital
evidence are identified and defined as follows:

Categories of training

Awareness: Training designed to provide the student with a general knowledge of the
major elements of digital evidence including, specific product capabilities

Skills and techniques: Training designed to provide the student with the ability to
competently use specific tools and procedures

Knowledge of processes and relationships: Training designed to provide the student

with an understanding of digital forensics and when to apply that understanding given
various situations

458
Court procedures:

Witness testimony: Training designed to provide the student with the ability to present
reliable digital evidence-based testimony in court

Case preparation: Training designed to provide the student with the ability to prepare
accurate and reliable exhibits

Continuing education: Training designed to provide personnel with ongoing training in

digital forensics

Specialized applications and technologies: Training in specific subdisciplines or in

specialized areas

Competency: A competency-testing program incorporates a number of components:

Required levels of skill and knowledge for a job category should be identified by the
agency. These levels should be driven by the requirements of the specific tasks to be
accomplished.

A course should be designed or identified by the agency or its agent to provide the skills
and information necessary for the agency's personnel to attain competency in those skills

If determined to be necessary by the agency, a competency test should be developed and

administered to test these skills.

Different types of competency tests may be developed depending on the various skills
required

Job categories

Management: Includes personnel who are responsible for setting agency policies and/or
making budget decisions

Command/Supervision: Includes personnel who supervise and/or direct personnel

engaged in the field of digital forensics

Examiner: Includes personnel for whom digital evidence recovery is a major component
of their routine duties. The personnel may be responsible for the collection of digital
evidence as a part of their duties as well as responsible for the analysis of the evidence.

Technician: Includes personnel who prepare digital evidence for examination and
analysis

First Responder: Includes personnel who are the first to secure, preserve and/or collect
digital evidence at the crime scene

459
Topical areas for focused training

The following section delineates specific topical areas in which personnel should receive
focused training to effectively fulfill their digital forensic duties. It should be noted that
in some instances a single person might occupy multiple job categories.

Managers, commanders/supervisors

Status of digital evidence technology

Legal issues

Industry, market and user trends for new and emerging technologies

Sources of digital evidence used in criminal activity

Description of core technologies

Basic forensic science

Basic digital technology

Strengths and limitations in media imaging

Strengths and limitations of digital forensic tools (e.g. hardware and software)

Strengths and limitations of personnel capabilities

Competency and continuing education with respect to current digital technology

Psychological stress

Current life cycle-cost comparisons and limitations hardware and software

Strategic alternatives

Contact procedure for technical support

References/information sources

Examiner

Recognize the presence of other forms of physical evidence not related to digital
evidence such as fingerprints and/or other types of biological evidence

460
Understand agency procedure for handling physical evidence

General training

Safety issues

Maintain chain of custody and data integrity

Ethics

General forensic principles and practices

Evidence handling (to preserve integrity of evidence)

Court testimony skills

Admissibility (Daubert) hearing testimony (issue awareness)

Quality assurance (consistency within the forensic community)

Basic crime scene management (understanding scene and evidence complexity)

Technical writing

“Best Practices” (i.e., technical procedures)

SOP’s

Position specific training relevant to the specific sub-discipline should include the
following:

Audio

Hardware

Types

Recognition

Tools

Media types

Software

Applications

461
File identification

Operating systems

Malicious code recognition

Storage formats

Logical

Physical

File systems

Scientific and technical foundations

Basic digital theory

Frequency fundamentals

Sound

Hearing

462
Computer Forensics

Hardware

Types

Recognition

Tools

Media types

Installation and configuration

Software

Applications

File identification

Operating systems

Malicious code recognition

Networks

Network topology

NOS types

Network security

Internet infrastructure and protocol

Storage formats

Logical

Physical

Partitioning

File systems

463
Forensic analysis procedures

Scientific and technical foundations

Data interface technology

Operating system technologies

Operating system fundamentals

Installation, configuration, and upgrading

Diagnosing and troubleshooting

Networks

Core hardware objectives

Installation, configuration, and upgrading

Diagnosing and troubleshooting

PC preventive maintenance, safety, and environmental issues

Motherboard, processors, and memory

Basic networking

Image Analysis (TBD)

Video (TBD)
Technician
Safety Issues
Recognize the presence of other forms of physical evidence not related to digital
evidence such as fingerprints and/or other types of biological evidence
Contact procedure for technical support (i.e., who to call)
Identification of digital evidence
Media types and remain current of new media formats technologies
Evidence handling (to preserve integrity of evidence)
Use of tools for media acquisition (hardware and software)
Maintenance of the chain of custody
Demonstration of competency (written or practical exam)
First Responders
Safety issues

464
Recognize the presence of other forms of physical evidence not related to digital
evidence such as fingerprints and/or other types of biological evidence
Contact procedure for technical support (who to call)
Recognize the presence of digital evidence at the crime scene
Proper collection and preservation techniques
Creation and maintenance of the chain of custody
Demonstration of competency (written or practical exam)
Issues to consider when addressing training needs

A number of issues should be considered when addressing an agency's training needs.

The following section provides guidance for selecting training providers and addressing
continuing education and testimony training needs.

Continuing education

Continuing education can be obtained from training conferences, trade shows, and
specialized courses. This training should address updates and the use of new technologies
as it relates to:

Hardware

Software

Techniques applicable to the digital evidence recovery process

Forensic procedures beneficial to digital evidence

Testimony training

This training should address the use of digital evidence in court using techniques such as:

Lecture-type presentation relevant to court testimony

Moot court

Court monitoring

Training documentation

To demonstrate compliance with training, conduct the following:

Develop a written training program

Provide a training syllabus

465
Document performance

Establish a formal means of recognition of successful completion of the training such as a

certificate, letter, or memorandum.

466
History: Guidelines and Recommendations for Training in Digital Evidence
Revision Issue Date Section
08/20/2003 All
1 02/04/2004 p. 2
2 02/04/2004 p. 2
3 02/04/2004 p. 2
4 02/04/2004 p. 2
5 02/04/2004 p. 2
6 02/04/2004 p. 2
7 02/04/2004 p. 2
8 02/04/2004 p. 2
9 02/04/2004 p. 3
10 02/04/2004 p. 3
11 02/04/2004 p. 3
History
Document drafted (August 20, 2003)
Under “Introduction,” replaced “in the work with
digital evidence” with “that encounter”
Under “Introduction,” replaced “computer” with
“digital”
Under “Introduction,” replaced “evidence recovery”
with “forensics”
Under “Introduction,” added a fourth bullet: “Maintain
awareness of technological advancements”
Under “Definition of Categories,” replaced “would
benefit from the training” with “encounter digital
evidence”
Under “Categories of Training”:
“Knowledge of processes and relationships”: replaced
“evidence recovery” with “forensics” Court procedures:
replaced “the student” with “personnel”
Continuing education: replaced “evidence recovery”
with “forensics”
Under “Categories of Training”:
Replaced “Specialized applications” with “Specialized
Applications and Technologies”
Under “Categories of Training,” “Specialized
Applications and Technologies”:
Replaced “disciplines” with “sub-disciplines”
Replaced “Categories of Users” with “Job Categories”
Under “Job Categories”:
Command/Supervision: replaced “in the use of digital
evidence” with “in the field of digital forensics”
Under “Job Categories,” moved “First Responder”
from the third bullet to the last
467
 Under “Job Categories,” moved “Examiner” to the third
12 02/04/2004 p. 3 bullet

Under “Job Categories,” moved “Technician” to the

13 02/04/2004 p. 3 fourth bullet

Under “First Responder,” replaced “preserve and/or

collect digital evidence from the scene” with “secure,
14 02/04/2004 p. 3 preserve and/or collect digital evidence at the crime
scene”

Under “Examiner,” removed “are not only” and added

15 02/04/2004 p. 3 “as well as”

Under “Topical Areas for Focused Training”:

Replaced “user groups” with “personnel” Replaced
“evidence recovery” with “digital forensic” Added “It
16 02/04/2004 p. 3
should be noted that in some instances, a single person
might occupy multiple job categories”

Under “Managers, Commanders/Supervisors,” “Status

of digital evidence technology”:
17 02/04/2004 p. 3 Deleted bullet “Extent of use and who are the users”
Deleted bullet “Industry and market trends”

Under “Managers, Commanders/Supervisors,” “Status

of digital evidence technology”:
Added two (2) new bullets:
“Industry, market and user trends for new and
18 02/04/2004 p. 3
emerging technologies”
“Sources of digital evidence used in criminal activity”

Under “Managers, Commanders/Supervisors,”

“Description of core technologies”:
19 02/04/2004 p. 3 Added the bullet “Basic Digital Technology”

Under “Managers, Commanders/Supervisor”, “Basic

Digital Technology”:
Revised bullet to read “Strengths and limitations of
20 02/04/2004 p. 3
digital forensic tools”

21 02/04/2004 p. 3 Under “Managers, Commanders/Supervisors”,

468
 “Strengths and limitations personnel capabilities”:
Revised bullet to read “Competency and continuing
education with respect to current digital technology”

Under “First Responders”:

Replaced the bullet “Recognizing physical evidence
such as fingerprints and/or blood spatter” with
“Recognize the presence of other forms of physical
evidence not related to digital evidence such as
fingerprints and/or other types of biological evidence
Deleted the bullet “Review available
22 02/04/2004 p. 3
publications/training materials addressing seizure of
digital evidence”
Added “who to call” to the end of the bullet “Contact
procedure for technical support” Replaced the bullet
“Identification of digital evidence; recognize, secure,
and seize” with “Recognize the presence of digital
evidence at the crime scene”
Under “Technician”:
Replaced the bullet “Recognizing physical evidence
such as fingerprints and/or blood spatter” with
“Recognize the presence of other forms of physical
23 02/04/2004 p. 4
evidence not related to digital evidence such as
fingerprints and/or other types of biological evidence”
Deleted the bullet “Safety Issue”

Under “Examiner”:
Added the bullet “Recognize the presence of other
forms of physical evidence not related to digital
24 02/04/2004 p. 4
evidence such as fingerprints and/or other types of
biological evidence”

Under “Examiner,” “General Training”:

Add two (2) bullets:
25 02/04/2004 p. 4 “Best Practices” (Technical Procedures)”
“SOP’s”

Under “Examiner”:
Revised the bullet “Position specific training should
include the following” to read “Position specific training
26 02/04/2004 p. 4
relevant to the specific sub-discipline should include the
following”

Under “Examiner,” “Position specific training relevant

27 02/04/2004 p. 4 to the specific sub-discipline should include the
following,” “Software”:

469
 Added the bullet “Malicious code recognition

Under “Examiner,” “Position specific training relevant

to the specific sub-discipline should include the
28 02/04/2004 p. 4
following”:
Added “if applicable” after “Networks

Under “Examiner”:
Deleted the bullet “Relevant Applications”
29 02/04/2004 p. 4 Deleted the bullet “Relevant Media (Digital/Analog)”
Replaced the bullet “Disk Geometry” with “Digital
Storage Formats”

Replaced blue text with black text throughout document

30 03/01/2004 All
per voter feedback

Under “Introduction,” deleted “digital” from “digital

31 04/14/2004 p. 2
forensics” (first paragraph, second paragraph)

Deleted “recovery” from “digital evidence recovery

32 04/14/2004 p. 2
technology” (second bullet)

Deleted “recovery” from “digital evidence recovery

33 04/14/2004 p. 4
examination” (see definition for “Examiner”)

34 04/14/2004 p. 6 Under “Examiner,” added “Audio” category

Moved “Networks” bullet to “Computer Forensics”

35 04/14/2004 p. 6
(new category under “Examiner” on p. 7)

Moved the “Digital Storage Formats” bullet under

“Examiner” to new category (“Computer Forensics”)
36 04/4/2004 p. 6
with new title “Storage Formats,” still under
“Examiner”

Moved “Forensic Analysis Procedures” bullet to new

37 04/14/2004 p. 6
category under “Examiners”: “Computer Forensics”

470
 Added new category under “Examiners”: “Computer
38 04/14/2004 p. 7
Forensics”

Added bullet “Scientific and Technical Foundations”

39 04/14/2004 p. 7-8
under “Examiner,” “Computer Forensics”

Added “Image Analysis” and “Video” under

40 04/14/2004 p. 8 “Examiner,” “Computer Forensics”; terms still need to
be defined

41 05/12/2004 All Reformatted entire document

42 05/12/2004 p. 1 Changed document version to 2.0 (from 1.0)

471
 APPENDIX D - SWGDE/SWGIT RECOMMENDED GUIDELINES FOR
DEVELOPING STANDARD OPERATING PROCEDURES

Disclaimer:
As a condition to the use of this document and the information contained therein, the
SWGDE/SWGIT request notification by e-mail before or contemporaneous to the
introduction of this document, or any portion thereof, as a marked exhibit offered for or
moved into evidence in any judicial, administrative, legislative or adjudicatory hearing or
other proceeding (including discovery proceedings) in the United States or any Foreign
country. Such notification shall include: 1) The formal name of the proceeding,
including docket number or similar identifier; 2) the name and location of the body
conducting the hearing or proceeding; 3) subsequent to the use of this document in a
formal proceeding please notify SWGDE/SWGIT as to its use and outcome; 4) the name,
mailing address (if available) and contact information of the party offering or moving the
document into evidence. Notifications should be sent to: execcmte@swgde.org.

Redistribution Policy:
SWGDE/SWGIT grant permission for redistribution and use of all publicly posted
documents created by SWGDE/SWGIT, provided that the following conditions are met:

1. Redistributions of documents, or parts of documents, must retain the

SWGDE/SWGIT cover page containing the disclaimer.

2. Neither the name of SWGDE/SWGIT, nor the names of its contributors, may be
used to endorse or promote products derived from its documents.

3. Any reference or quote from a SWGDE/SWGIT document must include the

version number (or create date) of the document and mention if the document is in a draft
status.

472
Recommended Guidelines for Developing Standard Operating Procedures

Introduction:
Standard Operating Procedures (SOPs) are agency unique documents describing the
methods and procedures to be followed in performing routine operations. SOPs are
essential to improve the quality and to implement uniform processes for conducting
digital & multimedia evidence forensic tasks in a precise, accurate manner. SOPs should
be task-based and written for each procedure conducted. They should be reviewed at
least annually. The previously approved versions of an SOP should be retained for
reference.

Scope:
SOPs should conform to agency-specific policies. Such policies may address document
format, workflow, approval process, and tasks performed. SOPs may be stored
separately, in one large collected manual, or organized by functional unit. For instance, a
single manual may be more convenient, but having separate SOP documents may be
more amenable to the discovery process. SOPs should contain all information necessary
to perform the task being described. Individual agency needs and/or processes will dictate
what information is necessary.

General Guidelines:
SOPs may include but are not limited to:

The name of the SOP, effective date and/or other version control.
The purpose and scope of the SOP.
Definitions and abbreviations that are not commonly used or have a special connotation
in the SOP. The source of these definitions should be cited.
A list of equipment, materials and standards/controls. Note: Since equipment and
material lists are frequently updated, it may be beneficial to create a separate listing of
this equipment. This will allow for a document that can be updated independent of the
SOP. Equipment calibration and similar preparatory steps, if applicable.
Any known limitations of the equipment, software or procedure.
A list of steps used in performing the task, including appropriate parameters or options to
be used.
Appropriate references. This may include equipment manuals, other published
procedures, journal references, etc.
Any additional information/materials the examiner needs to be aware of that are not
already included in the sections above, such as safety issues or operational precautions.
Authorization and approval information.

Sample SOPs are provided for your reference. These are examples only and are not
meant to be boilerplate.

473
Sample Standard Operating Procedure
Wiping Media
Version: Draft 1.0 (08/2003)
Version: Revised Draft 1.1 (02/2004)
Version: Revised Draft 2.0 (4/2004)

Note: The sample standard operating procedures are given as an example only and are
not meant to be used without revision.

Introduction/Scope:
This procedure applies to wiping media for hard disk drives and other digital media. This
procedure applies to computer forensic examiners in this agency.

Purpose:
To completely erase by overwriting all data on digital media including both physical and
logical structures.

Equipment:

" Media to be wiped

" Examination station
" ABC software wiping utility (current or appropriate version)

Definitions:
Wiping - To completely erase by overwriting all data on digital media including both
physical and logical structures,

Calibration:
None

Limitations:
This procedure may not apply to all forms of media, such as tapes or diskettes.

Procedure:

1. Ensure the examination station is powered off.

2. Attach media to be wiped to examination station.

3. Power on the examination station.

4. Start wiping process utilizing appropriate software commands.

5. When process is complete, verify the media has been wiped.

6. Power off examination station.

474
7. Remove the media.

References:
ABC user manual for software wiping utility.

Notes:
Examiners should double check media before wiping to ensure no irreplaceable data will
be lost.

History:

Section
Revision Date Change
1.1 01/05/2004 Notes Spelling correction

This standard operating procedure has been approved for use.

Jane Doe
Approving Authority
Date

Sample Standard Operating Procedure

Video Processing

Note: The sample standard operating procedures are given as an example only and are
not meant to be used without revision.

Do a visual inspection of the tape and cassette housing to

Ensure housing is intact

Inspect tape for damage (e.g., twisting, separation)

If damage is found, take corrective action and document.

Enable any record-protection device (e.g., punch-out tab, slide record tab, remove record
button).

Determine if the submitted tape is an original or a copy. If it is an original, proceed to

Step 4. If it is a copy, contact the submitter and request that original tape be submitted,
and terminate examination of the copy. If the copy is the best available, proceed with the
examination.

475
Determine the make, model, and settings of the device used to record the submitted
video, if possible. These settings may include the recording format and speed.

Select the appropriate playback device(s) to achieve optimal signal quality.

Using the selected devices and settings, review the submitted video to locate the pertinent
segment(s).

Determine the appropriate playback speed for processing.

A time-base corrector may be used to stabilize the signal for playback and permit
adjustment of video, chroma, pedestal levels, or other signals.

At the examiner’s discretion, a working copy of the pertinent segment may be generated
using an available analog or digital device.

10. The images may be enhanced using a number of processing operations that may
include but are not limited to histogram equalization, multiframe averaging, contrast and
levels adjustments, and sharpening.

Once enhanced, the final images are output to appropriate media.

476
History: SWGDE/SWGIT Recommended Guidelines for Developing Standard
Operating Procedures for Digital Forensic Examinations

Revision Issue Date Section History

08/20/2003 All Document drafted August 20, 2003

Defined “Purpose” of the document; added
“Recommended” to “Guidelines for Developing
1 02/03/2004 p. 2
Standard Operating Procedures (SOP) for Digital
Forensic Examinations”
Included the title “Recommended Guidelines for
2 02/03/2004 p. 2 Developing Standard Operating Procedures for
Digital Forensic Examinations” below “Purpose”
3 02/03/2004 p. 2 Changed “is” to “are”
Revised the explanation of Standard Operating
Procedures to include as the last sentence, “The
4 02/03/2004 p. 2 previously approved versions of a standard
operating procedure should be retained for
reference.”
Added the section “Limitations” between
“Calibration” and “Procedure”; explained
5 02/03/2004 p. 3 “Limitations” as “Any known limitations of the
equipment or procedure should be listed in this
section.”
6 02/03/2004 p. 3 Replaced “Procedures” with “Procedure.”
Revised the explanation for “Procedure”; added the
last sentence, “This section should include the
7 02/03/2004 p. 3
appropriate parameters or options to be used during
the procedure’
Revised the “Notes” section to include the following, “.
8 02/03/2004 p. 3
. . such as safety issues or operational precautions.’
Added an “Approval Statement”: This statement
should contain the signature of the individuals with
9 02/03/2004 p. 3
authority to approve the use of the Standard
Operating Procedure and the date of the signature.
Added a “Note” stating, “The sample standard
10 02/03/2004 p. 3 operating procedures are given as an example only
and are not meant to be used without revision.”
Under “Sample SOP: Wiping Media,” added a
“Limitations” section between “Calibration” and
11 02/03/2004 p. 4
“Procedure.” The “Limitations” section reads, “This

477
 procedure may not apply to all forms of media, such
as tapes or diskettes”
Under “Sample SOP: Wiping Media,” added under
12 02/03/2004 p. 5 “Notes”: “This standard operating procedure has
been approved for use”
Added “Jane Doe, Approving Authority, and Date” at
13 02/03/2004 p. 5 the end of the “Sample SOP: Wiping Media”
document
14 02/03/2004 pp. 6-7 New SOP: “Video Capture Procedure”
15 02/03/2004 pp.8-9 New SOP: “Archiving Digital Images”
16 02/25/2004 All Document reformatted (jb)
Removed names of members from page 2 (per voters’
request); replaced all words in blue text with black text
17 03/01/2004 All
(per voters’ request); pagination is different from Feb.
2004 document due to modifications made to p. 2
Added text box, “The SWGDE Recommended
Guidelines for Developing Standard Operating
Procedures (SOP) for Digital Forensic Examinations
were written to provide agencies with a suggested
format for writing a SOP. The committee
intentionally left the procedure sections vague.
18 04/13/2004 p. 2
Other professional organizations and scientific
groups have made recommendations as to the steps
to be followed during the actual examination.
SWGDE recommends that agencies refer to the
public documents published by those organizations
to determine the best procedures to follow.”
Under “Title,” changed “date of release” to “effective
19 04/13/2004 p. 2
date.”
Under “Procedure,” added, “If procedures are
20 04/13/2004 p. 3 numbered, this is an indication that the steps have a
specific order.”
Revised “Note”: replaced “The sample standard
operating procedures are given as an example only
and are not meant to be used without revision” with
21 04/13/2004 p. 3
“The sample standard operating procedures are
given as an example structure only; the content is
not meant to be used without revision.”
Added “Note” to “Sample SOP: Wiping Media”, “The
sample standard operating procedures are given as
22 04/13/2004 p. 4
an example only and are not meant to be used
without revision.”
Under “Sample SOP: Wiping Media,” changed title
“Introduction” to “Introduction/Scope”
23 04/13/2004 p. 4
Under “Introduction/Scope,” replaced “The sample
standard operating procedures are given as an

478
 example only and are not meant to be used without
revision” with “This procedure applies to wiping
media for hard disk drives and other digital media.
This procedure applies to computer forensic
examiners in this agency.”
Under “Sample SOP: Wiping Media,” “Calibration,”
24 04/13/2004 p. 4
changed “Not applicable” to “None.”
Under “Sample SOP, Wiping Media,” “Limitations,”
25 04/13/2004 p. 4 changed “(tapes, diskettes, SAN etc.)” to “such as
tapes or diskettes.”
Under “Sample SOP, Wiping Media,” added “History”
26 04/13/2004 p. 5 section
Added table under “History”
Under “Sample SOP, Video Capture Procedure,” added
boxed text, “The sample standard operating
27 04/13/2004 p. 6 procedures are given as an example structure only;
the content is not meant to be used without
revision.”
Under “Sample SOP, Video Capture Procedure,”
replaced title “Introduction” with
“Introduction/Scope”
28 04/13/2004 p. 6
Under “Sample SOP, Video Capture Procedure,”
“Introduction/Scope,” replaced “video forensic
examiner” with “forensic video examiner.”
Under “Sample SOP, Video Capture Procedure,”
“Purpose,” replaced “To describe the procedure to
29 04/13/2004 p. 6 capture and maximize the quality of the video signal
captured” with “To capture and maximize the
quality of the video signal capture.”
Under “Sample SOP, Video Capture Procedure, added
30 04/13/2004 p. 7
after “Procedure No. 5”: “and calibrate.”
Under “Sample SOP, Video Capture Procedure,”
31 04/13/2004 P. 7 “Procedure No. 7,” replaced “minimize” with
“maximize”
Under “Sample SOP, Video Capture Procedure,” added
32 04/13/2004 p. 7
a “History” section
Added boxed text to “Sample SOP, Archiving Digital
33 04/13/2004 p. 8
Images.”
Under “Sample SOP, Archiving Digital Images,”
34 04/13/2004 p. 8 replaced title “Introduction” with
“Introduction/Scope”
Under “Sample SOP, Archiving Digital Images,”
“Purpose,” replaced “The digital images are to be
35 04/13/2004 p. 8 transferred to the archival media and verified the
image files can be opened” with “To transfer the
digital images to the archival media and verify that

479
 the images can be opened.”
Under “Sample SOP, Archiving Digital Images,” added
36 04/13/2004 p. 9
“History” section
37 04/13/2004 Added “Sample” to all SOP pages
All
Whole document rewritten by joint SWGDE/SWGIT
38 07/22/2004
All committee

Drafted by the Forensic Committee: August 20, 2003

Modified by the Forensic Committee: February 3, 2004
Reformatted February 24, 2004
Revised March 1, 2004 (based on SWGDE voter feedback)
Revised by the Forensic Committee: April 13, 2004
Reformatted May 10, 2004
Rewritten by SWGDE/SWGIT July 22, 2004

480
 APPENDIX E - PROFICIENCY TEST PROGRAM GUIDELINES

Version: Draft
Drafted by Standards/Accreditation: February 4, 2004
Reformatted February 24, 2004
Revised by Standards/Accreditation: April 14, 2004
Reformatted May 17, 2004
Revised by SWGDE/SWGIT July 21, 2004

Disclaimer:
As a condition to the use of this document and the information contained therein, the
SWGDE requests notification by e-mail before or contemporaneous to the introduction of
this document, or any portion thereof, as a marked exhibit offered for or moved into
evidence in any judicial, administrative, legislative or adjudicatory hearing or other
proceeding (including discovery proceedings) in the United States or any Foreign
country. Such notification shall include: 1) The formal name of the proceeding,
including docket number or similar identifier; 2) the name and location of the body
conducting the hearing or proceeding; 3) subsequent to the use of this document in a
formal proceeding please notify SWGDE as to its use and outcome; 4) the name, mailing
address (if available) and contact information of the party offering or moving the
document into evidence. Notifications should be sent to: execcmte@swgde.org.

Redistribution Policy:
SWGDE grants permission for redistribution and use of all publicly posted documents
created by SWGDE, provided that the following conditions are met:

1. Redistributions of documents, or parts of documents, must retain the SWGDE

cover page containing the disclaimer.

2. Neither the name of SWGDE, nor the names of its contributors, may be used to
endorse or promote products derived from its documents.

3. Any reference or quote from a SWGDE document must include the version
number (or create date) of the document and mention if the document is in a draft status.

Proficiency Test Program Guide

Purpose
To provide a guide to implement a Digital and Multimedia Evidence (DME) proficiency
test program.

481
Scope
The proficiency test program, which is one component of a Quality Assurance program,
should verify that the technical procedures are valid and that the quality of each
examiner’s work is being maintained.

Subdisciplines
Computer Forensics
Forensic Audio
Video Analysis
Image Analysis

Test Preparation and Design

Proficiency tests may be internal or external, open or blind. Tests shall be subdiscipline
specific, process based, and representative of items routinely examined. The test shall be
prepared and anticipated results documented by an individual or organization identified
by the tested agency as technically knowledgeable in the subdiscipline. A second
individual identified by the tested agency as technically knowledgeable in the
subdiscipline shall confirm the suitability for testing, the completeness of the test and
anticipated results. The test should be representative of routine DME casework. It should
be noted that Examiners and technical support personnel need only demonstrate
proficiency in those processes which are representative of their routine activities.
Furthermore, examiners need not demonstrate competency in all of the processes
listed in order to be considered qualified to perform individual examination
processes.

482
The proficiency test may include, but is not limited to, one or more of the processes listed
below.
Computer Forensic Audio Video Analysis Image Analysis
Forensics
Write Protect Write/Record Protect Write/Record Protect Write/Record Protect
Media Media Characterization Media Characterization Media Characterization
Characterizatio
n
Physical Duplicate/Copy Duplicate/Copy Reconstruction/Recovery
/Logical Copy
Restoration Reconstruction/Recovery Reconstruction/Recovery Image Restoration
Directory Playback Optimization Playback Optimization
Listing
Erased File Data Extraction Data Extraction Authentication
Recovery
Residue Data/Signal Analysis Data Analysis Enhancement
Extraction
Search by Enhancement Enhancement Timeline Reconstruction
Criteria
Internet Authentication Authentication Image Content Analysis
Activity
Password Voice Analysis Demonstrative Report of Findings
Recovery Comparison
Verification Report of Findings Photogrammetry Photogrammetry
Identification Format/Standard Timeline Sequencing Duplicate/Copy
and/or recovery Conversion Reconstruction
of hidden
information
Identification Report of Findings Photographic
and/or recovery Comparison
of encrypted
data
Report of Format/Standard Demonstrative
Findings Conversion Comparison
DeMultiplex
Image Restoration
Photographic
Comparison
Image Content Analysis

Test Approval
Test preparation documentation, test design, and anticipated results will be provided to an
individual technically knowledgeable in the subdiscipline and the quality assurance
personnel for approval.

483
Distribution
Personnel actively performing or technically assisting in examinations will be required to
successfully complete at least one proficiency test annually. The unit must participate in
one external proficiency test annually. It is recommended that personnel be tested
annually in each subdiscipline in which they actively perform or technically assist in
examinations.

Testing Process
Proficiency tests will be conducted according to the agency approved protocols in effect
at the time of the proficiency test.

Review of Test Results

The results and supporting documentation will be evaluated by qualified personnel
identified by the agency. Additionally, results and the evaluation will be provided to the
management and reviewed with the individual tested.

Documentation
The proficiency test results and supporting documentation will be retained in accordance
with the agency’s documentation retention policy.

Corrective Action
Inconsistencies in the proficiency test results will be resolved in accordance with the
corrective action policy of the agency’s DME program. The corrective action policy
should address inadequacies of the test, process, and the tested individual.

484
GLOSSARY:

Authentication: The process of determining whether a recording or image is

original continuous, free from unexplained alterations (additions, deletions, edits, or
artifacts), and consistent with the stated operation of the recording device used to make it.

Blind Proficiency Test: Proficiency test in which the analyst is unaware of the test
nature of the sample at the time of the analysis.

Computer Forensics:The application of science and engineering to the legal problems of

digital evidence. (SWGDE)

Copy/ Duplicate: An accurate reproduction of information contained in the data

objects independent of the original physical item.

Data/Signal Analysis: a. Audio, analysis of non-voice signals to identify,

compare, and interpret these signals. Recordings might include gunshots or DTMF
(telephony) signaling for analysis. (FBI FAVIAU)

b. Video (Define)

Digital Evidence (DE): Information of probative value stored or transmitted in

binary form. (SWGDE)

Directory Listing: A list of all the files on media. It may also contain other
information such as the size of the files and amount of free space remaining. (Newton’s
Telecom Dictionary)

Enhancement: Processing of recordings for the purpose of increased

intelligibility, attenuation of noise, improvement of understanding the recorded material,
and improvement of quality or ease of hearing or viewing.

Erased File Recovery: The process for recovering deleted files.

External Proficiency Test: A proficiency test managed and controlled outside to the
agency. (Consistent with ASCLD/LAB)

File Slack: Space between the logical end of the file and the end of the last allocation
unit for that file. (TWGEDE document)

Image:a. An accurate digital reproduction of all data contained on a digital storage

device (e.g. hard drive, CD-ROM, flash memory, floppy disk). Maintains contents and
attributes. (TWGEDE)

485
b. An imitation or representation of a person or thing, drawn, painted, photographed, etc.
(Webster /SWGIT)
Image Analysis: Image Analysis is the application of subject matter expertise to the
interpretation of subjects or objects depicted in images. It can also include the
application of image science expertise to the extraction of information from images, the
characterization of image features, and the interpretation of image structure.

Image Restoration Any process applied to an image that has been degraded by a
known cause, such as defocus or motion blur, so the effects of that degradation are
partially or totally removed.

Internal Proficiency Test: A proficiency test managed and controlled within the DE
unit. (Consistent with ASCLD/LAB)

Media: Objects on which data can be stored. (Computerwords.com/ SWGDE)

Media Characterization: The process of inspecting, identifying, and noting the

physical and/or logical properties of the media.

Open Proficiency Test: A proficiency test in which the person being tested is aware
the sample is a test.

Password Recovery: The process of locating and identifying a series of

characters used to prevent access to data.

Photogrammetry: Photogrammetry is the art, science, and technology of obtaining

reliable information about physical objects and the environment through the processes of
recording, measuring, and interpreting photographic images and patterns of
electromagnetic radiant energy and other phenomena.” [from “The Manual of
Photogrammetry, 4th Edition, 1980, ASPRS]. In forensic applications, photogrammetry
(sometimes called “mensuration”) most commonly is used to extract dimensional
information from images, such as the height of subjects depicted in surveillance images
and accident scene reconstruction. Other forensic photogrammetric applications include
visibility and spectral analyses.

Photographic Comparison: Assessment of the correspondence between features in

images and known objects for the purpose of rendering an opinion regarding
identification or elimination.

Playback Optimization: The process of determining the most suitable equipment

and settings for analyzing the output signal.

Reconstruction/Recovery: The process of repairing damaged media or file formats in

order to allow the retrieval of data.

486
Restoration: The process of restoring data from an image/copy to it’s original state.

Residue: Data contained in unallocated space or unused allocated space or file

slack. (SWGDE 1/15/03)

Timeline/Sequence Reconstruction: The process of relating data, images, and/or

audio to one another in an ordered succession.

Verification: The process of confirming the accuracy of the data to the original
evidence.

Video Analysis: The scientific examination, comparison and or evaluation of video.

Write Protect: Hardware and/or software methods of preventing modification of

media content.

Note: Determine which terms/words found in this document need to be defined. Use
definitions across the subdisciplines when possible. Breakout to separate definitions
where needed. Rec’d input from some of the SWGIT members Jan. 2003 and have
included above.

Technical Work Group Examination of Digital Evidence

487
History: SWGDE Proficiency Test Program Guidelines

Revision Issue Date Section History

02/04/2004 All Document drafted Feb. 4, 2004

1 02/04/2004 Glossary Deleted “Digital Evidence Examiner” (p. 5,

reformatted document).

2 02/04/2004 Glossary Deleted “Image Comparison” (p. 6, reformatted

document).

3 02/04/2004 Glossary Deleted “Internet” (p. 6, reformatted document).

4 02/04/2004 Glossary Deleted “the best rather than proper?” from the
“Playback Optimization” definition (p. 7,
reformatted document).

5 02/04/2004 Glossary Deleted “Search by Criteria” (p. 7, reformatted

document).

488
APPENDIX F - U.S. DEPARTMENT OF JUSTICE

Federal Bureau of Investigation

Washington, D. C. 20535

July 2, 2001

Dear Colleague,
The Scientific Working Group on Imaging Technologies (SWGIT) was created to
provide leadership to the law enforcement community by developing guidelines for good
practices for the use of imaging technologies within the criminal justice system. In this
issue of Forensic Science Communications, we present one such document relating to
those guidelines for your review.
This document, "Definitions and Guidelines for the Use of Imaging Technologies in the
Criminal Justice System," was previously released as a draft in 1999 for public review
and comment. Based on the resulting feedback, we revised the document and now present
a final version.
This document represents the work of more than 30 photographers, scientists, instructors,
and managers from more than two dozen federal, state, and local law enforcement
agencies, as well as from the academic and research communities. The document
represents the consensus opinion of this membership and should not be construed as the
official policy of any one of the represented agencies.
A goal of the SWGIT is to engage the entire law enforcement imaging community in the
development of these guidelines. Please review this document carefully and give us your
feedback. Instructions are attached.
Thank you for your consideration.

Sincerely,

Richard W. Vorder Bruegge

Chair, SWGIT

489
APPENDIX F - GUIDELINES FOR FIELD APPLICATIONS OF IMAGING
TECHNOLOGIES IN THE CRIMINAL JUSTICE SYSTEM

Scientific Working Group on Imaging Technologies (SWGIT)

Version 2.3, December 6, 2001

Introduction
The purpose of this document is to:
Provide specific recommendations and guidelines for the use of imaging technologies in
law enforcement field applications.
Describe the advantages and disadvantages of silver-based film cameras, instant
photography cameras, digital still cameras, video cameras, and hybrid imaging systems in
law enforcement field applications.
Provide general guidelines for preparing agency-specific imaging technologies standard
operating procedures (SOPs) for law enforcement field applications.
Provide imaging equipment recommendations.
This document addresses the photographic documentation of events or subjects that are
not in a controlled environment (e.g., forensic laboratory or studio).
The field applications addressed in this document include the following imaging:
General crime scene photography
First responder (FR) photography
When crime scene photography personnel will not be called
Prior to arrival of crime scene photography personnel
Surveillance photography
Tactical surveys
Hazardous materials (HAZMAT) crime scene photography
Aerial photography
Accident scenes
Arson photography
Autopsy photography
Bomb scene photography
Mass disaster photography
Search warrant photography
Gang-related graffiti photography (FR)
Field mug shots and tattoos (FR)
Victim photography

Advantages and Disadvantages of Major Image Capture Technologies in Field

Applications

The selection of an acquisition device (camera) is driven by the purpose and requirements
of the end product. Therefore, the final use of the image should determine the choice of
the camera.
The recommendations for primary and secondary image capture devices are dependent on
current technology and may change subject to changes in technology. These
recommendations are made based on the practical experience of the SWGIT membership

490
in the acquisition and analysis of the images discussed herein. Agencies should decide
what technologies are best suited to meet the requirements of their mission-specific tasks.
As long as an agency can demonstrate and document that its choice of technologies is
adequate to meet its anticipated needs, the agency should not feel required to adhere to
the SWGIT recommendations.

Silver-Based Film Cameras

It is strongly recommended that a camera capable of manual override, with
interchangeable lenses, off-camera flash, and a tripod mount be used as the primary
capture device along with conventional silver-based film in 35 mm format or larger as the
primary capture media for evidentiary photography/imaging.
Advantages of silver-based film cameras in field applications:
Highest resolution of available image capture options
Highest dynamic range of available image capture options
Best color range of available image capture options
Most flexibility of currently available image options
Most durable storage medium
More readily available in the field than video or digital storage media
Disadvantages of silver-based film cameras in field applications:
Need for separate processing/printing facilities
Relatively long processing time
Environmental hazards generated by processing byproducts
Preprocessing fragility (i.e., temperature, humidity, x-ray effects, expiration)
No means of immediate image evaluation (with the exception of instant film)

Discussion
Resolution: The best measure of resolution is the evaluation of output imagery, which is
the product of a series of steps. However, since this document is devoted to field
applications, the following discussion is restricted to camera evaluation only. Users
should verify resolution by visually examining images of test targets in their specific
environments.

SWGIT uses the following definitions of resolution: "Measure of capability to delineate

picture detail;" and "The ability of a photographic system to record fine detail." These
definitions are a subset of those found in ANSI/A Technical Report TR26-1993:
Resolution as it Relates to Photographic and Electronic Imaging.

Traditionally, film manufacturers measure resolution in terms of line pairs per millimeter
(LP/mm) or lines per millimeter. Lines per millimeter refers to each line (black or white),
thus there are always twice as many lines as there are line pairs over a given distance.
Manufacturers of digital cameras frequently describe image size in terms of number of
pixels. As stated in ANSI/A TR26-1993, "There is a common practice of referring to
digital resolution as simply the total number of pixels within a frame or field, or
alternately as the number of pixels in the horizontal and vertical directions. Alone, this
information is useful to indicate the amount of data that can be handled in a single field at
a given moment, but tells nothing about the unit's ability to resolve spatial information."

491
(Note that the words frame and field in the quote refer to a photographic field of view.
These should not be confused with the terms used in video technology.)

The ability to resolve spatial information can only be determined by testing a specific
imaging system. In order to compare technologies, the total information that can be
represented in the sensor is discussed. This constitutes an upper limit to the actual
achievable resolution.

It is possible to directly compare the maximum amount of information that can be

represented by any two sensors by comparing the total number of pixels per frame. To
compare film to the sensors in digital cameras (CCD/CMOS), it is necessary to relate line
pairs per frame to pixels per frame.
Common film types encountered in law enforcement field applications have optimal
resolutions in the range of 40 - 160 line pairs per millimeter. Black and white films
typically used at crime scenes have resolutions at the upper end of this range. Color films
used at crime scenes have resolutions at the lower end of this range.
A single frame of 35 mm ISO 200 color film is 36 mm wide by 24 mm high. With a
resolution of 50 line pairs per millimeter, such a frame can resolve the following:

36mm x 50 LP/mm = 1800 line pairs horizontally and 24mm x 50 LP/mm = 1200 line
pairs vertically.
The equivalent number of pixels in a single frame is then calculated:
1800 line pairs x 2 pixels/line pair = 3600 pixels horizontally and
1200 line pairs x 2 pixels/line pair = 2400 pixels vertically.
This represents a total of 3600 x 2400 = 8,640,000 pixels.
A digital camera with a detector that is 3040 x 2008 pixels in size contains more than six
million (6,104,320) pixels. This is referred to as a 6-megapixel camera.

There is a tradeoff between the field of view and the resolution that can be represented by
a sensor. If the field of view is held constant, then the resolution will vary with the
number of pixels. If resolution is held constant, then the field of view will vary with the
number of pixels.
If the field of view is held identical for both sensors above (35 mm ISO 200 color film
and a 6-megapixel CCD), the film, with 40 percent more pixels than the CCD (8.64
million versus 6.1 million), will provide an improvement in resolution of approximately
20 percent.

Alternatively, if the resolution is held constant for both sensors, the film will cover a field
of view that is 40 percent larger than the CCD.

The resolution that can be achieved in a digital camera will be lower than the upper limit
(ideal conditions) discussed above. Some research has found that it takes approximately
four pixels to capture and reproduce a line pair under test conditions, instead of the
representation by two pixels. Using this standard, the pixel resolution of film is
effectively doubled.

492
NOTE: Discussing the resolution of video systems is beyond the scope of this document.
SWGIT will address issues relating to video resolution in future documents. To compare
the size of images generated from each of these sensors, a common output resolution
must be defined. A conservative divisor of 200 pixels per inch (ppi) is generally used to
determine the output size.

In the above discussion, only film and digital sensors were considered. In reality, an
image is captured and later displayed using an entire system in which several factors may
affect the resolution of the particular image. The quality of the optics (lens or lenses) used
to focus the image on the sensor plays an extremely important role and may greatly limit
the overall resolution of the system. Also, differences in display methods may limit or
enhance the perceived resolution.

CCD sensors often achieve color acquisition by using one sensor array with pixel cells of
alternating color sensitivity. Thus the overall resolution of the image will be less than the
specified number of pixels on the sensor. One way to ameliorate this situation is to use a
camera that contains three CCDs instead of one. This allows one to have a separate CCD
for each primary color, red, green, and blue. Therefore, for the same specified number of
pixels at the sensor, a three-CCD camera will provide higher resolution than a single-
CCD camera.

Two other factors that can effect resolution include the contrast in the scene and noise. In
this context, contrast refers to the apparent difference between the brightest and darkest
parts of the scene. As contrast increases, resolution increases. Noise refers to random
variations that limit the fidelity of detection and reproduction systems, such as the
granularity of photographic images. As noise increases, resolution decreases. Identifying
the specific effects of these factors on each of the sensors discussed above is beyond the
scope of this document.

Dynamic Range: The difference between the brightest highlight and darkest value that a
sensor (film or CCD) can detect and record in a single image. Negative film provides two
to four f-stops more than most digital cameras. This increased dynamic range allows
capture of both shadow and highlight details in a single frame of film. These same details
might require several different images (at different capture settings) when recorded with a
digital camera.

Color Range: The range of colors that can be detected by a sensor compared to normal
human vision. Negative film has a color range that is superior to CCDs.

Flexibility: The selection of speeds and types of film available. Silver-based photography
provides a wider selection of film speeds and types than digital cameras. Film can be
selected for specific applications in the field, and the film speed or type can be changed
on-site to meet specific needs.

493
Instant Print Cameras
Advantages of instant print cameras in field applications:
Immediacy of the final image (instant viewing/verification of image)
Operational security (all processing is in-house)
Disadvantages of instant print cameras in field applications:
Limited resolution of image
Production of copies requires multiple steps and can reduce image quality
High cost per image
Manual override, interchangeable lenses, or off-axis flash rarely offered
Digital Cameras
Advantages of digital cameras in field applications:
Immediacy of the final image (instant viewing/verification of image)
Ability to transmit and disseminate image with minimum of intermediate steps
On-site image management
Potential for on-site printing
Operational security (all processing is in-house)
Environmental impact more friendly than film

Disadvantages of digital cameras in field applications:

1. Battery or power supplies:
2. Environmental impact
3. Availability
4. Power conversion
5. Limited availability of storage media (available only from specialized stores)
6. Storage media subject to damage from electromagnetic fields
7. Image acquisition subject to electromagnetic interference
8. Hardware and software can be proprietary and incompatible among manufacturers
9. Legacy file problem (evolution of technology, including hardware and software, may
impact ability to access archived images over time)

Video Cameras
NOTE: Fixed camera video surveillance systems are not addressed in this document.
They will be addressed in future SWGIT documents.
Advantages of video cameras in field applications:
Real-time motion record capability
Immediacy of image (instant viewing/verification of image)
Ability to transmit and disseminate image with minimum of intermediate steps
More environmentally friendly than film
Ability to print in the field
Ability to synchronize and capture audio

Disadvantages of video cameras in field applications:

1. Battery or power supplies:
2. Environmental impact
3. Availability
4. Power conversion

494
5. Some high-quality storage media available only from specialized stores
6. Storage media subject to damage from electromagnetic fields
7. Image acquisition highly subject to electromagnetic interference
8. Resolution of still images is less than that of digital or silver-based capture media
9. Limited color fidelity (VHS and 8 mm formats, in particular)
10. Reduced media lifetime
11. Automatic compression in some formats
12. Weight and portability of equipment may be an issue

Notes on video formats:

VHS and 8 mm formats are the most commonly available formats but have the worst
signal-to-noise ratio of any video format (greatest amount of noise).
Super VHS and Hi-8 formats are the second most commonly available formats and have
somewhat better signal-to-noise ratio than VHS.
Beta SP and MII formats are professional-broadcast quality and are the best analog
format available.
Digital video quality varies, the high end is better than analog systems.

Hybrid Imaging Systems

A hybrid system is the combination of silver-based photography and digital imaging
technology that typically involves the conversion of silver-based film or print images to
digital images through the use of scanners. Hybrid imaging systems incorporate some of
the benefits of both film and digital image technologies and are recommended for those
agencies and organizations seeking to add digital imaging technologies to their
photographic resources.

Advantages of hybrid imaging systems in field applications:

1. Shortens darkroom time for producing prints
2. Maintains high-quality original film images
3. Offers flexibility of digital image processing
4. Enables easy electronic transmission of images
5. Enables image analysis
6. Simplifies case file management
7. Enables the use of a variety of output devices
8. Permits the production of copies from prints generated through instant photography
9. Disadvantages of hybrid imaging systems in field applications:
10. Separates processing/printing facilities
11. Has a relatively long processing time
12. Generates environmentally hazardous byproducts
13. Demonstrates a preprocessing fragility (i.e., temperature, humidity, x-ray effects,
expiration)
14. Has no means of immediate image evaluation (with the exception of instant film)

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Guidelines for Standard Operating Procedures (SOPs)

General Guidelines for a Crime Scene Photography SOP

TITLE: Crime Scene Photography SOP
PURPOSE: To permanently document, by qualified personnel, evidence and other details
at a crime scene for future reference
NOTE: Crime scene photography generally requires the ability to:
Record information that crime scene personnel may not know was important at the time
the images were captured
Deal with varying lighting and physical conditions
Accurately represent the details and colors in a scene
Get close-up and wide-angle images with accurate spatial relationships
Crime scene photography is usually a time-limited activity when there is only one
opportunity to correctly complete the task. Depending on the nature of the crime or
incident, conditions at a crime scene may dictate the selection and use of differing
equipment and techniques.

EQUIPMENT: (Image Capture Devices)

Silver-based film cameras are recommended for use as the primary image capture device.
The minimum recommendation is a 35 mm (SLR) camera capable of manual override,
interchangeable lenses, off-camera flash, and tripod mount
Digital still imaging can be used in a supplementary capacity (see Digital Cameras).
Digital still imaging can be used as the primary image capture device when the
performance of the equipment can be shown to meet anticipated needs
Video imaging can be used in a supplementary capacity. S-VHS, Hi-8, or better-quality
formats are recommended. It is suggested that cameras have the ability to incorporate
external/wireless audio, the ability to disable on-camera audio, and incorporate/disable
in-camera image stabilization (See Video Cameras)
Other standard photographic equipment as necessary

PROCEDURES: Agencies should follow agency-specific step-by-step instructions for

documenting crime scene evidence.
CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: See Advantages and Disadvantages of Major Image Capture
Technologies in Field Applications
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agencies should refer to agency-specific documentation and
manufacturers' manuals.

General Guidelines for a First Responder (A) SOP

The only images taken are those taken by the first responding officer(s).
TITLE: First Responder Photography SOP

496
PURPOSE: To document conditions found at an incident by the first law enforcement
official(s) on the scene where a crime scene photography unit or specialist will not be
requested
NOTE: Examples may include: domestic violence incidents, traffic accidents, minor
property crimes, and other incidents as defined by agency-specific policies. Photography
generally is not the first responder's primary responsibility, and the first responder may
have only a minimal amount of photography training.
EQUIPMENT: (Image Capture Devices)
Silver-based media film camera. Minimum recommendation is a 35 mm camera with
flash and close-up capability
Digital still imaging. The minimum recommendation is for a camera with more than 1600
x 1200 pixels (>2 megapixels), on-camera viewer, close-up capability, flash, and
removable storage media
Video imaging can be used in a supplementary capacity. S-VHS, Hi-8, or better-quality
formats are recommended. It is suggested that cameras have the ability to incorporate
external/wireless audio, disable on-camera audio, and incorporate/disable in-camera
image stabilization (See Video Cameras)
Other standard photographic equipment as necessary
PROCEDURES: Agencies should follow agency-specific step-by-step instructions for
documenting crime scenes.
NOTE: Images from separate incidents should be clearly delineated through a change of
storage media or through proper documentation.
CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: Successful capture of close-up images will require adhering to
manufacturers' specifications. Images captured digitally typically have a limited
enlargement capability that is less than those captured using 35 mm film (See Advantages
and Disadvantages of Major Image Capture Technologies in Field Applications).
Successful capture of images also requires utilization of fresh media (e.g., film that is not
past expiration and has been stored properly) and well-maintained equipment.
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agencies should refer to agency-specific documentation and
manufacturers' manuals.

General Guidelines for a First Responder (B) SOP

Images taken by the first responding officer(s) prior to arrival of a crime scene
photographer.
TITLE: First Responder Photography SOP
PURPOSE: To document conditions found at an incident by the first law enforcement
official(s) on the scene prior to the arrival of a crime scene photographer
NOTE: This guideline is directed toward documenting transient conditions that might be
lost prior to the arrival of crime scene photographers. Examples include situations in
which evidence must or might be moved, lost, or altered. Photography generally is not

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the first responder's primary responsibility, and the first responder may have only a
minimal amount of photography training.
EQUIPMENT: (Image Capture Devices)
Silver-based media film camera. The minimum recommendation is 35 mm camera with
flash, close-up capability
Digital still imaging. The minimum recommendation is for a camera with more than
1600x1200 pixels (>2 megapixels), on-camera viewer, close-up capability, flash, and
removable storage media
Video imaging can be used in a supplementary capacity. S-VHS, Hi-8, or better-quality
formats are recommended. It is suggested that cameras have the ability to incorporate
external/wireless audio, disable on-camera audio, and incorporate/disable in-camera
image stabilization (See Video Cameras)
Other standard photographic equipment as necessary
PROCEDURES: Agencies should follow agency-specific step-by-step instructions for
documenting crime scenes.
NOTE: Images from separate incidents should be clearly delineated through a change of
storage media or proper documentation.
CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: The successful capture of close-up images will require adhering to
manufacturers' specifications. Images captured digitally or with video typically have a
limited enlargement capability that is less than those captured using 35 mm film (See
Advantages and Disadvantages of Major Image Capture Technologies in Field
Applications). Successful capture of images also requires using fresh media (e.g., film
that is not past expiration and has been stored properly or new, unused videotapes) and
well-maintained equipment.
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agencies should refer to agency-specific documentation and
manufacturers' manuals.

General Guidelines for a Surveillance Photography SOP

TITLE: Surveillance Photography SOP
PURPOSE: To document acts and individuals engaged in those acts as they occur
NOTE: Surveillance activities may involve highly specialized techniques and equipment
that require technical training and knowledge and are best accomplished by trained
specialists.
EQUIPMENT: (Image Capture Devices)
Silver-based media film camera. The minimum recommendation is a 35 mm camera with
capability to disable both the flash and infrared auto-focus transmitter
Digital still imaging. The minimum recommendation is for a camera with a minimum
pixel resolution of 2000 x 1500 pixels (3 megapixels), capability to accommodate long
telephoto lenses, and disable the flash and infrared auto-focus transmitter. In covert
surveillance situations, illumination of the photographer by the LCD screen may
compromise safety

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Video imaging can be used in a supplementary capacity. S-VHS, Hi-8, or better-quality
formats are recommended. It is suggested that cameras have the ability to incorporate
external/wireless audio, disable on-camera audio, and incorporate/disable in-camera
image stabilization (See Video Cameras)
Other standard photographic equipment as necessary

NOTE: State laws may limit the legality of audio taping. Check local statutes for legality
of all surveillance activities.
SPECIALIZED EQUIPMENT: Night vision or thermal imaging equipment
PROCEDURES: Agencies should follow agency-specific step-by-step instructions for
documenting crime scenes. If audio is used, simultaneous recording of audio with video
on the same media and testing of the system is strongly recommended.
CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: The successful capture of images sufficient for identification of depicted
individuals and/or objects (e.g., license plates) will require close attention to the selection
and appropriate use of equipment. Images captured digitally or with video typically have
a limited enlargement capability that is less than those captured using 35 mm film (See
Advantages and Disadvantages of Major Image Capture Technologies in Field
Applications). The successful capture of images also requires utilization of fresh media
(e.g., film that is not past expiration and has been stored properly or new, unused
videotapes) and well-maintained equipment.
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agencies should refer to agency-specific documentation and
manufacturers' manuals.

General Guidelines for a Tactical Survey SOP

TITLE: Tactical Survey SOP
PURPOSE: To document conditions at a location so that plans can be made for future
law enforcement activities
NOTE: This type of photography is directed at obtaining general information regarding
the physical layout and major contents of a location in preparation for law enforcement
activities.
EQUIPMENT: (Image Capture Devices)
Silver-based media film camera. Minimum recommendation is 35 mm camera
Digital still imaging. Minimum recommendation is for a camera with more than 1600 x
1200 pixels (>2 megapixels)
Video imaging can be used in a supplementary capacity. S-VHS, Hi-8, or better-quality
formats are recommended. It is suggested that cameras have the ability to incorporate
external/wireless audio, disable on-camera audio, and incorporate/disable in-camera
image stabilization (See Video Cameras)
Other standard photographic equipment as necessary
PROCEDURES: Agencies should follow agency-specific step-by-step instructions for
documenting crime scene locations.

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CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: Location-specific limitations may apply.
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agencies should refer to agency-specific documentation and
manufacturers' manuals.

General Guidelines for a HAZMAT Scene Photography SOP

TITLE: HAZMAT Scene Photography SOP
PURPOSE: To permanently document, by qualified personnel, evidence and other details
at a crime scene that may contain biological, chemical, and/or radiological hazards
NOTE: A careful assessment of each HAZMAT scene is necessary prior to committing
any personnel or equipment. The means for inserting, removing, and sanitizing
equipment and personnel from a scene should be planned prior to initial entry. HAZMAT
scene photography generally requires:
Recording information that the crime scene personnel may not realize was important at
the time the images were captured
Contending with varying lighting conditions
Accurately representing all of the details and colors in a scene
Getting close-up and wide-angle images with accurate spatial relationships
HAZMAT crime scene photography is usually a time-limited activity when there is only
one opportunity to correctly complete the task. This type of photography usually involves
the use of protective clothing and gear that will make the operation of photographic
equipment more difficult.
EQUIPMENT: (Image Capture Devices)
Silver-based film cameras are recommended for use as the primary image capture device.
Minimum recommendation is 35 mm (SLR) camera capable of manual override,
interchangeable lenses, off-camera flash, and tripod mount. If protective housings are not
available but needed, disposable, waterproof 35 mm cameras may be necessary for some
HAZMAT scene photography
Digital still imaging can be used as the primary means when the performance of the
equipment can be shown to meet anticipated needs or when contamination issues may
preclude the use of silver-based media. Otherwise, digital still imaging can be used in a
supplementary capacity (See Digital Cameras). Minimum recommendation is for a 3-
megapixel camera
Video imaging can be used in a supplementary capacity. S-VHS, Hi-8, or better-quality
formats are recommended. It is suggested that cameras have the ability to incorporate
external/wireless audio, disable on-camera audio, and incorporate/disable in-camera
image stabilization (See Video Cameras)
Other standard photographic equipment as necessary
SPECIALIZED EQUIPMENT: Equipment for protecting personnel and camera systems
PROCEDURES: Agencies should follow agency-specific step-by-step instructions for
documenting crime scene evidence.

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CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: Protective equipment will hamper the use of some equipment, and
conditions may not permit the use of other equipment (e.g., flash, film). (See Advantages
and Disadvantages of Major Image Capture Technologies in Field Applications)
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agencies should refer to agency-specific documentation and
manufacturers' manuals.

General Guidelines for an Aerial Photography SOP

TITLE: Aerial Photography SOP
PURPOSE: To document locations, activities, and geographical relationships using
aircraft as a platform
NOTE: Aerial photography may involve highly specialized techniques and equipment
which require technical training and knowledge and is best accomplished by trained
specialists.
EQUIPMENT: (Image Capture Devices)
Silver-based media film camera. The minimum recommendation is 35 mm camera
capable of manual operation
Digital still imaging. The minimum recommendation is for a camera with a pixel
resolution of 3000 x 2000 pixels (6 megapixels) or higher
Video imaging can be used in a supplementary capacity. S-VHS, Hi-8, or better quality
formats are recommended. It is suggested that cameras have the ability to incorporate
and/or disable external/wireless audio and on-camera audio. It is strongly recommended
that image stabilization be used (See Video Cameras)
Other standard photographic equipment as necessary
SPECIALIZED EQUIPMENT: Night vision or thermal imaging equipment
PROCEDURES: Agencies should follow agency-specific step-by-step instructions for
aerial photography activities.
CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: Check the legality of all surveillance activities. Images captured
digitally or with video typically have a limited enlargement capability that is less than
those captured using 35 mm film (See Advantages and Disadvantages of Major Image
Capture Technologies in Field Applications). Successful capture of images also requires
using fresh media (e.g., film that is not past expiration and has been stored properly, and
new, unused videotapes) and well-maintained equipment.
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agencies should refer to agency-specific documentation, manufacturers'
manuals, and local statutes.

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General Guidelines for an Accident Scene Photography SOP
When agency policy does not require that crime scene photography personnel respond—
see General Guidelines for a First Responder (A) SOP.
When agency policy requires that crime scene photography personnel respond--see
General Guidelines for Crime Scene Photography SOP.

General Guidelines Covered Under General Guidelines for Crime Scene Photography
SOP
General Guidelines for an Arson Scene Photography SOP
General Guidelines for Autopsy Photography SOP
General Guidelines for a Bombing Scene Photography SOP
General Guidelines for a Mass Disaster Scene Photography SOP
General Guidelines for a Search Warrant Photography SOP
General Guidelines Covered Under General Guidelines for a First Responder SOP
General Guidelines for a Gang Related Graffiti Photography SOP
General Guidelines for a Field Mug Shots and Tattoos Photography SOP
General Guidelines for a Victim Photography SOP

502
 APPENDIC H - CONSIDERATIONS FOR MANAGERS

Scientific Working Group on Imaging Technologies (SWGIT)

Version 1.2, December 6, 2001
This document provides managers with considerations generated by SWGIT members.
The migration to new imaging technology may significantly affect current work
processes and should be done only after examining current operating procedures and
completing a needs assessment. This should involve the participation of the
organization's imaging and/or subject matter experts. Examining current operating
procedures is the crucial first step in implementing new imaging technology.
Consideration 1: Needs Assessment1
Prior to selecting digital imaging technology, current practices must be examined to
determine if there is a need to replace or enhance existing technology.
Consideration should be given to a hybrid imaging system where some or all of the
current equipment is used in conjunction with a new technology.
Consideration 2: Cost Analysis
Prior to selecting a digital imaging system, a cost-benefit analysis must be conducted to
determine the cost justification of a system purchase and to determine the possible
advantages and disadvantages to the agency with its implementation.
This analysis would allow a financial comparison between the current and proposed
imaging systems to make a procurement decision.
To determine a cost estimate, the following components should be considered: system
hardware, software, and maintenance; application software; communications hardware
and software; training; project management; facilities upgrades and site preparation; and
staffing and miscellaneous costs.
A typical cost justification includes the following major areas: a study of current
operations, proposed system architecture, equipment pricing, and financial indicators,
including a payback period.
Consideration 3: Image Resolution1
When determining resolution requirements, the intended usage, data storage
requirements, and the need for accurate reproduction of the image must be considered.
Consideration 4: Image Storage2
Original images must be preserved on separable media.
The selection of a storage media may depend on budget considerations for the agency.
Each has its own advantages and disadvantages.
Consideration 5: Image Compression
Compression affects image quality and should be considered carefully.
Lossy compression, such as JPEG, can result in the loss of critical details. The use of this
type of compression may render an image unsuitable for forensic analysis.
Consideration 6: Equipment Evaluation
Information used to evaluate suitability of new imaging technology should include
feedback from agencies currently using the equipment in similar applications, product
reviews, and vendor specification sheets.
Prior to making a final selection, require a demonstration of new imaging technologies
using representative samples of casework.
Do not rely solely upon prepackaged demonstrations.

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Consideration 7: Standard Operating Procedures (SOPs)
SOPs must be developed to ensure consistency, quality, integrity, and repeatability of the
process.
A staff member should be responsible for the overall project management, system
administration, and maintenance of the SOPs.
It is the responsibility of a staff member, rather than vendors and manufacturers, to
maintain written documentation of system procedures and SOPs, including access and
security policies and procedures.
Consideration 8: Training3
Initial and continuing training in imaging technology is required.
Consideration 9: Recurring Costs
Administrative managers should be aware of the cost of maintaining and upgrading
imaging systems. Unless these costs are factored into the budget, the system is in danger
of becoming obsolete. Some agencies annually budget approximately 15 percent of the
original system acquisition cost for upgrades, training, and maintenance.
Consideration 10: Legal Considerations
SOPs should be designed to protect the integrity of the images.
The user should be familiar with how the rules of evidence apply.

1
See SWGIT Guidelines for Field Applications of Imaging Technologies
2
See SWGIT Definitions and Guidelines for the Use of Imaging Technologies in the
Criminal Justice System
3
See SWGIT Guidelines and Recommendations for Training in Imaging Technologies in
the Criminal Justice System

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 APPENDIX 1 –SWGDE BEST PRACTICES

Version 1.1
Drafted July 26, 2001
Revised October 2002, January 31, 2003
Revised February 2004
Approved for Comment February 4, 2004
Reformatted February 24, 2004

Disclaimer:
As a condition to the use of this document and the information contained therein, the
SWGDE requests notification by e-mail before or contemporaneous to the introduction of
this document, or any portion thereof, as a marked exhibit offered for or moved into
evidence in any judicial, administrative, legislative or adjudicatory hearing or other
proceeding (including discovery proceedings) in the United States or any Foreign
country. Such notification shall include: 1) The formal name of the proceeding,
including docket number or similar identifier; 2) the name and location of the body
conducting the hearing or proceeding; 3) subsequent to the use of this document in a
formal proceeding please notify SWGDE as to its use and outcome; 4) the name, mailing
address (if available) and contact information of the party offering or moving the
document into evidence. Notifications should be sent to: execcmte@swgde.org.

Redistribution Policy:

SWGDE grants permission for redistribution and use of all publicly posted documents
created by SWGDE, provided that the following conditions are met:

1. Redistributions of documents, or parts of documents, must retain the SWGDE

cover page containing the disclaimer.

2. Neither the name of SWGDE, nor the names of its contributors, may be used
to endorse or promote products derived from its documents.

3. Any reference or quote from a SWGDE document must include the version
number (or create date) of the document and mention if the document is in a draft
status.

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BEST PRACTICES FOR DIGITAL EVIDENCE LABORATORY PROGRAMS

PART 1: Recommendations for Education and Training

SECTION 1: INTRODUCTION

1.1 Recommendations listed below are intended to apply to any examiner who:

Forensically examines and analyzes digital evidence or related materials, or

directs such examinations to be done.

As a consequence of such examinations, signs reports for legal and administrative

proceedings and provides testimony as required.

SECTION 2: MINIMUM RECOMMENDATIONS FOR EDUCATIONAL

REQUIREMENTS (for a further explanation of personnel/duties see section 7)

2.1 TECHNICIAN/ASSISTANT

Have education, skills, and abilities commensurate with their responsibilities.

2.1.2 Have on-the-job training specific to their position.

2.2 EXAMINER

An examiner should have at least a baccalaureate degree with science courses. An

examiner without a baccalaureate degree, should meet one of the following conditions:

Sixty semester hours of college level study to include course work with science courses;

OR

A minimum of two (2) years practical experience in the area of digital evidence
examination, and have demonstrated competency following the completion of a formal,
documented training program.

2.3 TECHNICAL MANAGER/LEADER

Meet all the requirements of an examiner.

Have a minimum of two (2) years of experience as an examiner in the forensic analysis of
digital evidence.

Exhibit knowledge necessary to evaluate results and conclusions.

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SECTION 3: CONTINUING PROFESSIONAL DEVELOPMENT

3.1 All personnel have an ongoing responsibility to remain current in their field. In
addition, agencies should provide support and opportunities for continuing professional
development. The recommended minimum continuing professional development
requirements for personnel are:

Forty annual hours of training relevant to the examiner’s responsibilities. All training,
once completed, must be documented. The training can be provided from a variety of
sources, including but not limited to:

Courses taught at the post-secondary educational level

Courses taught by vendors

In-service training conducted by the employer

In-service training taught by external provider

Attendance at workshops and participation in relevant scientific meetings or conferences.

To maintain membership in a field related professional organization.

SECTION 4: MINIMUM RECOMMENDATIONS FOR TRAINING PROGRAMS

Agencies should set their training programs to meet their needs as they relate to the types
of casework encountered, equipment available, and the level of competency of trainees.

A written training program, approved by the agency’s management, focusing on the

development of the theoretical and practical knowledge, skills and abilities necessary to
perform duties assigned, includes:

A training syllabus including descriptions of the knowledge and skills required by an

examiner (specific topic areas), milestones of achievement, and methods of testing or
evaluating competency.

Documented standards of performance and a plan for assessing theoretical and practical
competency against these standards (e.g. written and/or oral examinations, critical
reviews, mock casework, etc., per topic area).

A period of supervised casework that is representative of the type of casework required to

be performed.

Documentation verifying that the trainee has achieved the desired competence per
specific topic area.

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4.2 Topic areas in the training program should include, as a minimum, the following:

4.2.1 Relevant background information on digital evidence, such as:

4.2.1.1 Hardware

4.2.1.2 Software

4.2.1.3 Operating systems

4.2.1.4 Relevant applications

4.2.1.5 File identification

4.2.1.6 Relevant media (digital/analog)

4.2.1.7 File systems

4.2.2 Techniques, methodologies and equipment utilized in the examination of

digital evidence and related materials, such as:

4.2.2.1 Forensic analysis procedures

4.2.2.2 Best practices (technical procedures)

4.2.2.3 Standard operating procedures

4.2.3 Quality assurance, such as:

4.2.3.1 Quality assurance (for consistency within the forensic community)

4.2.3.2 Technical writing (for concise, clear reports)

4.2.3.3 Presentation skills (for the explanation of information)

4.2.3.4 General forensic principles and practices (for base of knowledge)

4.2.4 Expert/Court testimony and legal requirements, such as:

4.2.4.1 Public speaking (to build confidence in speaking situations)

4.2.4.2 Testimony skills (to establish a comfort level for testimony)

4.2.4.3 Admissibility (Daubert) Hearing Testimony (for issue awareness)

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 4.2.4.4 General criminal justice (to understand authority and result of
examinations)

4.2.4.5 Basic crime scene management (to understand scene and evidence
complexity)

4.2.5 Agency policies and procedures as they relate to the examination of digital
evidence and related materials, such as:

4.2.5.1 Safety (for the purpose of risk management and personal safety)

4.2.5.2 Security (to preserve chain of custody)

4.2.5.3 Ethics (to conform to a standard of integrity)

4.2.5.4 Evidence handling (to preserve integrity of evidence)

4.2.5.5 Training documentation (to demonstrate compliance)

An individual providing training must have the knowledge, skills, and abilities in the
subject area for which they are providing instruction.

SECTION 5: MINIMUM DOCUMENTATION/REFERENCE MATERIAL

AVAILABLE TO AN AGENCY PERFORMING DIGITAL EVIDENCE
EXAMINATIONS

Documentation/reference resources should be available and accessible to examiners in

hard copy or electronic form, such as:

College/university level textbooks as references to theory and practice in key subject

areas, e.g. hardware, software, and operating systems.

Reference literature pertaining to digital evidence.

Operation and maintenance manuals for all hardware and software available for use by
the examiner.

Relevant publications and periodicals.

Agency quality manual and standard operating procedures.

Relevant jurisdictional legislation (e.g., statutes and case law relating to digital evidence,
etc.).

Internet access.

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PART 2: Recommendations for Quality Assurance Guidelines

SECTION 6: INTRODUCTION

A digital evidence program should incorporate quality assurance. It is the goal of these
guidelines to provide a framework of quality management in the processing of digital
evidence, including evidence handling, management practices, analyses, and reporting.
6.1 QUALITY MANAGEMENT SYSTEM
A documented quality management system must be established and maintained.

The personnel responsible must be clearly designated and shall have access to
management responsible for organizational policy

6.1.2 The quality management system must cover all procedures and reports associated
with evidence

SECTION 7: PERSONNEL

7.1 JOB DESCRIPTION

The job descriptions for all personnel should include responsibilities and duties.

7.2 DESIGNATED PERSONNEL AND RESPONSIBILITIES

An individual (however titled) may be responsible for more than one of the following
duties:
Quality Assurance Manager: A designated person who is responsible for maintaining the
quality management system (including an annual review of the program) and who
monitors compliance with the program.

Health & Safety Manager: A designated person who is responsible for maintaining a
Health and Safety program (including an annual review of the program) and who
monitors compliance with the program.

Operational Manager: A designated person who has the overall responsibility and
authority for the operations of the unit.

Technical Manager/Leader: A designated person who has the overall responsibility and
authority for protocols and analytical methodologies.

Examiner: A designated person who:

Examines and analyzes digital evidence or related materials, or directs such examinations
to be done.

Signs reports for legal and administrative proceedings.

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Technician/Assistant: A person who works with evidence, but typically does not issue
reports for court purposes.

7.3 QUALIFICATIONS/EDUCATION
The agency should articulate its minimum qualifications, training and education
requirements consistent with those stipulated in Part 1 of this guide.

7.4 TRAINING
The agency must establish and document a training program and qualifying procedure for
all technical personnel. A written training program, approved by management, should
focus on the development of the theoretical and practical knowledge, skills and abilities
necessary to examine digital evidence and related materials as enumerated in Part 1 of
this guide.

7.5 MAINTAINING QUALIFICATIONS

The agency must establish and document the minimum continuing professional
development requirements for all technical personnel as enumerated in Part 1 of this
guide.

SECTION 8: PHYSICAL PLANT

FACILITY REQUIREMENTS
8.1.1 The facility shall provide adequate safety and security for personnel and
operations.
8.1.2 The facility must meet required health and safety standards.
8.1.3 The facility must contain adequate space to perform required analytical functions
and prevent alteration/damage to evidence.
A fume hood may be needed when the physical evidence poses a health and/or safety
hazard to the examiner (e.g., for digital evidence that was seized in a clandestine drug
lab, a crime scene containing biological materials, or other potentially hazardous
environments). It must be properly maintained and monitored according to an
established schedule.
8.1.5 A facility should maintain general cleanliness.
8.1.6 Facilities must be designed to ensure the proper safekeeping of evidence, data,
and records to protect from loss, cross-transfer, contamination and/or deleterious change.
Appropriate precautions should be taken with regard to electrostatic discharge, electrical
and magnetic fields to ensure the integrity of the digital evidence.
Appropriately secured storage areas must be provided.

SECTION 9: EVIDENCE CONTROL

The unit shall have and follow a documented evidence control system to ensure the
integrity of physical and digital evidence.

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9.1 RECEIVING AND IDENTIFYING EVIDENCE
The unit must maintain records of requests for service and of the respective items of
evidence. A unique identifier must be assigned to each case file or record. This file or
record must include at least the following:
9.1.1 The request for service document or a copy thereof.
9.1.2 The identity of the party requesting the service and the date of the request.
9.1.3 A description of items of evidence submitted with each having a unique item
identifier.
9.1.4 The identity of the person who delivers the evidence, along with the date of
submission. For evidence not delivered in person, descriptive information regarding the
mode of delivery and tracking information.
9.1.5 The chain of custody record.
9.1.6 Documentation of communication with the submitter.

9.2 INTEGRITY OF EVIDENCE

Evidence must be properly secured and labeled in accordance with the agency’s digital
evidence handling policy. Appropriate storage conditions shall ensure that the digital
evidence is not altered or lost. All actions taken with regard to the digital evidence will be
documented. A description of the evidence shall be compared to documentation prior to
examination. Any irregularities should be identified at this time, documented in the case
file and the submitter promptly informed.

9.3 STORAGE OF EVIDENCE

Access to the evidence storage area must be granted only to persons with authorization.
Access shall be controlled.

9.4 DISPOSITION OF EVIDENCE

Records must be kept regarding the disposition of all items of evidence.

9.5 DOCUMENTATION PROCEDURES

All records, such as results of examinations, measurements, notes, calibrations, spectra
and reports, shall be retained in a secure fashion.

SECTION 10: EXAMINATION PROCEDURES

10.1 PROCEDURES FOR DIGITAL EVIDENCE EXAMINATION

10.1.1 The unit shall have and follow written examination procedures.
10.1.2 Work practices shall be established to prevent contamination of evidence during
examination procedures.
10.1.3 The unit shall monitor the examination procedures using appropriate controls and
traceable standards.
Examination procedures must be validated in compliance with Section 14.

10.2 QUALIFICATION OF REFERENCE MATERIALS

10.2.1 The credibility of reference material should be confirmed prior to their first use.

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10.2.2 Unconfirmed reference materials must be qualified prior to use.
10.2.3 All qualifications must be documented to include the name of the individual who
performed the qualification and the date of qualification.

SECTION 11: EQUIPMENT PERFORMANCE

“Equipment” in this section refers to the non-evidentiary hardware and software the
examiner utilizes in the course of an examination.
11.1 Equipment must be monitored and documented to ensure proper performance is
maintained.
11.2 Only suitable and properly operating equipment shall be employed.
11.3 The manufacturer's operation manual and other relevant documentation for each
piece of equipment should be readily available.

SECTION 12: DOCUMENTATION, REPORTS, AND REVIEW

DOCUMENTATION
12.1.1 Examination documentation must contain sufficient detail to allow a peer to
reproduce the results obtained by the original examiner.
12.1.2 Evidence handling documentation should include: chain of custody, the initial
count of evidence to be examined, information regarding the packaging and condition of
the evidence upon receipt by the examiner, a description of the evidence, and
communications regarding the case.
12.1.3 Examination documentation should include items such as: observations,
examination processes and results, and supporting charts, graphs, and spectra generated
during an examination.
12.1.4 Documentation must be preserved according to written agency policy.

12.2 REPORTS
12.2.1 Reports issued by the unit must address the requests of the submitter.

Reports should include:

12.2.2.1 Identity of the reporting agency

12.2.2.2 Case identifier or submission number

12.2.2.3 Identity of the contributor

12.2.2.4 Date of receipt

12.2.2.5 Date of report

12.2.2.6 Descriptive list of submitted evidence

12.2.2.7 Identity of examiner

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12.2.2.8 Results/Conclusions

12.2.3 Written procedures for the release of case report information should be
established.

12.3 REVIEW

12.3.1 The agency must have a written policy establishing the protocols for technical and
administrative review.
The agency must have a written policy to determine the course of action should an
examiner and reviewer fails to agree.

SECTION 13: COMPETENCY AND PROFICIENCY TESTING

Each agency should participate in at least an annual proficiency-testing program and

should have written protocols for testing the competency and proficiency of its
examiners.

13.1 COMPETENCY TESTING

13.1.1 Units will monitor and document the competency of their examiner trainees and
technical support personnel prior to assumption of casework responsibilities.
13.1.2 Competency testing samples should be representative of the unit's normal
casework.
13.1.3 Competency testing must comply with the unit’s standard operating procedures
and other protocols.

PROFICIENCY TESTING - INTERNAL

13.2.1 Each examiner shall be proficiency tested annually in each sub-discipline in
which casework is performed.
13.2.2 The proficiency testing samples should be representative of the examiner's normal
casework.
13.2.3 The test examination must comply with the unit’s standard operating procedures.

PROFICIENCY TESTING - EXTERNAL

13.3.1 Each unit shall be proficiency tested annually in order to verify the unit's
performance.
13.3.2 The proficiency testing samples should be representative of the unit's normal
casework.
13.3.3 The test examination should follow the unit’s standard operating procedures.
The proficiency tests shall be obtained from approved test providers where available.

SECTION 14: VALIDATION

14.1 Validation is required to demonstrate the examination procedures and tools are
suitable for their intended purpose.

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14.1.1 Minimum acceptability criteria should be described along with means for
demonstrating compliance.
14.1.2 Validation documentation is required.

SECTION 15: INTERNAL AUDITS

15.1 Audits should be conducted at least once a year.

15.2 Records of each audit must be maintained and should include the scope, date of
the audit, name of the person(s) conducting the audit, findings, and corrective actions
taken, if necessary.

SECTION 16: DEVIATIONS AND DEFICIENCIES

In the course of examining digital evidence and related materials, the unit may experience
results that are anomalous in some manner. Each unit must have a written policy to deal
with deviations and deficiencies.
16.1 As used in this guide, a deficiency is any erroneous examination result or
interpretation, or any unapproved deviation from an established policy or procedure in an
examination.

16.2 As used in this guide, a deviation is a departure from the established policies and
procedures.

Comment: In developing policy the following may be considered: a requirement for

immediate cessation of the activity or work of the individual or tool involved, if
warranted by the seriousness of the deficiency, as defined in the written policy; a
requirement for administrative review of the activity or work of the individual involved; a
requirement for evaluation of the impact this deficiency may have had on other activities
of the individual or other examiners; a requirement for documentation of the follow-up
action taken as a result of the review; a requirement for communication to appropriate
employees of any confirmed deficiency which may have implications for their work.

SECTION 17: HEALTH AND SAFETY

The agency must have a documented health and safety program in place to meet the
needs of the unit.

17.1 HEALTH AND SAFETY REQUIREMENTS

17.1.1 All personnel should receive appropriate health and safety training.
17.1.2 The digital evidence unit shall operate in accordance with agency policy and
comply with any relevant statutory regulations.
17.1.3 Health and safety manual(s) shall be readily available to all personnel.

SECTION 18: DOCUMENTATION

In addition to casework documentation the unit should maintain documentation on the
following topics:

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18.1.1 Quality manual

18.1.2 Standard operating procedures

18.1.3 Training

18.1.4 Validation of tools

18.1.5 Physical workspace

18.1.6 Equipment maintenance/calibration

18.1.7 Health and safety

18.1.8 Evidence handling tracking system

18.1.9 Annual assessment of the quality management system

18.1.10 Proficiency testing

18.1.11 Report of findings

18.1.12 Court testimony monitoring

18.1.13 Competency testing

18.1.14 Evidence seized

18.1.15 Audits

18.1.16 Corrective action policy/procedures

18.1.17 Complaints and conflict resolution

18.1.18 Reference materials (including source and qualification).

18.1.19 Equipment inventory (e.g. manufacturer, model, serial number, acquisition

date).

SECTION 19: QUALITY MANUAL

19.1 The agency’s quality system policies and objectives shall be defined in a Quality
Manual. A comprehensive Quality Manual must contain or reference the documents or
policies/procedures pertaining to the following:

19.1.1 A quality policy statement including objectives and commitments by management

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19.1.2 The organization and management structure of the unit, its place in any parent
organization, and relevant organizational charts

19.1.3 The relationships and responsibilities of management, technical operations, and

support services in implementing the quality system

19.1.4 Job descriptions, education, and up-to-date training records of unit staff

19.1.5 Control and maintenance of documentation of case records and procedure

manuals

19.1.6 The unit’s procedures for ensuring that measurements are traceable to appropriate
standards, where available

19.1.7 The type and extent of examinations conducted by the unit

19.1.8 Validation of test procedures used

19.1.9 Handling evidence

19.1.10 The use of standards and controls in unit procedures

19.1.11 Calibration and maintenance of equipment

19.1.12 Practices for ensuring continued competence of examiners including

proficiency testing programs, and internal quality control schemes (e.g., technical review)

19.1.13 Gaining feedback and taking corrective action whenever discrepancies are
detected

19.1.14 Monitoring court testimony to ensure the reporting of scientific findings in

an unbiased and effective manner

19.1.15 Unit protocol permitting departures from documented policies and

procedures

19.1.16 Dealing with complaints

19.1.17 Disclosure of information

19.1.18 Audits and quality system review

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PART 3: Recommended Procedures for Digital Forensic Examinations

The following information is provided as guidance for the development of agency

Standard Operating Procedures (SOP). The SOP should address each of the following
elements:

SECTION 19: REVIEW THE REQUEST FOR SERVICE/EXAMINATION

Ascertain legal authority to perform the requested examination. The examiner will be
provided with the legal authority that allows him/her to examine digital evidence.
Examples of such authority include: consent to search by owner, subpoena, search
warrant, or other legal authority.

Review documentation provided by the requestor to determine the processes necessary to

complete the examination.

SECTION 20: RECEIPT OF EVIDENCE PROTOCOL

Maintain chain of custody per established agency standard operating procedures for
handling digital evidence.

Coordinate with the investigator and/or other forensic examiners when other forensic
examinations may be required. Specifically, the order in which these forensic
examinations will be conducted should be determined prior to any examination. (e.g.
latent print analysis, DNA analysis, hair fiber analysis)

SECTION 21: CONDUCT PHYSICAL INSPECTION OF ITEMS

PRESENTED FOR DIGITAL EXAMINATION

Inspect and document the evidence received. Note condition of items received and any
exceptions between the inventory of items received and the evidence reviewed by the
examiner.

Assess the power needs for devices with volatile memory. Follow agency policy for the
handling of these devices.

SECTION 22: PREPARATION FOR EXAMINATION

The examiner should maintain evidence integrity and document any exceptions.
Establish conditions to prevent the possibility of data contamination.

SECTION 23: CONDUCT EXAMINATION

Document evidentiary settings and configurations, if possible.

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Extract digital information necessary to meet requirements of the examination.

Analyze and/or interpret the extracted digital information.

SECTION 24: DOCUMENT THE EXAMINATION

The documentation must contain a sufficient level of detail such that another competent
examiner could reproduce the same extracted results.

Report(s) issued must meet the requirements of the agency.

SECTION 25: QUALITY CONTROL

Adhere to the agency’s quality control procedures which should include:

Technical/Peer review.

Administrative review.

SECTION 26: ISSUE REPORT

The report must be signed and dated by the examiner. The signature may be electronic or
physical as per agency standards.

SECTION 27: DISPOSITION OF EVIDENCE

Adhere to organization’s evidence disposition policy.

GLOSSARY

Administrative Review
A procedure used to check for consistency with laboratory policy and for editorial
practice. (ASCLD/LAB)

Audit
A review conducted to compare the various aspects of a laboratory’s performance with a
standard for that performance. (ASCLD/LAB)

Digital Evidence
Information of probative value stored or transmitted in binary form. (SWGDE)

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Digital Evidence Examiner (Examiner)
An individual responsible for the duplication, extraction and/or analysis of information
from digital evidence, generation of work product, writing reports, and testifying in legal
and administrative proceedings. (SWGDE)

Qualification Testing
Process to provide sufficient confidence that reference materials utilized are valid.

Quality Assurance
Those planned and systematic actions necessary to provide sufficient confidence that a
laboratory’s product or service will satisfy given requirements for quality.
(ASCLD/LAB)

Reference Materials
As used in this document, this refers to items such as published literature, hardware and
software documentation, hash sets, header sets, etc. (SWGDE)

Technical/Peer Review
An evaluation of reports, notes, data, and other documents to ensure an appropriate and
sufficient basis for the scientific conclusions. This review is conducted by a second
qualified individual. (In accordance with ASCLD/LAB)

Validation
The process of performing a set of experiments that establish the efficacy and reliability
of a technique or procedure or modification thereof. (ASCLD/LAB)

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 APPENDIX J - GENERAL GUIDELINES FOR CAPTURING LATENT
IMPRESSIONS USING A DIGITAL CAMERA

Scientific Working Group on Imaging Technologies (SWGIT)

Version 1.2, December 6, 2001

Introduction
The purpose of this document is to describe the proper documentation of latent print
evidence in the field by qualified personnel when using a digital camera.
The recommendations offered in this document are made in accordance with current
National Institute of Standards and Technology (NIST) guidelines specifying 1000 pixels
per inch (ppi) at 1:1 as the minimum resolution.

Equipment
It is recommended that a professional digital camera kit consist of, at a minimum, the
following items:
Professional digital camera capable of interchangeable lenses, manual override for
exposure and focus, off-camera flash, remote shutter release, and tripod mount
Macro lenses capable of 1:1
Dedicated electronic flash designed for digital camera, capable of off-camera operation
Dedicated electronic flash cable to permit off-camera operation
Remote shutter release
Tripod capable of various angles and positions
Artificial light sources (e.g., flood lights, flashlights)
Digital storage media including additional media, as needed
Portable computer with appropriate software for downloading and viewing images at the
scene
Appropriate cable connections (e.g., USB, Firewire, parallel) and/or PCMCIA capability
Scaling devices graduated in millimeters
Photographic log
The camera/capture devices listed in Chart 1 will meet the required 1000 ppi standard.
However, this is not an endorsement or a recommendation for the brand names or models
of equipment listed. This is not an all-inclusive list; there are other cameras that will
achieve this resolution.

General requirements for portable computer dedicated for field use:

Processor speed 400 MHZ or faster
Color display
System memory of 128 MB or higher
Minimum hard drive of 10GB
Connectivity capability with camera
Appropriate camera software for image file acquisition
Appropriate software for file management
Network capability
AC power adapter/12V DC power adapter
CD-R/W (for CD-R media)

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Procedures: Agency-specific step-by-step instructions for the capture of latent
images should be followed.
Images from separate incidents should be clearly delineated by a change of storage media
or by proper documentation.

Procedure 1: Lens calibration to achieve a minimum of 1000 ppi

The following procedures should be completed prior to field use.
The pixel dimensions on the sensor determine the camera-to-subject distance, and
therefore, the area of maximum coverage for 1000 ppi.
Find the pixel resolution on the chart to determine what the image size will be. If the
camera is not listed on the chart, see the manufacturer's specification sheet for the pixel
resolution size.

To determine the area in millimeters,

Divide the pixel resolution by 1000, then multiply by 25. (Twenty-five millimeters equals
approximately one inch.) For example, 1524 X 1012 equals 37 mm X 25 mm (rounded to
the lowest millimeter).
Make a template to the exact dimension of the area of coverage, (37 mm X 25 mm).
Place template on a flat surface and fill image area in viewfinder with template and scale.

After achieving the camera-to-subject distance,

Mark lens with pencil, photograph template with scale, and acquire image into computer.
Calibrate image with calibration software to actual size (1:1).
Print image and measure the scale to verify size. If this is correct, the lens is calibrated.

If this is larger than actual size,

Move the camera away from the template, refocus, and mark the lens.
Repeat steps 5, 6, 7, and 8. Once verified, this becomes the camera-to-subject maximum
distance to provide 1000 ppi.

When the above procedure has been completed,

Scribe a line on the side of the lens over the pencil mark (recommended). This is the
known setting to achieve the correct resolution (1000 ppi).
Physically move the camera in and out to focus the image. This will ensure that the
resolution will not change (which would happen if you adjust the lens focus).

Procedure 2: Camera setup for latent impression photography

A typical standard operating procedure includes the following techniques used for field
and laboratory settings.
Locate visible impressions to be captured.
Capture overall view of impression area without a scale with appropriate lighting.
Capture overall view of impression area with scale and appropriate lighting.
Mount camera on tripod with camera at a 90-degree angle to the impression. Do not use a
magnetic level. (Avoid contact or proximity of magnetic fields with storage media and

522
camera because these fields may erase stored images and data and interfere with image
capture).
Light visible impression appropriately.
Place scale/identification tag adjacent to impression without obscuring detail. A tag
should contain the following minimum information:
Fill image area in viewfinder with impression and scale using lens calibrated with camera
in use.
Take light meter readings and adjust camera settings to capture image.
Capture impression using correct exposure as indicated by the light meter. If necessary,
capture additional images of the impression by bracketing exposures up one f-stop and
down one f-stop.
Visually verify images.
If images are unacceptable, re-photograph.
Repeat steps 7 through 11 for each lighting position used for that impression.
After the evidence is processed for impressions, follow steps 5 through 11 as appropriate
for all latent prints developed.
Prepare photographic log or worksheet per agency policy.
When using more than one storage media, uniquely identify each device.

Procedure 3: Use of a portable computer in field operations to acquire file/images

Connect camera or removable media to computer according to manufacturer's
specifications.
Create and name a file folder on the computer's hard drive to receive original image files.
The camera or software may require unique file folder names for each download. Care
should be taken not to overwrite existing image files from previously downloaded media.
Some cameras reset their file counters whenever media is changed.
Prepare subdirectories for receiving downloaded images from camera or media. Create
and name a subdirectory, using unique naming convention, in sequential order.
Copy all original files to appropriate subdirectory.
Verify that all images have been copied into the correct subdirectory.
Set file permissions to preclude accidental deletion of files.
If appropriate, erase removable media for reuse. Agency-specific standard operating
procedures should dictate whether reuse of storage media is acceptable.

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Guidelines and Recommendations for Training in Imaging Technologies in the
Criminal Justice System

Scientific Working Group on Imaging Technologies (SWGIT)

Version 1.2, December 6, 2001
The consistent and reliable use of silver-based, video, and digital imaging technologies in
the criminal justice system requires the competent and appropriate training of personnel.
The purpose of this document is to provide guidelines and recommendations for such
training.
It should be recognized that some agencies may choose to provide training other than
what is recommended in this section. In such circumstances, those agencies should
demonstrate and document that the training selected is adequate to meet their anticipated
needs.

Introduction
Personnel in the criminal justice system who work with images must be aware of the
capabilities and limitations of specific imaging technologies. Those engaged in the
production or the use of images should be aware of the procedures commonly followed
within the law enforcement community and should strive to meet or exceed these
recommendations. They should also endeavor to maintain awareness of new
developments. In support of these goals, the following recommendations are offered to
personnel engaged in the production of images:
Define and employ quality assurance programs to ensure the implementation of valid and
reliable procedures for the task.
Maintain proficiency by pursuing continuing education courses in imaging technology.
Maintain awareness of legal developments relating to the use of imaging technologies in
the criminal justice system.

Definitions of Categories
Several categories of imaging technology training relevant to the criminal justice system
as well as the categories of the system users who would benefit from the training are
identified and defined as follows:

Categories of Training
Awareness: Training designed to provide the student with a general knowledge of the
major elements of a given imaging technology including specific product capabilities
Skills and techniques: Training designed to provide the student with the ability to
competently use specific imaging equipment
Knowledge of processes and relationships: Training designed to provide the student with
an understanding of imaging technology and the ability to apply that technology to
various applications
Court procedures: witness testimony: Training designed to provide the student with the
ability to present reliable imaging technology-based testimony in court
Court procedures: case preparation: Training designed to provide the student with the
ability to prepare and review accurate and reliable imaging technology-based evidence

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Continuing education: Training designed to provide the student with additional and
updated training in imaging technologies
Specialized applications: Training in specific disciplines or in specialized areas
Proficiency: Proficiency training incorporates a number of components:
Required levels of skill and knowledge for a job category should be identified by the
agency. These levels should be driven by the requirements of the specific tasks to be
accomplished.
A course should be designed by the agency or its agent, to provide the skills and
information necessary for the agency's personnel to attain competency in those skills
If determined to be necessary by the agency, a proficiency test should be developed and
administered to test these skills.
Different levels of proficiency tests may be developed depending on the level of skill and
experience of the personnel.

Categories of Users
Management: Includes personnel who are responsible for setting agency policies and/or
making budget decisions
Command/Supervision: Includes personnel who supervise and/or direct personnel
engaged in the use of imaging technologies
Law Enforcement Officer: Includes personnel who use imaging technologies as a minor
component of their routine duties. If the person is routinely involved in the basic
photographic documentation of crime scenes, then this person would fall into the crime
scene technician category
Crime Scene Technician: Includes personnel for whom imaging is a major component of
their routine duties. Crime scene technicians are divided into two categories. Level 1
technicians routinely perform only basic photographic or videographic documentation of
crime scenes. Level 2 technicians routinely perform forensic photographic techniques,
including specialized photography of impression evidence
Criminalist/Examiner: Includes personnel for whom imaging is a major component of
their routine duties. The personnel are not only responsible for the acquisition of images
as a part of their duties but may also be responsible for the analysis of these images
Photographer/Videographer/Specialist: Includes personnel for whom imaging is the
major component of their routine duties
Lawyer: Includes prosecutors and defense attorneys
Judge: Includes personnel who are responsible for the acceptance or rejection of imaging
technology-based evidence in court proceedings
Legal Assistant: Includes personnel who are responsible for preparing materials that will
be offered in court proceedings
Trainer: Includes personnel who are responsible for providing instruction to others in
imaging technology-related areas

Recommended Training Levels

Table 1 provides an assessment of the level of training necessary for each category.

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Topical Areas for Focused Training
The following section delineates specific topical areas in which user groups should
receive focused training to effectively fulfill their imaging technology-related duties.

Managers, Commanders/Supervisors, Lawyers, and Judges (awareness and issues

training)
Status of imaging technology
Legal issues
Extent of use and who are the users
Industry and market trends
Description of current technologies
Strengths and weaknesses of silver imaging
Strengths and weaknesses of digital imaging
Strengths and weaknesses of video imaging (analog and digital)
Current life cycle-cost comparisons and limitations
Strategic alternatives for the agency
Determination of imaging needs
Sequence of equipment/software acquisitions
Actions to avoid or lessons learned
References/information sources

Legal Assistants (basic levels of skill for recording images)

Working knowledge of the basic fundamentals of photography and/or videography
Working knowledge of the capabilities and limitations of equipment
Selection and operation of the appropriate cameras (digital, video, or film) and
accessories
Preparation of court presentations including images

Law Enforcement Officers (first responder)

Operation of cameras with an understanding of the capabilities and limitations of the
equipment assigned as a part of their routine duties
Selection, framing, and composition of appropriate images
Procedures for recording quality images in various situations
Proper collection and preservation of the recording media
Creation and maintenance of the chain of custody
Demonstration of competency
Demonstration of proficiency through testing

Crime Scene Technicians Level 1 (with video or adjustable still cameras)

Basic levels of skill and knowledge for recording a crime scene
Various images to take
Set-ups for each type of image
Working knowledge of the fundamentals of photography and/or videography
Proper collection and preservation of the recording media
Creation and maintenance of the chain of custody

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Working knowledge of the capabilities and limitations of equipment
Selection and operation of the appropriate cameras (digital, video, or film) and
accessories
Demonstration of competency
Demonstration of proficiency through testing

Crime Scene Technicians Level 2 (capable of training Level 1 crime scene technicians
and law enforcement officers)
Comprehensive knowledge of and experience in forensic photography techniques, such
as
Retrieving impression evidence such as fingerprints and/or blood spatter
Selecting the appropriate film and equipment based on knowledge of the capabilities and
limitations of the various aspects of imaging
Solving difficult non-routine imaging problems
Awareness of film processing and image processing options; (i.e., the effects of the push
process or contrast adjustments)
Videography techniques (refer to LEVA Guidelines at www.leva.org)
Knowledge of how to use the most common image processing tools and techniques
Competency demonstration
Proficiency demonstration through testing

Imaging Specialists
Personnel include photographic specialists, forensic scientists, and forensic video
analysts. These personnel are capable of training law enforcement officers and Level 1
and Level 2 crime scene technicians.
Working knowledge of how to use the various applicable aspects of the imaging chain
Expertise in using techniques applicable to a particular discipline
Photogrammetry
Surveillance imaging
Frequency domain conversion; (i.e., Fast Fourier Transform filtering)
Alternate light sources and contrast filtering
Demonstration of competency
Demonstration of proficiency through testing

Trainers
Classroom techniques
Development of lesson plans
Preparation of audio-visual materials
Development of student exercises
Selection of text books and reference materials
Development of course exams
Development of proficiency exams
·Development of course evaluation processes
Demonstration of competency in subject matter
Demonstration of proficiency in subject matter by testing

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Issues to Consider when Addressing Training Needs
A number of issues should be considered when addressing an agency's training needs.
The following section provides guidance for selecting training providers and addressing
continuing education and testimony training needs.

Selecting a Training Provider

Continuing Education
Continuing education can be obtained from training conferences, trade shows, and
specialized courses. This training should address updates and the use of new imaging
technologies such as:
Equipment
Software
Imaging techniques applicable to law enforcement
Scientific techniques beneficial to forensic imaging

Testimony Training
This training should address the use of image-based evidence in court such as:
Lecture-type presentation relevant to court testimony
Moot court
Court monitoring

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APPENDIX K - RECOMMENDATIONS AND GUIDELINES FOR THE USE OF
DIGITAL IMAGE PROCESSING IN THE CRIMINAL JUSTICE SYSTEM

Scientific Working Group on Imaging Technologies (SWGIT)

Version 1.2, June 2002

Purpose
The purpose of this document is to provide recommendations and guidelines for the use
of digital image processing in the criminal justice system. The objective is to ensure the
successful introduction of forensic imagery as evidence in a court of law. This document
includes brief descriptions of advantages, disadvantages, and potential limitations of each
major process.

Background
Digital image processing is an accepted practice in forensic science. It is the position of
the Scientific Working Group on Imaging Technologies (SWGIT) that any changes to an
image made through digital image processing are acceptable in forensic applications
provided the following criteria are met:
The original image is preserved
The processing steps are logged when they include techniques other than those used in a
traditional photographic darkroom
The end result is presented as an enhanced image, which may be reproduced by applying
the logged steps to the original image
The recommendations of this document are followed

Introduction
This document addresses digital image processing and related legal considerations in the
following four categories:
Image enhancement
Image restoration
Image compression
Image analysis
When using digital image processing techniques, use caution to avoid the introduction of
unexplainable artifacts that add misleading information to the image and the loss of
image detail that could lead to an erroneous interpretation. Any processing techniques
should be applied only to the working image.
The successful introduction of forensic imagery as evidence in a court of law is
dependant upon the following four legal tests:
Reliability
Reproducibility
Security
Discovery

Definitions
Apple QuickTime™ Movie Format (MOV file format): Apple file format for storing and
displaying compressed video sequences.

529
Artifact: Any visible feature or distortion in a recorded image or output image that is not
present in the corresponding imaged object or input image. Image artifacts can be
introduced inadvertently by hardware or software or intentionally by an operator. The
latter type includes annotation or other direct alteration of an image in order to clarify or
call attention to some particular image content. Artifacts introduced by hardware and
software generally degrade an image and, if severe enough, can impair interpretation.
AVI (Audio/Video Interlaced): Microsoft file format for storing and displaying
compressed video sequences.
Compression ratio: The size of an image data file before compression divided by the file
size after compression.
Copy image: A reproduction of information contained in a primary or original image.
Deinterlacing: Separating an interlaced frame into two separate fields.
Discovery: The criminal defendant's right to confront and challenge the evidence.
Forensic: The use or application of scientific knowledge to a point of law, especially as it
applies to the investigation of crime.
GIF (Graphical Interchange Format): A lossless compression file format commonly used
for graphic images.
Image analysis: The extraction of quantitative information from an image beyond which
is readily apparent through visual examination.
Image averaging: The process of averaging together similar images, such as sequential
video frames, to reduce noise in stationary scenes.
Image compression: The process of reducing the size of a data file.
Image enhancement: Any process intended to improve the visual appearance of an image.
Image processing: Any activity that transforms an input image into an output image.
Note: Image processing does not mean that the input image is overwritten during the
process. Forensic image processing should be performed only on working images.
Image restoration: Any process applied to an image that has been degraded by a known
cause, such as defocus or motion blur, so the effects of that degradation are partially or
totally removed.
Image synthesis: Any process that renders an image through the use of computer graphics
techniques for illustrative purposes (e.g., age progression, facial reconstruction,
accident/crime scene reconstruction). This subject is beyond the scope of this document.
Interlaced scan: Video image format. The video frame consists of two fields. The first
field contains all the odd-numbered horizontal lines and the second field all the even-
numbered lines. All standard TV video signals used in North America and elsewhere
under the NTSC (RS-170, CCIR) standard are in the interlaced format.
Interpolation: A process by which the apparent resolution of an image is increased. In
most cases the software mathematically averages adjacent pixel densities and places a
pixel of that density between the two.
JPEG (Joint Photographic Experts Group): A lossy image compression process. Users
can set their own quality settings on a sliding scale within the application software.
JPEG 2000: An image compression process currently under development.
LZW (Lempel-Ziv-Welch): A lossless compression process used by the TIFF and GIF file
formats.
MPEG (Motion Pictures Experts Group): Similar to JPEG, a standard compression
algorithm used to compress video and audio sequences.

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Original image: An accurate and complete replica of the primary image, regardless of
media. For film and analog video, the primary image is the original image.
Primary image: Refers to the first instance in which an image is recorded onto any media
that is a separate, identifiable object or objects. Examples include a digital image
recorded on a flash card or a digital image downloaded from the Internet.
Progressive scan: (Noninterlace) Video in which each image frame contains information
from every horizontal scan line of the imaging sensor.
Reliability: The extent to which information can be depended upon.
Reproducibility: The extent to which a process yields the same results on repeated trials.
Security: The extent to which the evidence has been preserved and safeguarded.
TIFF (Tagged Image File Format): A standardized image file exchange format. It is
widely supported by both hardware and software manufacturers and is platform
independent. Can be lossless or lossy.
Working image: Any image subjected to processing.

Image Enhancement
Image enhancement is any process intended to improve the visual appearance of an
image. This includes processes that have a direct counterpart in the conventional silver-
based photographic laboratory and those that can be accomplished only by using a
computer.

Traditional Enhancement Techniques

Traditional enhancement techniques are techniques that have direct counterparts in
traditional darkrooms. They include brightness and contrast adjustment, color balancing,
cropping, and dodging and burning. These traditional and acceptable forensic techniques
are used to achieve an accurate recording of an event or object.
Brightness adjustment is used when the image is too bright or too dark. If the image is
made too bright, there is a risk of loss of detail in light areas. If the image is made too
dark, there is a risk of loss of detail in the dark areas.
Color balancing is the adjustment of the color components of an image. The purpose of
color balancing is to render the colors in the scene faithfully. Improper color balance
adjustment can render colors inaccurately, and objects will appear to have the wrong
color when compared to the actual subject.
Contrast adjustment is used when the image lacks sufficient contrast. If the image
contrast is increased too much, there is a risk of loss of detail in both light and dark areas.
Cropping is used to remove that portion of the image that is outside the area of interest.
Dodging and burning have the same effect as brightness adjustment but are used in
localized areas.
Spotting traditionally has been used to remove artifacts due to dust and scratches on the
negatives, but it is not considered to be an acceptable practice on any forensic image.
Note: The use of spotting and cropping techniques may come under scrutiny in a court of
law. Specific agency policies should address the use of these techniques.

Nontraditional Enhancement Techniques

Some nontraditional image enhancement processes are used and accepted by a variety of
scientific fields such as medicine, aerospace, and cartography. These processes have no

531
direct counterpart within traditional silver-based photography. In fact, only recently have
they been applied within the forensic environment; therefore, their general acceptance
may be subject to challenge. Examples of nontraditional processes discussed here are
color processing, linear filtering, nonlinear contrast adjustments, pattern noise reduction,
and random noise reduction.
Color processing includes color space transformations, pseudocoloring, and hue and
saturation adjustments. These techniques can be used to modify the color characteristics
of objects within an image. Caution: Application of these techniques can compromise the
color fidelity of the image.
Linear filtering techniques include sharpening, deblurring, edge enhancement, and
deconvolution. They are used to increase the contrast of small detail in an image. If a low
degree of enhancement is used, the image will remain an accurate representation of the
scene. If a high degree of enhancement is used, the image may no longer be an accurate
representation of the overall scene, though still may be useful as an adjunct for
interpretation of small details. Caution: A high degree of enhancement can also increase
the visibility of existing noise and artifacts. Examples of noise include film grain, snow
appearing on a TV screen, or random color dots.

Nonlinear contrast adjustments include gamma correction, grayscale transformation,

curves, and look-up tables. They are an extension of traditional photographic
sensitometric techniques and are used to adjust the contrast in selected brightness ranges
within the image. For example, details may be brought out in the shadow areas without
affecting the highlight areas. Caution: A severe adjustment can cause loss of detail, color
reversal, and the introduction of artifacts.

Pattern noise reduction filters identify repeating patterns in the image and allow the user
to selectively remove them. This type of filter can be used to remove patterns such as
fabric weaves, window screens, security patterns, and halftone dots. Caution: Overuse of
this technique can cause selective removal of relevant image detail.
Random noise reduction techniques include such filters as low pass, blurring, median,
and despeckling. They are used to reduce the contrast of small detail in the image in order
to suppress random noise. Caution: Overuse of this technique can cause loss of relevant
detail.

Considerations for the Application of Image Enhancement Techniques

Question: What type of image must not be enhanced?

Answer: A primary or original image.
Discussion: Because a primary or original image represents the first instance where the
image is recorded onto any media, or it is an accurate and complete replica of the primary
image, it must not be altered or modified. Enhancements are performed only on working
images.
Question: Is it necessary to document the enhancement process used to produce an
enhanced image?
Answer: The need to document the enhancement process is determined by the process
used.

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Discussion: Documentation of enhancement steps is not necessary when using traditional
darkroom techniques. When using nontraditional image enhancement techniques such as
unsharp masking or random noise reduction, enhancement steps should be documented in
the case notes in sufficient detail to enable another comparatively trained individual to
repeat the steps and produce the same output when the image is subjected to image
analysis.
Question: In a legal setting, are enhanced images discoverable?
Answer: Yes.
Discussion: All images may be discoverable. In cases where images are enhanced, both
the original and the enhanced image, along with associated documentation, may be
discoverable.
Question: Who is responsible for testifying about an enhanced image?
Answer: The person doing the enhancement or a person skilled in and knowledgeable
about the enhancement process that was used.
Discussion: The person who performed the enhancement is best qualified to testify about
the enhancement techniques used. However, there may be occasions where the court will
require the assistance of additional subject-matter experts.
Question: Are there legal ramifications associated with the software used specifically for
image enhancement?
Answer: Yes.
Discussion: Some considerations may include:
Have the particular functions within the software been accepted by the scientific
community?
Does the software perform as the manufacturer purports?
Has the use of this software been reviewed by the judicial system?
Does the software have "-ins" that are produced by another manufacturer?
Is the enhancement process repeatable and reliable?

Image Restoration
Image restoration is any process applied to an image that has been degraded by a known
cause (e.g., defocus or motion blur) to partially or totally remove the effects of that
degradation.
Limitations are imposed on this technique by any noise in the image and by the fact that
information that has been totally lost cannot be replaced. Often partial restoration can be
successful even when total restoration is impossible.

Restoration Techniques
Blur removal is a filtering technique designed to partially or completely remove an image
blur imposed by a known cause. It differs from the image enhancement filtering
processes because the blur removal filter is designed specifically for the process that
blurred the particular image under examination. Examples include defocus and motion
blur, since these blurring phenomena can be described mathematically. Thus, a specific
filter can be designed to compensate for each blur. The degree to which a blur can be
successfully removed is limited by noise in the image, the accuracy with which the actual
blurring process can be described mathematically, and the fact that information has been

533
totally lost and cannot be replaced. Often partial deblurring can be successful even when
total deblurring is impossible.
Color balancing is the extension of grayscale linearization to a color image. It is the
adjustment of the color components of an image. The purpose of color balancing is to
render the colors in the scene faithfully. For example, a color test target having known
colors can be placed in the scene prior to recording the image. Then a grayscale
transformation (nonlinear contrast stretch) can be designed for each color channel (red,
green, and blue) to place the different colors on the test target in their proper relationship.
It is commonly assumed that the color of other objects in the scene will be rendered
accurately as well. Improper color balance can render colors inaccurately, causing objects
to appear to have the wrong color.
Geometric restoration is the removal of geometric distortion from an image. Its purpose is
to restore the proper spatial relationships among the objects in the scene. It can be used
for the removal of geometric distortion, such as that introduced by a curved mirror or a
fish-eye lens. It differs from image warping in that the geometric transformation is
designed specifically for the process that distorted the particular image under
examination. The degree to which geometric distortion can be successfully restored is
limited by the accuracy with which the actual distortion process can be described
mathematically and the fact that information that has been totally lost (e.g., hidden behind
another object or obscured from the camera) cannot be replaced. Often partial geometric
restoration can be successful even when exact geometric restoration is impossible.
Grayscale linearization is the adjustment of brightness relationships among the objects in
a scene. The purpose of grayscale linearization is to render faithfully the different
brightness values in the scene. For example, a monochrome test target having known
gray values can be placed in the scene prior to recording the image. Then a grayscale
transformation (nonlinear contrast stretch) can be designed to place the different gray
values on the test target in their proper relationship. It is commonly assumed that the
other objects in the scene will be put in their proper brightness relationship as well.
Improper grayscale linearization can render brightness values inaccurately so that objects
may appear brighter or darker than they actually appeared when the image was recorded.
Warping, unlike other image restoration processes, changes the spatial relationships
among the objects in an image. It is analogous to printing a photograph on a rubber sheet,
then stretching the sheet in different directions and then tacking it down. Warping can be
used, for example, to remove perspective from an image or to "unroll" a poster that was
wrapped around a pole. Used improperly, it can distort the natural appearance of the
objects in a scene.

Considerations for the Application of Image Restoration Techniques

Question: What type of image must not be restored?
Answer: A primary or original image.
Discussion: Because a primary or original image represents the first instance where the
image is recorded onto any media, or it is an accurate and complete replica of the primary
image, it must not be altered or modified.
Question: Is it necessary to document the restoration process?
Answer: Yes.
Discussion: Documentation of restoration steps is always required.

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Question: Are restored images discoverable in legal proceedings?
Answer: Yes.
Discussion: All images may be discoverable. In cases where images are restored, both
the original and the restored image, along with associated documentation, may be
discoverable.
Question: Who is responsible for testifying about a restored image?
Answer: The person doing the restoration or a person skilled in and knowledgeable about
the restoration process that was used.
Discussion: The person who performed the restoration is best qualified to testify about
the restoration techniques used. However, there may be occasions when the court will
require the assistance of additional subject-matter experts.
Question: Are there legal ramifications associated with the software used specifically for
image restoration?
Answer: Yes.
Discussion: Some considerations may include:
Have the particular functions within the software been accepted by the scientific
community?
Does the software perform as the manufacturer purports?
Has the use of this software been reviewed by the judicial system?
Does the software have "plug-ins" that are produced by another manufacturer?
Is the restoration process repeatable and reliable?
Has the degradation process been accurately modeled?

Image Compression
Digital images produce a large amount of data to be stored. Image compression
techniques reduce the storage requirements by making image data files smaller.

Compression Processes
Lossless compression reduces file size by removing redundant information. Because the
redundant information can be replaced in order to display the image, lossless
compression results in no loss of information. Lossless compression does not alter the
content of an image when it is decompressed. An example of a file format that uses
lossless compression is the graphical interchange format (GIF).
Lossy compression achieves greater reduction in file size by removing both redundant
and irrelevant information. Because the irrelevant information (as determined by the
compression algorithm) cannot be replaced upon reconstruction of an image for display,
lossy compression results in some loss of image content as well as the introduction of
artifacts. The degradation occurs each time the image is saved in a lossy file format.
Higher compression ratios result in the loss of more information. Normally the degree of
compression can be specified. Depending upon the application, lossy compression may
render an image less useful. Caution: Lossy compression should be used with care to
avoid material degradation of the image. Additionally, the compression settings used by
one camera or software program may not be the same as the compression settings used by
another camera or software program.
The commonly used joint photographic experts group (JPEG) image storage format
employs lossy image compression. It is applied to the image in 8-pixel by 8-pixel blocks.

535
Normally, the degree of compression can be specified prior to storing the image. At high
compression ratios, JPEG could remove important image detail and introduce blocking
artifacts as the block boundaries become visible. Digital cameras often create digital
images in JPEG format, so that some lossy compression is unavoidable. The degree of
compression should be set low enough that important image content is not lost or
obscured by artifacts.

Considerations for the Application of Image Compression Techniques

Question: What type of image must not be compressed?
Answer: It depends on the end use and need.
Discussion: In instances where the primary or original image is already compressed, it
should not be further compressed using lossy compression processes; additional data will
be lost. Sources of compressed primary images may include electronic booking
photographs, some types of digital camera images, and images downloaded from the
Internet or E-mail. The file format is not an indicator of the compression history for an
image. For example, a TIFF file may have been previously compressed in a lossy file
format (JPEG). Be aware that the end use of any image may change over time, and the
use of compression may become problematic. Images intended for laboratory analysis
should not be compressed using a lossy process.
Question: Is it necessary to document the compression history of an image?
Answer: It depends on the intended use of the image.
Discussion: The type and degree of compression may become an issue in a judicial
proceeding. Documentation may be necessary in a court of law when argued that
compression might have introduced artifacts or relevant information was lost.
Question: Who is responsible for testifying about a compressed image?
Answer: The person doing the compression can testify about the settings used to
compress an image.
Discussion: Questions concerning the actual compression process should be referred to
individuals who possess sufficient technical expertise to explain the specific process.

Quantitative Image Analysis

Quantitative image analysis is the process used to extract quantitative (measurable) data
from an image, whereas cognitive image analysis is the process used to extract visual
information from an image. This section discusses quantitative analysis only.
Quantitative image analysis requires proper calibration of the image. In a digital image
the pixel spacing must be known in order to extract accurate size measurements. Objects
that are different distances from the camera will have different pixel spacing. The
accuracy of the extracted measurements will depend upon the accuracy of calibration.
Caution: The use of image compression can degrade the accuracy of subsequent
quantitative image analysis.
An example of a quantitative image analysis might be if a circular object in an image
includes 314 pixels, and the area covered by a single pixel is one square millimeter, then
one can conclude that the area of the object is 314 square millimeters. Similarly, if the
distance between the adjacent pixels in an image of a document is 0.02 inches, and the
length of the document is 340 pixels, then it must be 340 times 0.02, or 6.8 inches long.
These examples do not consider perspective distortion.

536
Quantitative Image Analysis Techniques
Colorimetry is the quantification of the color of an object.
Image authentication verifies that the original image has not been altered.
Photogrammetry is the science involving methods, techniques, and analytical procedures
used to make accurate measurements of distances and/or sizes of objects from
photographic images.
Photometry is the measurement of light values of objects in an image.

Considerations for the Application of Image Analysis Techniques

Question: Which types of image should be subjected to quantitative image analysis?
Answer: A working image.
Discussion: Because a primary or original image represents the first instance where the
image is recorded onto any media, or it is an accurate and complete replica of the primary
image, it must not be altered or modified.
Question: Is it necessary to document quantitative image analysis?
Answer: Yes.
Discussion: Documentation of quantitative image analysis steps is required in sufficient
detail to enable another comparably trained individual to repeat the steps and produce the
same conclusions.
Question: Are analyzed images discoverable?
Answer: Yes.
Discussion: All analyzed images, documentation, and conclusions may be discoverable.
Question: Who is responsible for testifying about an analyzed image?
Answer: The person doing the analysis or a person skilled in and knowledgeable about
the analysis performed.
Discussion: The person who performed the analysis is best qualified to testify concerning
the techniques used. However, there may be occasions where the court will require the
assistance of additional subject-matter experts.
Question: Are there legal ramifications associated with the software used specifically for
image analysis?
Answer: Yes.
Discussion: Some considerations may include:
Have the particular functions within the software been accepted by the scientific
community?
Does the software perform as the manufacturer purports?
Has the use of this software been reviewed by the judicial system?
Does the software have "plug-ins" that are produced by another manufacturer?
Is the analysis repeatable and reliable?
Additional Imaging Considerations
Question: Where does image processing take place, in the field or in a controlled
environment?
Answer: Both.
Discussion: Whereas most image processing takes place in a controlled environment,
some image processing, such as photogrammetry and image compression, may take place
in the field.

537
Question: Who performs image processing?
Answer: Photographers, analysts, and technicians.
Discussion: The person performing the processing must be properly trained.
Question: What are file management processes?
Answer: File management processes are the capture, storage, indexing, retrieval, and
archiving of image files.
Discussion: Agencies and organizations should establish file management procedures for
managing image files for use at a later date.
Question: Does image processing alter images?
Answer: Yes.
Discussion: The purpose of image processing is to alter the images in a controlled,
predictable, and repeatable manner. Image processing does not mean that the input image
is overwritten during the process. Forensic image processing should only be performed
on working images.

Guidelines for Digital Image Processing Standard Operating Procedures

The purpose of image processing procedures is to apply processing techniques intended
to enhance, restore, compress, and/or analyze digital images. The success of the
processing of digital images is measured against the four legal tests: reliability,
reproducibility, security, and discovery. To achieve success, standard operating
procedures should be followed. Appendix A is a sample standard operating procedure.

Guidelines for Equipment

The agency should address the following minimum hardware and software equipment
requirements.
Hardware:
Input/capture device
Image processing systems
Output devices
Storage/archive
Software:
Image management
Image processing

Guidelines for Procedures

Agencies should establish specific step-by-step procedures for image processing
according to agency requirements using SWGIT guidelines. These procedures should
address the following as a minimum:
Capture
Processing
Storage/archive
Image management
Security
Output

538
Guidelines for Calibration
If necessary, agencies should develop calibration procedures specific to their needs.

Guidelines for Calculations

If necessary, agencies should develop calculation procedures specific to their needs.

Guidelines for Limitations

Agencies should take into consideration agency-specific budget, equipment,
management, and accrediting agency requirements.

Guidelines for Safety

Agencies should develop safety procedures specific to their needs.

Guidelines for References

Agencies should maintain its agency-specific documentation, manufacturers' manuals,
and SWGIT guidelines.

Guidelines for Training

Agencies should document procedures to ensure sufficient training to afford competence
and proficiency with applicable image processing. Refer to the Guidelines and
Recommendations for Training in Imaging Technologies in the Criminal Justice System
at the following:

539
 APPENDIX L - DEFINITIONS, RECOMMENDATIONS, AND GUIDELINES
FOR THE USE OF FORENSIC VIDEO PROCESSING IN THE CRIMINAL
JUSTICE SYSTEM

Scientific Working Group on Imaging Technologies (SWGIT)

Version 1.2 June 2003

Mission | Introduction | Definitions | Equipment

Guidelines for Video Processing Standard Operating Procedures
Steps for Processing Video Tape

Mission
The mission of the SWGIT Forensic Video Subcommittee is to provide guidelines
regarding video images and their capture, playback, processing, enhancement, storage,
and output in a forensic environment.

Introduction
The purpose of this document is to provide definitions, recommendations, and guidelines
for the use of video capture and processing to ensure the successful introduction of video
imagery as evidence in a court of law. This section includes definitions, equipment used,
guidelines for standard operating procedures, and general procedures for video
processing.

Definitions
CD/DVD (compact disc/digital versatile disc): Optical disc formats designed to function
as data storage media.
Camcorder: A self-contained video camera and recording device.
Capture card/frame grabber: A piece of computer hardware that converts an analog
video signal to digital data.
Deinterlacing: Separating an interlaced frame into two separate fields.
Enhancement: Any process intended to improve the visual appearance of an image.
Field: An element of a video signal containing alternate horizontal lines. In NTSC-
interlaced video, the scanning pattern is divided into two sets (odd and even) of spaced
lines that are displayed sequentially. Each set of lines is called a field, and the interlaced
set of the two sets of lines is a frame.
Forensic: Relating to or dealing with the application of scientific knowledge to legal
problems, especially in relation to the detection of crime.
Forensic video analysis: The scientific examination, comparison, and/or evaluation of
video in legal matters.
Frame: Lines of spatial information of a video signal. For interlaced video, a frame
consists of two fields, one of odd lines and one of even lines, displayed in sequence. For
progressive scan (noninterlaced) video, the frame contains samples starting from one
instant and continuing through successive lines to the bottom of the frame.

540
Interlaced scan: Video image format. The video frame consists of two fields. The first
field contains all the odd-numbered horizontal lines and the second field all the even-
numbered lines.
Monitor: An electronic device used to display live or recorded images.
Multiplexer/demultiplexer (muxer/demuxer): A device used to combine multiple video
signals into a single signal or separate a combined signal. These devices are frequently
used in security and law enforcement applications for recording and/or displaying
multiple camera images simultaneously or in succession.
NTSC: National Television Standards Committee.
Output: The means by which an image is presented for examination or observation.
Playback: Recorded material viewed and heard as recorded, facilitated by camcorder,
videocassette recorder, or other device.
Processing: Any activity that transforms an input image and/or signal into an output
image and /or signal.
Production switcher: A device used to mix video signals from two or more sources (e.g.,
cameras, videocassette recorder/players, time-base correctors, character generators) for
dissolves, wipes, and other transition effects.
Routing switcher: A device used to direct the path of one or more signals into one or
more devices.
Time-base corrector (TBC): An electronic device used to correct timing inconsistencies
and stabilize the playback of the video signal for optimum quality. It also synchronizes
video sources allowing image mixing.
Time-lapse videocassette recorder: A type of video recorder that can be set to record
continuously over long periods, achieved by the tape moving in steps and recording one
frame or field at a time. These devices are frequently used in security and law
enforcement applications.
Vectorscope: An electronic device that measures a video signal's chrominance (color)
performance.
Video: The electronic representation of a sequence of images, depicting either stationary
or moving scenes. It may include audio.
Video distribution amplifier: A device used to divide single video signals, while boosting
their strength for delivery to multiple video devices.
Videocassette recorder (VCR): Multifunction machine intended primarily for playback
and recording of videotape stored in cassettes.
Waveform monitor: An electronic device that provides a graphic display of a video
signal's strength.
Equipment
The purpose of this section is to identify some of the equipment used to view, process,
and enhance video images.
Playback devices must be capable of producing an accurate representation of the recorded
image. Playback devices include but are not limited to the following:
Videocassette recorders, including time-lapse recorders
Camcorders
CD/DVD players
Digital media players
Monitors

541
Processing/Enhancement
Multiplexer
Time-base corrector
Capture card
Frame grabber or other image-capturing device
Computer
Software
Waveform monitor/vectorscope
Editing system
Monitor
Routing switcher
Production switcher
Distribution amplifier
Output/Storage
Monitor
Printer
Videocassette recorder
Storage devices (e.g., computer, CD/DVD recorder, internal or removable memory
storage devices)

Guidelines for Video Processing Standard Operating Procedures

TITLE: Video Processing Standard Operating Procedures
PURPOSE: To apply processing techniques intended to enhance and/or analyze video
images. Note: The successful processing of video images should be made with regard to
the four legal tests: reliability, reproducibility, security, and discovery.
EQUIPMENT: The agency should address the following minimum equipment
requirements:
Hardware
Playback devices
Image-processing systems
Output devices
Storage/archive
Software
Image management
Image processing
PROCEDURES: Agencies should establish specific step-by-step procedures for video
processing in accordance with SWGIT guidelines and agency requirements. These
procedures should address the following, as a minimum:
Playback
Processing
Storage/archive
Image management
Security
Output
CALIBRATION: If necessary, agencies should develop procedures specific to their
needs.

542
CALCULATIONS: If necessary, agencies should develop procedures specific to their
needs.
LIMITATIONS: Agencies should take into consideration budget, equipment,
management, and accrediting agency requirements.
SAFETY: Agencies should develop procedures specific to their needs.
REFERENCES: Agency-specific documentation, manufacturers' manuals, and SWGIT
guidelines.
TRAINING: Agencies should document procedures to ensure sufficient training to afford
competence and proficiency with applicable video processing. (See Guidelines and
Recommendations for Training in Imaging Technologies in the Criminal Justice System
at www.fbi.gov/hq/lab/fsc/backissu/april2002/swgittraining.htm).

Steps for Processing Videotape

Agencies should establish specific step-by-step procedures for video processing in
accordance with SWGIT guidelines and agency requirements. These procedures should
address the following, as a minimum.
Do a visual inspection of the tape and cassette housing to
Ensure housing is intact
Inspect tape for damage (e.g., twisting, separation)
If damage is found, take corrective action and document.
Enable any record-protection device (e.g., punch-out tab, slide record tab, remove record
button).
Determine if the submitted tape is an original or a copy. If it is an original, proceed to
Step 4. If it is a copy, contact the submitter and request that original tape be submitted,
and terminate examination of the copy. If the copy is the best available, proceed with the
examination.
Determine the make, model, and settings of the device used to record the submitted
video, if possible. These settings may include the recording format and speed.
Select the appropriate playback device(s) to achieve optimal signal quality.
Using the selected devices and settings, review the submitted video to locate the pertinent
segment(s).
Determine the appropriate playback speed for processing.
A time-base corrector may be used to stabilize the signal for playback and permit
adjustment of video, chroma, pedestal levels, or other signals.
At the examiner's discretion, a working copy of the pertinent segment may be generated
using an available analog or digital device.
The images may be enhanced using a number of processing operations that may include
but are not limited to histogram equalization, multiframe averaging, contrast and levels
adjustments, and sharpening. (See Recommendations and Guidelines for the Use of
Digital Image Processing in the Criminal Justice System at
www.fbi.gov/hq/lab/fsc/backiussu/jan2003/swgitdigital.htm) .
Once enhanced, the final images are output to appropriate media.

543
 APPENDIX M - GENERAL GUIDELINES FOR PHOTOGRAPHING
FOOTWEAR IMPRESSIONS

Scientific Working Group on Imaging Technologies (SWGIT)

Version 1.1 June 5, 2003

Introduction | Recommended Equipment

Procedure for Footwear Impression Photography

Introduction
The purpose of this document is to describe the proper method of photographing
footwear evidence by qualified personnel.
It is recommended that digital cameras not be used for capturing footwear evidence until
research identifying the minimum resolution required to record these impressions is
complete.

Recommended Equipment
Professional camera, minimum 35mm, with interchangeable lenses, manual override for
exposure and focus, off-camera flash and remote shutter capability, and tripod mount
Macro lens capable of 1:1
Dedicated electronic flash with extension cable for off-camera operation
Remote shutter release
Tripod capable of various angles and positions
Artificial light sources (e.g., floodlights, flashlights)
Leveling device
A variety of black-and-white and color negative film
Appropriate scales
Photographic log
Reflector
Device for blocking ambient light

Procedure for Footwear Impression Photography

A typical standard operating procedure should include the following:
Locate the visible impressions to be photographed.
Photograph the overall view of the area with identifying markers for each impression
using appropriate lighting.
Photograph the midrange view of the impression area with the identifying marker.
To photograph a close-up view:
Mount the camera on a tripod with the film plane parallel to the impression.
Light the impression to bring out the maximum detail. Multiple exposures using various
settings (bracketing) and lighting techniques may be required.
Photograph with and without scale. The scale/identification tag should be placed adjacent
to the impression without obscuring detail and be at least the length and width of the
impression.

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If the impression is processed (e.g., with fingerprint powder or chemicals), re-photograph
after each process.
Prepare the photographic log or worksheet according to agency policy.

545
 APPENDIX N - GENERAL GUIDELINES FOR PHOTOGRAPHING TIRE
IMPRESSIONS

Scientific Working Group on Imaging Technologies (SWGIT)

Version 1.1 June 5, 2003

Introduction | Recommended Equipment

Procedure for Tire Impression Photography

Introduction
The purpose of this document is to describe the proper method of photographing tire
impression evidence by qualified personnel.
It is recommended that digital cameras not be used for capturing tire impression evidence
until research identifying the minimum resolution required to record these impressions is
complete.

Recommended Equipment
Professional camera, minimum 35mm, with interchangeable lenses, manual override for
exposure and focus, off-camera flash and remote shutter capability, and tripod mount
Macro lens capable of 1:1
Dedicated electronic flash with extension cable for off-camera operation
Remote shutter release
Tripod capable of various angles and positions
Artificial light sources (e.g., floodlights, flashlights)
Leveling device
A variety of black-and-white and color negative film
Appropriate scales
Photographic log
Reflector
Device for blocking ambient light

Procedure for Tire Impression Photography

A typical standard operating procedure should include the following:
Locate the visible impressions to be photographed.
Photograph the overall view of the area with identifying markers for each impression
using appropriate lighting.
Photograph the midrange view of the impression area with the identifying marker.
To photograph a close-up view:
Mount the camera on a tripod with the film plane parallel to the impression.
Take multiple overlapping exposures, mapping the entire tire impression.
Light each overlapping section of the impression to bring out the maximum detail.
Multiple exposures using various settings (bracketing) and lighting techniques may be
required.
Photograph with a scale. The scale should be placed along the entire length of the
impression without obscuring detail.

546
If the impression is processed (e.g., with fingerprint powder or chemicals), re-photograph
after each process.

Prepare the photographic log or worksheet according to agency policy.

547
 APPENDIX O - RECOMMENDATIONS AND GUIDELINES RELATING TO THE
USE OF CLOSED-CIRCUIT TELEVISION (CCTV) SYSTEMS IN COMMERCIAL
ESTABLISHMENTS

SCIENTIFIC WORKING GROUP ON IMAGING TECHNOLOGIES (SWGIT)

Dear Colleague,
The Scientific Working Group on Imaging Technology (SWGIT) was created by the Federal
Bureau of Investigation (FBI) to provide leadership to the law enforcement community by
developing guidelines for good practices for the use of imaging technologies within the
criminal justice system. The SWGIT consists of over thirty representatives of federal, state,
and municipal law enforcement organizations, as well as imaging scientists from the
academic community.
In late 2002, the FBI asked the SWGIT to develop recommendations and guidelines relating
to the use of closed-circuit television (CCTV) systems in commercial establishments.
Attached to this letter is the final version of that document.
SWGIT anticipates that this document will be revised over time, as technology and the needs
of law enforcement change. Therefore, you are encouraged to review this document and
provide feedback to us, so that future versions will address the needs of the broadest possible
community.

Specific instructions for providing feedback are on the next page. Please note that you are
being asked to send electronic (e-mail) feedback to both me and Marla Carroll, the chair of
our Forensic Video Subcommittee.
A goal of the SWGIT is to engage broad communities in the development of our guidelines.
Your participation in this process will help us achieve that goal. Thank you for your
consideration.
Sincerely,
Richard W. Vorder Bruegge
Chair, SWGIT

Instructions for suggesting changes to SWGIT documents or submitting general

comments
If you wish to suggest changes in a SWGIT document or submit comments you may do so
electronically or via regular mail.
Formal changes to SWGIT documents will only be considered if the following information is
included:
Title of the document for which the change is suggested;
Name of individual requesting the change;
Organization or Affiliation of the requestor;
Address of the organization;
Telephone number and e-mail address, if available;
Specific identification of wording to be eliminated, noting document section and/or page
number; (if applicable)
Specific wording to be added; (if applicable)
Justification describing reason for making the change.
If simply submitting comments, please be sure to include the following:
Your name;
Your job title;
Name and address of your agency;
Telephone number and E-mail address at which you may be reached (if available); and

548
Identify the specific document, section and/or page number to which you are referring, if
applicable.

If replying electronically (i.e., E-Mail) include your name and address information in the
body of your e-mail and enter "SWGIT CCTV Feedback" as your "subject" line. You may
include your comments in the body of your e-mail or as an attachment in either WordPerfect
or Word format.

Forward your comments to the following e-mail addresses:

rvorderbruegge@fbiacademy.edu
Marla_Carroll@sheriff.org

If replying via regular mail include your name and address information in a cover letter,
followed by your comments, and forward them to the following address:
Richard W. Vorder Bruegge
FBI - ERF - FAVIAU
Building 27958-A
Quantico, VA 22135

Quantico, VA 22135

549
POSTER PRESENTATIONS

550
 SCENE OF CRIME

3D scanning and documentation of objects in forensic science

Walter Brüschweiler, Jörg Arnold, Marcel Braun

Scientific Forensic Service, Zurich City Police,Zeughausstrasse 9

CH-8004 Zurich, Switzerland
walter.brueschweiler@stp.stzh.ch

Key words : Forensic Photogrammetry (FPHG); 3D-digitising-surface Scanner; Patterned

Injuries; Car Accidents, Train Accidents, Airplane Accidents

The documentation of objects in forensic science by photography reduces a three-dimensional

item to a two-dimensional level. Especially if you intend to reconstruct an event as a whole or
partially e.g. the analysis of an injury-causing instrument in a murder case, the impact of two
cars, trains or airplanes in a road, railway or flight accident, you need the highest possible
accuracy of the documentation. Therefore a detailed three-dimensional documentation is a must.
The Forensic 3D/CAD supported Photogrammetry (FPHG) is the basic method to achieve on
scale 3D data.
The advantage of the application of FPHG is that objects like the injuries and the incriminated
instruments, the deformations of the vehicles can be photographed – following some simple rules
– even with a standard 35 mm camera. The data of a series of pictures of an object are fed into
computer programmes and thereby calculated into a 3D data model as a true-to-detail
representation of the item. This allows to examine - in the virtual space of the computer – for
example patterned injuries on a human body with respect to matching potentially incriminated
instruments or deformations of two vehicles in shape, size, depth and angle.
The mentioned procedure can be essentially simplified by using a no-contact optical 3D-
digitising-surface scanner. The advantage is not only to save time. You also get a much higher
number and density of points in the virtual space. That results in a higher accuracy of the 3D
models of the objects to be compared with each other. Combining photography and scanning
enhances the illustrative value of the reconstruction.

551
 Entomological sampling kit
(A little step for the crime scene technician,
a bigger one for the forensic entomologist ?)
Laurent Dourel, Emmanuel Gaudry

Institut de recherche criminelle de la gendarmerie nationale - Département Entomologie

1, boulevard Théophile Sueur
F-93111 Rosny-sous-Bois cedex, France
etm.ircgn@gendarmerie.defense.gouv.fr

It is well known that a good sampling is a first guarantee to realise a good expertise.
Improvement of the quality of the analysis is the aim of each analyst. It is particularly more
important in Forensic science because results induce consequences for the inquiry and their
interpretation has to be justified (testimony of experts during trials).
Since its creation in 1992, staff of the department of Forensic Entomology (Forensic Science
Institute of the French Gendarmerie) has been training Crime Scene Technicians (CST) in the
collection of insects at crime scene and at autopsy. Nevertheless, during several years of activity,
we faced the following situations. (i) Quality of the samples (alive and dead specimens) at their
arrival at the laboratory was not constant. (ii) The collection was sometimes lacking (fauna not
representative). (iii) Insects were sometimes not gathered at all (lack of specific material? An
oversight?).
Several meetings with CSTs and the technical assistants who aid territorial units, on crime
scenes, showed there was a real need to provide them with practical assistance when making a
collection, in the form of a kit containing basic collecting materials, forms and guidelines.
In May 2004, 463 entomological sampling kits (performed by ourselves) were supplied to 237
Criminal Investigation Units (66% of total CIU).
We propose to draw up a balance sheet dealing with the setting up of such kit throughout the 22
French regions.

552
 Human scent identification dogs
Florence Scombart, Daniel Grignon

Sous-direction de la police technqiue et scientifique

service central d'identité judiciaire
31, avenue Franklin Roosevelt 69134 Ecully cedex (France)

Locard's principle stipulates that a person can neither go to a place nor come from it, neither
enter nor leave a room, without bringing and leaving something that belongs to him or her.
“Inevitably, and whatever the precautions taken may be, we leave traces ….” In this case, on the
crime scene or in its vicinity, the perpetrator always leaves an odour.
Scent identifications are based upon the assumptions that every person has a unique odour, that
the odour of a person remains stable in time and that dogs can discriminate between people
based on this odour.
Although there is no 100% scientific evidence that these assumptions are true, there is enough
evidence to use correctly performed and controlled scent identifications for investigative
purposes.
It is possible either to compare scents recovered from the crime scene with the body odour of a
suspect or to establish a link between scents from various scenes in order to confirm or to discard
the possibility that they have been committed by the same unidentified person.
Scent identification was developped thirty years ago in Eastern Europe and more particularly in
Hungary where the two French dog handlers and four dogs have been trained for 5 months.
After an experimental stage which lasted two years, the four scent identification dogs of the
French police began working on operational cases in 2003 and have so far performed some 10
identifications.
The various stages of a scent identification procedure
The recovery of scent traces takes place on the crime scene with objects that are likely to have
been in contact with the perpetrator. Special cloths are needed to recover the scents.
Collection has to take place using only a sterilized equipment (glass jars, cloths and tweezers).
The duration of the collection depends on the places, on the time elapsed since the commission
of the offense and on the surface on which the traces were left, but it will take at least half an
hour or even more.
Recovering scent traces with a cloth is done by placing the absorber on the scented surface and
by wrapping the surface with the absorber.
To prevent other scents from contaminating the absorber, it must be covered with an aluminium
sheet.
The collection of body odours : when a suspect is arrested, his body odour is recovered from his
hands by holding two absorbers in each hand for ten minutes.
The scent identification line-up
The test is performed in a closed room. The handler is helped by an assistant.
An identification line-up arrangement is made of five glass jars.
The dog sniffs at the jar containing the scent trace, at its handler’s command walks along the
line-up arrangement of glass jars containing a single scent from the suspect and other
comparative material. As soon as the dog has found the matching scent, it indicates by lying
down in front of the jar containing the matching scent. The test is performed several times
changing the position of the containers out of the sight of both dog and handler.
To conclude that a suspect's odour matches the scent traces recovered on the crime scene, the test
must be performed by two separate dogs and each dog must indicate the suspect's odour twice.
The procedure is video recorded.

553
 FINGERPRINTS

Decision making processes involved in fingerprint identification:

The influence of emotional context on finding a match.
Ailsa E. Péron1, Itiel E. Dror1, Sara-Lynn Hind1, and David Charlton2
1
School of Psychology, University of Southampton, UK
2
Fingerprint Bureau, Sussex Police, UK

Fingerprint identification, like other cognitive processes, gives the false impression that it is a
purely data driven process. Such processes, supposedly, are driven solely by the information in
the incoming stimulus. In fingerprint analysis this data consists of patterns (such as ridges,
furrows, and whorls) within the impressions themselves.
However, research demonstrates that context plays a major role in filling in gaps and interpreting
ambiguous data. Furthermore, context can override incoming data, even to the extent that the
data is contradicted and we end up perceiving what the context dictates rather than what is
actually there.
Contextual influences are many and varied. In the research reported here we focus on emotional
context which is task-related. Emotional context refers to the emotional state of the decision
maker who is examining fingerprints and trying to see whether or not there is a match. Task-
related emotional context refer to conditions in which emotions are evoked directly from the task
itself.
In this study 27 participants examined 2,484 pairs of fingerprints. In 75% of the trials we
introduced task-related emotional context. We wanted to examine if our manipulation could
cause the participants to be motivated to try and find a match rather than just examine if there is
a match. Thus, we examined whether task-related emotional context increases the likelihood of
finding a match. The remaining 25% of the trials were no context and provided a baseline control
measure.
The emotional context was created by providing background stories and photographs from crime
scenes. Half of the stories and photographs consisted of highly charged emotional content (with
victims of attacks and arson), whereas the other half had emotional content of a lesser degree
(such as bike theft). In addition to having manipulations of high emotional context, low
emotional context, and no emotional context (the control baseline), we introduced subliminal
messages. In 25% of the trials we subliminally flashed the words ‘guilty’ and ‘same’ to further
bias the decision maker to find a match. This was done in addition to the high emotional
condition so as to maximise the strength of our manipulations aimed at biasing the decision
making processes involved in fingerprint identification.
The pairs of fingerprints consisted of impressions of varying clarity. A quarter were relatively
easy to judge, a quarter were relatively hard to judge, and half were ambiguous (not enough
information to judge if they matched or not).
The data revealed that the high emotional manipulation caused participants to increase the rate of
deciding that fingerprint pairs matched. The addition of subliminal messages to high emotional
context further increased the likelihood of finding a match. However, these effects were limited
to ambiguous fingerprints. When the fingerprints were not ambiguous, the emotional
manipulations and subliminal messages were not able to contradict clear non-matching
fingerprints. Hence, while emotional context may influence matching decisions when
fingerprints are ambiguous or degraded, it is not sufficient to override matching decisions based
on clear and detailed fingerprints regardless of difficulty. Our findings are based on non-expert
fingerprint professionals. Further research needs to investigate in what ways expertise and
experience may make people more or less susceptible to these and other contextual influences.

554
 TOOLMARKS & IMPRESSIONS

Serial number restoration in metal surface using digital image processing

and etching techniques

Ladario Da Silva1 & Paulo Acioly Marques Dos Santos2

1
Serviço de pericas em armas de fogo do instituto de criminalistica Carlos Eboli, rua D.
Pedro I, 128, Centro, CEP 20060-060, Rio De Janeiro, (Brasil)
2
Laboratorio de Optico Aplicada do Instituto de Fisica da Universidade Federal
Fluminenese, Av. Litoranea, S/N, praia Vermelha, CEP 24210-340, Niteroi, Rio De Janeiro
(Brasil)
ladario@if.uff.br; pams@if.uff.br

Keywords : Firearms, serial Number Restoration, Digital Image Processing, Applied Optics.
We present a combined cheap method, using non-destructive – digital image processing – and
traditional etching techniques, to recovering obliterated firearms serial number in a metal (steel)
surface. In this work, we report on the characteristics of the method and present some results.
In Rio De Janeiro, a southeast state of Brazil, many of the apprehended firearms have their serial
number obliterated commonly either by strong abrasion or by dotting. One of the most used
traditional method of recovering obliterated stamped serial number is based on chemical
reactions, generally etching solutions [1-2], which are destructive. We investigate a promising
new combined method combining both non-destructive and destructive techniques. This
approach, sometimes, avoid loss of evidence for further analyses. It consists, basically, in a
carefully smooth of the surface and successive capture of the scattered light by the obliterated
region using a stereomicroscope coupled with a digital camera and a flexible cold light source,
appropriate for oblique illumination. By varying the angle between the light and the surface, it
suffices, in certain cases, to see the digits or parts of them directly in the stereoscope or in a
graphical display. Selecting useful image processing filters on the acquired images [3-5], we
could enhance them. This method has already proven to be useful, in certain aluminium dotted
pistol frames, whose serial number was written by laser, when etching methods are not
successful. Digital image processing techniques can also be used for enhancement of images of
recovered serial umbers by destructive usual methods, which sometimes lack of definition. This
method has also the advantage that the laboratory apparatus are, nowadays, basic and almost
standard for any small forensic lab as they can used for other evidence analysis. There are also
free digital image processing programs and filters. This technique can probably be used to
restoring other obliterated marks of similar characteristics. Results are summarized as follows :
(i) The non-destructive method works sometimes very fine with not so destroyed steel surfaces
and in some punctuated aluminium surfaces; (ii) image processing technique enhances the
recovered serial numbers by destructive methods or consists itself in a non-destructive method;
(iii) different filters or combination of filters might be prepared for each sample.

555
 FIREARMS

Ballistic fingerprinting databases

Jan De Kinder

Nationaal Instituut voor Criminalistiek en Criminologie (NICC-INCC)

Vilvoordsesteenweg 98-100, B-1120 Brussels, Belgium

A ballistic imaging database system is based on the following premise: When a gun is fired, it
may leave distinguishing marks on the fired bullet and cartridge case. A searchable database with
images of such marks from all new guns that are sold could be a useful investigative tool. Such a
database would permit the linking of evidence bullets or cartridge cases back to the gun that fired
them, without the need for physically obtaining the firearm. Evidence found at a shooting
incident would be scanned and compared to all entries in the database. Ideally, the system would
provide investigators with the serial number of the firearm which can lead the investigators to the
registered owner. Such a database could be called a “ballistic fingerprint” database or reference
ballistic imaging database (RBID).
A number of questions prior to setting up of ballistic fingerprinting databases are discussed.
These questions can be classified into three categories: (1) concerning the efficiency of such
databases, (2) forensic issues and (3) procedurial issues to be dealt with. The current New York
State legislation is used as a illustration of the choices to be made when setting up a ballistic
fingerprinting database. European data from the possession and use of firearms at crime scenes
will be used to support the three arguments formulated against the installation of a ballistic
fingerprinting database.
In a second step, the feasibility of such systems was tested using the Integrated Ballistic
Identification System (IBISTM) which is successfully used with numerous regional but much
smaller “open case file” databases. In these studies, two cartridges were test fired from a large
number of firearms of the same make and model. One fired cartridge case was entered into the
reference database and a random selection of the remaining fired cartridge cases were compared
against this database. The second cartridge case can be of the same brand of ammunition or of a
different one.
In this presentation, an overview will be provided of the two studies conducted to date.
Suggestions on how to increase the potential performance of a ballistic fingerprint database will
be made. These suggestion will be based on encoding multiple cartridge cases per firearm to
account for differences in ammunition characteristics, taking as many as possible marks from the
firearm and micromarking the important components of the firearm.

References:
Jan De Kinder, Science & Justice 42, 197-203 (2002).Jan De Kinder, Fred Tulleners and Hugues
Thiebaut, Forensic Science Internat. 204, 197-203 (2004)
AB1717 study: http://caag.state.ca.us/newsalerts/2003/03-013.htm

556
 BIOLOGY (incl. Hair)

Digital imaging and image analysis in forensic hair examination

Elizabeth Brooks1, Ian McNaught2 and James Robertson1

Forensic Services, Australian Federal Police, GPO Box 401, Canberra, ACT, (Australia)
Division of Health, Design & Science University of Canberra, ACT 2601 (Australia)
Elizabeth.Brooks@afp.gov.au

The human hair follicle cycle is a focus of research for a number of scientific disciplines as it
presents a dynamic model of a biological system. To the forensic scientist, shed hair at the crime
scene is a valuable source of evidence. Currently, forensic hair examiners are restricted to
characterizing hair essentially by microscopic features that, unfortunately, do not allow
individualizing single human hairs to the exclusion of all others. As such, human hair
comparison techniques used by the forensic scientist are firmly in the realms of ‘subjective’
assessment.
This study attempts to address this ‘subjectivity’ issue. Using digital camera technology and
image processing techniques, we have explored ways to reduce some of the limitations of
‘in/out-of-focus’ imagery and pigment pattern recognition currently experienced by the forensic
hair examiner. Evaluation of imaging systems resulted in selection of the Olympus DP70 digital
camera and Syncroscopy Automontage Software which combines manually selected focal planes
through the hair, usually between 9 and 12 images, vertically stacked to produce a final single
image.
Image analysis using V for Windows (Digital Optics Ltd) was performed on the montaged
images to obtain colour densities and pigment numbers and distributions over a range of
Caucasian head hairs, yielding statistically significant data for use in forensic hair examination.

557
 Use of an automated process for DNA typing of Buccal samples
to supply the French National database
Laure Delpech*, Olivier Marie, Cathy Boudas, Jean-Pierre Brigonne,
Erwann Lozano, Annick Taille, Sylvie Frackowiak and P.-E. Coiffait

Laboratoire de Police Scientifique – 97 Boulevard Camille Flammarion

13245 MARSEILLE Cedex 4 – France
*Laure.delpech@interieur.gouv.fr

The implementation of the French national database of DNA profiles requires, from the forensic
laboratories, highly increasing output in analytic treatment of mass forensic biological samples.
The registered DNA profiles concern suspects, convicted offenders, missing persons as well as
unknown crime scene samples . Among those samples, buccal material collected from
individuals are suitable candidates for automation, as the support of the samples (FTA kits) is
now standardized.
In our laboratory, we have set up a complete automated treatment of FTA samples, which allows
the typing of nearly one thousand profiles per month, realised by four analysts using one robot
line.
This automation has been developed following two approaches :
the development of a software set (that means the fully automatic integration of the data from
the reception of the samples to the printing of the results sheet),
the acquisition of a robotic system for the analytic step.
Practically, samples are first punched using the DBS puncher ; identification data (name, internal
references of the case, references of the procedure) are integrated in a dedicated program which
will trace the sample all along the process, up to the fill of the profile sheet to be sent to the
National Database. The robotic platform (THEONYX® MWG Biotech) operates the successive
washes of the samples, and, as the thermocycler is included in the platform, the amplification
(PCR) set up and course. Ninety six well plates are used, allowing 78 samples to be analysed per
run (the other wells consist in controls and ladders), each run consuming thirty minutes. The
automated process is then interrupted to drive the samples to the DNA capillary electrophoresis
system (ABI PRISM® 3100, Applied Biosystems) to generate the profiles.
A presentation of the whole system is proposed through a video.
The set up of the robotic platform has been realised in respect with the international quality
guidelines. A complete qualification study has been performed by our self, to control
reproducibility, sensibility and fiability of the machine, in parallel with testing the software.
Moreover, a special area is now dedicated to the robot, so that crime scene samples and
comparison samples are totally and physically separated.
At present, the process (robotic line and automatic integration of case and genetic data) runs in
routine. Although the cost of one single automatic analysis is not significatively different from
the manual analysis (except for the invest due to the machine), the incidences are obviously
considerable in the following terms :
output : an increase of approximately 700% profiles is obtained per month,
personnel involvement seriously reduced (analytic and administrative tasks simplified)
reliability of the analysis increased.
In conclusion, the automation of DNA typing is an obligatory step to accelerate the growth of the
national database. It is now possible to acquire flexible platforms adapted to different levels of
output, but the combination with a convenient informatics environment is of course, highly
recommended. After a couple of months of routine use, we consider our choice to be perfectly
suitable with our structure and our regional activity.

558
 FSS DNA expert systems
Dr Chris Maguire

The Forensic Science Service

Trident Court 2920 Solihull Parkway Birmingham Business Park, Birmingham B37 7YN
(UK)

There are many laboratories currently working to automate the process of DNA profiling and
several companies able to supply robotic workstations and liquid handling systems needed to
support such automation. The rate-limiting step for achieving a fully automated DNA process is
the automation of the interpretation of DNA profiles.
The FSS has developed a suite of software tools to manage this process, including:
Interpretation of single source DNA profiles and designation of alleles present
Designation and interpretation of mixed profiles
Anti contamination checking
Assessment of DNA profiling results for court purposes
The FSS has seen a number of significant benefits from using these software tools. These
benefits include:
An improvement in consistency as the software tools employ a set of objective rules for the
interpretation of single source and mixed DNA profiles
Demonstrable efficiency gains in both the analysis and interpretation of DNA profiles
De-skilling the interpretation of mixed DNA profiles
Maximising the loading rate of DNA profiles to the National DNA Database.
During this presentation the FSS will discuss the development of our suite of software
applications and present the lessons learnt during their development.

559
 ACOUSTICS & IMAGING

Forensic speech and audio analysis 2001-2004: a review

Ton Broeders and Jos Bouten

Netherlands Forensic Institute

Although the development of state-of-the-art speaker recognition systems has shown

considerable progress in the new millennium, performance levels do not as yet seem to warrant
large-scale introduction in anything other than relatively low-risk applications. Conditions
typical of the forensic context such as transmission channel mismatch, mismatch of linguistic
context and the complexity of proper threshold setting continue to pose a major challenge.
Consequently, the impact of automatic speaker recognition technology on the forensic scene has
been relatively modest. Meanwhile, forensic speaker identification practice continues to be
heavily dominated by the use of a wide variety of largely subjective procedures. Against this
background, the need to put alternative validation procedures in place is becoming more widely
accepted.
While the increasingly widespread availability of digital sound processing equipment as well as
its ease of operation make certain types of manipulation of audio recordings comparatively easy
to perform and difficult to detect, thereby severely limiting the possibilities of audio integrity
and authenticity examinations, new developments in tape authentication based on mains
frequency fluctuation and the visualisation of the magnetic domain using the Faraday principle
show considerable promise
A survey is provided of ongoing work in the area, based on reactions to a questionnaire.

560
 Forensic image analysis 2001-2004: a review
Jurrien Bijhold(1), Zeno Geradts(1), Lena Klasen(2)

1 Netherlands Forensic Institute (NFI)

2 Swedish Defense Laboratory (FOI)

The rapid development of digital imaging technology and widespread use of camera’s and video
recording systems for private and public applications has had a big impact on the development of
forensic image analysis. Three mainstreams of activities can now be distinguished in forensic
image analysis:
Imaging technology
Capturing images and video from analog and digital media, filtering and sorting large amounts of
images and video, coding and decoding data, detection of manipulation, image authentication,
identification of camera’s and systems as tools used for production of e.g. child porn movies. In
this field of expertise a lot of cooperation is needed with experts in audio technology, digital
evidence and information technology in order to keep up with all new developments.
Crime scene photography, laser scanning, photogrammetry and 3d-modeling
Crime scene recording using combinations of wide view and close up photography and laser
scanning, panorama views, 3d-modeling of crime scenes, 3d-models as tools for interpretation of
questioned video recordings of e.g. shooting incidents, car accidents or explosions, scenario
testing using 3d-models of the crime scene, human bodies with wound channels, virtual stringing
of bloodstain patterns, etc. In this field of expertise many new forensic applications are being
explored.
Biometric identification
The international concern for terrorist attacks has led to large investments in projects for testing
and introducing biometric systems based on finger scans, facial photographs and iris scans. The
demand for extremely large databases of finger scans and new insights from the development of
DNA evidence has led to a new interest for the process of fingerprint capturing and
identification.
While guidelines and procedures have been developed for forensic comparison of facial
photographs and estimation of body heights from surveillance video, it also has become apparent
that these methods for identification have to be used extremely carefully. New developments can
be expected from facial 3d-scans and 3d-data extraction from video.
The development of forensic image analysis has also been pushed by the consolidation of a
number of relatively new international working groups: the European group ENFSIDIWG
(methods and techniques), the US groups SWGIT (guidelines and best practice manuals) and
LEVA (training on video processing), and the Australian group EESAG (proficiency tests for
video and audio processing).
A survey is provided of ongoing work in the area, based on reactions to a questionnaire.

561
 M.A.R.I.N.A.
(Moyen Automatique de Recherche d’Images Non Autorisées)
Laurent Lesobre

Institut de recherche criminelle de la gendarmerie nationale - Département Informatique

Electronique
1, boulevard Théophile SueurF-93111 Rosny-sous-Bois cedex, France
inl.ircgn@gendarmerie.defense.gouv.fr laurent.lesobre@wanadoo.fr

MARINA is a software developed to assist investigators in their fight against the distribution of
child abuse images. It overviews, in read-only mode, the file systems of an investigated hard
drive, searching for images and videos that have been referenced as child pornography by
gendarmerie units, while preserving the original evidence.
The current version of MARINA is based on the use of MD5 hash signatures: a mathematical
function that does not permit to calculate the image back from the signature (non-reversible).
The database currently includes over 344.000 image signatures. This number has proven
sufficient to detect the most common locations of child pornography, but will increase in the
future with information from newer cases. The software presents itself in the form of a bootable
Linux CDROM.
The main features of this software are:
- The simple search of images and videos;
- The search and copy of images and videos (the copy is done to a hard drive provided by
the investigator);
- The copy of all images and videos (to enhance the finding capacities afterwards);
- The copy of archive (compressed) files or those linked to the use of electronic mail;
MARINA is currently available for all Gendarmerie units in France and will be deployed this
year to Police Nationale (the other national police force) units as well.

562
 DRUGS

Supporting complex criminal investigations by information derived from systematic

profiling of drugs.

A. Gallusser1, A. Biedermann1, Y. Specht2, P. Esseiva3, F. Anglada3

Federal Department of Justice and Police, Federal Office of Police, Forensic Science Unit,
Nussbaumstrasse 29, 3003 Berne, Switzerland
Federal Department of Justice and Police, Federal Office of Police, Branch Lausanne, Av.
Bergières 42, 1004 Lausanne, Switzerland
The University of Lausanne, School of Criminal Sciences, Institut de Police Scientifique,
Bâtiment de Chimie, 1015 Lausanne-Dorigny, Switzerland

Since 2002, the Federal Office of Police (Fedpol) carries out investigations under the direction of
the Attorney General of Switzerland in cases involving organised crime, money laundering and
corruption.
Drug-related offences such as importation, exportation, supply and possession are particularly
demanding areas of investigation. There is a great need for sources of information allowing for
further insight in the organisational structures of specific groups of offenders and their activities
on a national and international level.
One such source of information are links between samples of illicit drugs which may be
characterised by systematic physical and chemical profiling. The document describes
collaboration between police investigators, forensic scientists and a specialist laboratory. A
practical case is presented where the profiling of samples of illicit drugs has been found to
provide accurate, timely and useful information for linking spatially and temporally distinct
events on a national and an international level.
Current efforts of the Forensic Science Unit at Fedpol tend to incorporate such analyses
systematically in casework with the aim of providing unique and consolidated overviews of
cases in complex criminal investigations.

563
 A contribution to the chemical profiling of 3,4-Methylenedioxymethanphetamine
(MDMA) tablets
Pascal Gimeno, Fabrice Besacier, Huguette Chaudron-Thozet, josiane Girard, Alain
Lamotte

Laboratoire de police scientifique de Lyon

31, avenue Franklin Roosevelt, 69134 Ecully cedex (France)

A method for the profiling of 3,4-Methylenedioxymethanphetamine (MDMA) tablets is

presented. Impurities of interest are extracted from an alkaline buffer solution (pH 11.5) by
diethyl ether and submitted to Gas Chromatography – mass spectrometry analyses. Identification
of impurities is performed by electron impact ionisation (Ei) mass spectrometry and
confirmation by positive chemical ionisation (Ci+) mass spectrometry or , when possible, mass
spectrometry / mass spectrometry (MS²). The reproducibility evaluation and the profiling
comparison are performed using Selected Ion Monitoring (SIM) on the most intense impurity
mass fragment.
This profiling method allowed to identify new impurities such as p-methoxymethamphetamine
(PMMA) and 3,4-Methylenedioxy-N,N-dimethylbenzylamine. Repeat extractions of the same
sample gave an average relative standard deviation of less than 8% within the same day and 11%
between days.
Comparison of profiles showed a good potential of the method to discriminate MDMA samples.
Nevertheless, it is necessary to increase the number of linked and unlinked samples so as to
determine the correlation value threshold.

564
 Usefulness of MDMA Impurity Profiling for Intelligence and Legal Purposes

Dariusz ZUBA1, Małgorzata ŚWIST2, Bogumiła BYRSKA1, Jarosław WILAMOWSKI2,

Andrzej PARCZEWSKI1,2, Wojciech PIEKOSZEWSKI1
1
Institute of Forensic Research, Cracow, Poland
2
Faculty of Chemistry, Jagiellonian University, Cracow, Poland

Key words: profiling, Ecstasy, MDMA

Profiling of drugs appears a useful method in criminal investigation aimed at searching for illicit
drug production and distribution. It includes the chemical analysis of impurities derived from
their manufacture or from co-extraction. Although impurity profiling of seizure drugs is not a
routine technique, it could provides useful information about synthesis methods and it hepls to
establish whether the seizure drug samples originate from the same illegal laboratory or the same
production batch. Out of synthetic drugs, amphetamine and methamphetamine have been
thoroughly investigated in respect to the route specific impurities and comparative analysis. 3,4-
methylenedioxymethamphetamine (MDMA, Ecstasy) have not been sufficiently investigated so
far.
Institute of Forensic Research, in co-operation with Jagiellonian University and Central Forensic
Laboratory of the Police in Warsaw, realizes a project “Development of the analytical and
chemometrical procedure for Ecstasy profiling for needs of drug database”. In this presentation
the results obtained at the first stage of investigation are shown.
MDMA samples prepared by different routes, namely: reductive amination, Leuckart reaction
and safrole bromonation, were studied. The reductive amination was performed using different
reducing agent: sodium cyanoborohydride, aluminium amalgam and sodium borohydride. The
study covered also examination of MDMA precursor - 3,4-methylenedioxy-phenyl-2-propanone
(MDP2P or PMK), which was obtained by oxidising isosafrole and from piperonal. Each
synthesis was repeated three times in order to establish variety in composition of impurities
between different batches of PMK and MDMA.
Gas chromatography coupled to mass spectrometry (GC-MS) was applied to identify precursors,
intermediates and by-products. Liquid-liquid extraction (LLE) with n-heptane from carbonate
buffer of a pH 10 was used in sample preparation for GC-MS. Diphenylamine was applied as an
internal standard. Chromatographic separation was achieved on HP5-MS fused silica capillary
column.
High-performance liquid chromatography (HPLC) was tested as an alternative and confirmatory
method. The samples were prepared by means of solid-phase extraction (SPE). An MDMA
sample was dissolved in ammonium buffer (pH 8.5) containing diphenylamine and the impurities
were thicken on Bakerbond speTM Octadecyl column using methanol for extraction. Chromolith
Performance RP-18e monolithic column was used in HPLC analysis. The gradient separation
was performed using aqueous solution of phosphoric acid and acetonitryle. The gradient program
was optimised. Diode array detector (DAD) was used for detection of analytes.
The impurities pattern is a subject for further chemometric analysis. The obtained results till now
show that the worked-out methods allow to distinguish the samples prepared by different
synthesis route. They can also be useful in comparative analysis of seized drug samples.
The study was supported by the grant of the State Committee for Scientific Research, Warsaw,
Poland, number 0T 00C 01024.

565
 Scientific Contribution to the Fight against Cross-border drug trafficking
A European project between France and Switzerland
Lociciro S.*, Hayoz P.*, Dujourdy L.**, Besacier F.**, Margot P.*, Esseiva P.*, Guitton
J.***.

* Institut de Police Scientifique, University of Lausanne, BCH, 1015 Lausanne-Dorigny,

Switzerland
** Laboratoire de Police Technique et Scientifique de Lyon,
31 avenue Franklin Roosevelt, 69134 Ecully cedex, (France)
*** Institut des Sciences Pharmaceutiques et Biologiques, Universite Claude Bernard Lyon
I,
8 avenue Rockfeller, 69008 Lyon (France).

The aim of the project is to develop an harmonised analytical and statistical methodology
between two laboratories (IPS of Lausanne and LPS of Lyon) in order to provide “drug
intelligence” for the cocaine seized at the border and inside the two countries.
Common standard operating procedure for the analysis of cocaine samples will be established
and based on gas chromatography - flame ionization detection (GC-FID). The aim is to optimise
the chromatography of cocaine samples and to target minor alkaloids which are the signature of
each sample.
Once this optimisation is realized, these alkaloids can be used to compare samples in order to
highlight chemical links between cocaine seized in both areas. These links will be stored and
managed in a common database on the Internet. Data protection protocols ensure that the
exchange of information between the two laboratories is confidential.
This database will then be used to update data in quasi real time. The challenge is to put together
the chemical links and the traditional police information in order to interpret and validate the
value of chemical links. The services concerned (police, customs, public health) will be informed
about the results among others by using continuing education for network understanding. This
could also help police forces to find new traffic networks or to link dealers with no apparent
relationship.
Dissemination of the results will also be done through communication at international
conferences or publications.
The expected results of the project would :
- make police forces aware of profiling tool and issues in order to make them integrate this
information in their casework ;
- promote exchanges between drug enforcement services ;
- help to identify and dismantle the traffic networks between Switzerland and France, with
valuable consequences in terms of public health and social environment ;
- provide information about the quality and the toxicity of the products to the institutional
structures in charge of drug-addiction monitoring.

566
 FIRE

Development of validation kits for fire debris and DNA analysis

David M. Epstein & William J. Tilstone

NFSTC, 7881 114th avenue, Largo, Florida 33773 (USA)

dme@nfstc.org

Accreditation standards, especially ISO/IEC 17025 clause 5.4, require that test methods used be
properly validated before evidence is analyzed. Clause 5.4 gives some guidance for performing
validation studies. Other standards, such as Standard 8 of the Quality Assurance Standards for
Forensic DNA Testing Laboratories used in the United States, also require validation of test
methods and give more detailed guidance to laboratories. However, there have been no specific
guides provided to laboratories of the actual steps to take to demonstrate validity of test methods.
The National Forensic Science Technology Center (NFSTC) has worked within a cooperation
agreement with the United States National Institute of Justice ("2000-RC-CK-K001) to design
and test validation kits for testing fire debris as well as DNA. The focus on the kits and the two
areas of testing came from a focus group of crime laboratory directors sitting on the board of the
American Society of Crime Laboratory Directors (ASCLD). This poster will cover the planning,
design, production, and initial testing of the validation kits, which NFSTC will provide to
publicly-funded forensic laboratories in the United States in the coming months.

567
 EXPLOSIVES

Analytical problems with RDX blast residues

Dr. R.S. Verma & Mr. A.K. Dalela

Central Forensic Science Laboratory, Directorate of Forensic Science, Ministry of Home

Affairs, Govt. of India, Chandigarh – 160 036, INIDA.
cfslchandigarh@indiatimes.com

RDX has figured in sensational blasts in India such as killing of dignitaries, Bombay bomb blasts
1993 & 2003 and blast outside J & K assembly. Blasts of RDX formulations generate new
complications to the forensic scientists in addition to inherent problems. Extreme conditions of
temperature and pressure in blasts leave behind traces of parent substance too small to detect
easily. Additives of the formulations make analysis further difficult due to their own presence
and also their break down products. RDX also decomposes to many new products. Presumptive
tests, chromatographic analysis and FTIR spectrophotometric analysis of such samples provide
insufficient data for identification of parent explosive substance. Higher operational temperature
and hot surfaces of the GC-MS also decompose heat labile RDX. Better results have been
achieved with trace blast residues by improving upon extraction methods minimising impurities
and shortening capillary column length used in GC-MS. Scan by scan analysis of total ion
current chromatogram with their interpretation in relation to structures of the ions formed
revealed formation of additional structures, which can also form due to explosion of RDX. Some
of such products formed due to decomposition of RDX can be stable enough to remain in post
blast residues, creating spectrum, different to that of RDX, however, also similar to mass
spectrum of RDX due to the presence of some common ions. In-depth analysis of expanded
FTIR spectrum may also enhance the accuracy of results of trace level residues of RDX.

568
 Metallographic observation of mechanical twins in 304 stainless steel
after small charge explosions
D. Firrao, P. Matteis, G. Scavino, G. Ubertalli
Dip. di Sc. dei Materiali e Ing. Chimica, Politecnico di Torino, Torino, Italy

M.G. Ienco, P. Piccardo, M.R. Pinasco, E. Stagno

DCCI - Università di Genova, Italy

R. Montanari, S. Poggio, M.E. Tata

Dip. di Ing. Meccanica, Università di Roma-Tor Vergata, Roma, Italy

G. Brandimarte, S. Petralia
Marina Militare - Istituto Chimica Esplosivi – Mariperman, La Spezia, Italy

Optical metallography is the preferred tool to assess the existence of mechanical twins in
deformed metal parts. When FCC metal components are exposed to the effects of explosions,
twinning may become the preferred mode of plastic deformation in place of slip if the stacking
fault energy (SFE) is low. In the case of small charge explosions that yield limited overall plastic
deformations, the occurrence of mechanical twins in metal parts may become the only way to
single out the original cause of a destructive event.
Owing to their particularly low SFE’S, austenitic stainless steels are the best candidates for
experiments leading to the assessment of the effects of small charge explosions. In the
framework of a large research program encompassing various FCC metals, AISI 304 K steel
discs have been exposed to the explosion of 108 g TNT equivalent charges at distances ranging
between 5 and 80 cm. Polished 22 mm diameter, 3 mm thick steel discs were obtained from bars
solution annealed at 1200 and 1050 °C to yield 60 and 32 µm average grain size, respectively.
Larger grain size disks were also exposed at 54 g charges. After explosion surfaces were
observed both by scanning electron and optical microscopy, ascertaining that the latter yielded
best observation results. The discs were then cut along a diameter by EDM and their sections
observed for in depth effects.
The influence of charge-to-target distance, steel grain size and explosive charge is hereby
summarized.
At the shortest distances, surfaces showed alterations due to gas washing in every case. At
increasing distances mechanical twins became clearly observable, diminishing in deformed grain
frequency at distances above 12 cm. 108g charges gave no surface effect at distances above 20
cm for 32 µm grain sizes and above 22 cm for 60 µm grain sizes. For the latter microstructure,
such a limiting distance decreases to 15 cm with 54 g charges.
Upon sectioning mechanical twins never occupied the entire section. At very short distances they
are visible both at the impinging wave surface as well as at the reflected wave one, then only for
some depth from the front surface. With 108 charges such a deformed depth nullifies for the
smaller grain size at 15 cm charge-to-target distance and at 20 cm for the larger grain size. 60 µm
grain sizes disks showed no effect at 15 cm distance when the equivalent TNT charge was 54 g.
The above findings were then interpreted in terms of maximum shear stresses originated from a
shock wave pressure.

569
 The five terrorist attacks on 16 may 2003 in Casablanca (Moroccoc)
Agnès Guironnet , Anne Françoise Ferroud,

Laboratoire de Police Scientifique de Lyon, 31 avenue Franklin Roosevelt-69134 Ecully

Cedex - France

Twelve persons (four scientific explosive specialists, two from LPS1 Lyon, Two from LCPP2 and
eight police officiers from SCIJ3 ) made up this French team.
Five different sites were simultaneously aimed by 14 kamikases; Farah Hotel, Casa
Espana,Positano restaurant, Jewish Alliance, Jewish cemetery in the Medina.
We assisted the police investigator at the scene of explosion and the scientists in laboratory:
At the scene of explosion
We assisted them to investigate marks and items of evidence in the five sites (drawing up plans
and photography, samples) in order to establish the number of kamikases, the nature of the
explosives.
In the Laboratory
A small plastic bottle was found at the Farah Hotel, It contained a white substance with seven
metallic balls. This substance was analysed at the Casablanca Laboratory with the LCPP
assistance and ours. On may 18 th, the first analysis led to advance that it was TATP (Triacetone
TriPeroxyde) mixed with ammonium nitrat. The organic phase analysis were realized by GC/MS
and IRTF. The inorganic phase analysis were made by X diffraction and Ionic Chromatography.
The Morocco police searched house in two residences
In the first, some different materials were seized (bottles of acetone and hydrogene peroxyde,
agitator, glassware...). In the other, cracker, alarm clock were found. We assisted them to the
result operation and the “modus operandi” when explosive like TATP was discovered.

1
Laboratoire Police Scientifique
2
Laboratoire Central Préfecture Police
3
Service Central Identité Judiciaire
570
 Post blast detection of explosives residues and forensic analysis of debris in urban area
explosion experiments. Use of high-quality 3D digital camera for area mapping
A. Gregori1, A. Russo1, R. Calò1, L. Bosio1, G. Ciotola1, D. Coppe2, and L. Garofano1.

Raggruppamento Carabinieri Investigazioni Scientifiche1, Italy.

Istituto di Ricerche Esplosivistiche, Parma, Italy2.
risprchimica@carabinieri.it

The risk concerning terrorist attacks using explosive devices in the world is greatly increasing.
Even in Italy, a growing alarm is recently perceived. From this arises the need of performing
exercitations to improve the cooperation between the many Departments and to unify the
operational protocols.
In April 2004, a simulation in urban environment, covering the examination of the scene after an
explosive attack, has been performed. The activity involved personnel from 4 Carabinieri
Departments (Roma, Parma, Messina, Cagliari). The main objectives were:
To evaluate the effectiveness of the scene examination protocols currently utilized;
To test the field explosive detection device (Ionscan);
To gain ballistic information to verify the theoretical calculations for the determination of the
quantity of explosive utilized;
To verify the persistence of biological traces and fingerprints upon the remains of the starters and
other parts of the exploding devices;
To experiment new technologies for the 3D reconstruction of the explosion’s area.
To take fast video recordings to study the dynamic of the explosion and the distribution of the
fragments;
Five bombs were detonated, the first one made of 100 grams of RDX + 50 grams of TNT + 420
grams of gel explosive GOMA 2 ECO put in bag outside the window of a building. The second
was a car fire extinguisher, with the capacity of 2 litres, filled up with 250 grams of GOMA 2
ECO and 800 grams of RIOGEL and a slow action fuse, put inside a room of the building. A
small quantity of TATP has been blown up with an electrical starter to evaluate the explosive
potential and the best examination protocol (SPME). The other devices, of lesser potential,
consisted in RDX and TNT (90/10, the first one) and smokeless powder (pipe bomb, the second).

571
 ENVIRONMENTAL CRIME

Design and operation of an air analysis laboratory

Robert Bohn, Jim Hoban, and Laurence Strattan, Ph.D.

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

In the late 80’s, the U.S. Environmental Protection Agency published methods for the analysis of
volatile organic compounds (VOCs) collected in stainless steel canisters. The USEPA National
Enforcement Investigations Center (NEIC) has a dedicated air analysis laboratory with
instrumentation and equipment designed specifically for the analysis of air samples collected
using inert-lined canisters. This type of analysis has proven useful in routine casework involving
multimedia investigations, such as refineries and chemical plants, and has been required for
specific criminal cases and Homeland Security applications.
The inert-lined canisters are designed for “whole air sampling.” The canister takes and preserves
a portion of the atmosphere from that particular sampling location. The inert lining within the
canister keeps the contents, the sampled ambient air, from degrading prior to analysis.
This sampling method has several advantages over the use of sorbent tubes, another method of
VOC sampling. Canister sampling provides enough sample for multiple analyses and for quality
control (QC) measures; canisters sizes used by NEIC range from 400 mL to 15 L. Air samples
can be treated very much like liquid or solid samples. Analyses may include replicates, spikes,
and additional QC as deemed necessary by the analyst. Canisters are cleaned and tested for
cleanliness before being prepared for future field sampling.
Analysis is performed using gas chromatography with mass spectrometry (GC/MS) detection.
Detection limits for analysis range from the tens of parts per billion volume (ppbv) for a 1-mL
sample size to sub part per trillion volume (pptv) for hundreds-of-mL sample sizes. The method
used for this analysis is based on Method TO-15 from the USEPA “Compendium of Methods for
the Determination of Toxic Organic Compounds in Ambient Air.” The system can use either a 1-
mL sample loop with precise flow splitting, appropriate for industrial hygiene applications, or
flow measurement for samples from 20 mL to hundreds of mL, appropriate for ambient air
analysis.
Photos, technical specifications of the hardware and software involved in air analysis, details of
procedures involved for canister preparation for sampling, proper dilution of air standards during
analysis, and the cleaning of the canister post-analysis will be included in the poster. Additional
information regarding sources for air standards, instrumentation, and equipment will also be
provided.

572
 Determination of perfluorinated surfactant in water by liquid chromatography-negative
ion electrospray/ion trap mass spectrometry
C.R.Casey, Laurence Strattan, Ph.D., T.L. Jones-Lepp, and D.A. Alvarez

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

Perfluorinated surfactants are used in the production of a wide variety of products. These
compounds are persistent in the environment and have toxicological effects on humans and other
animals. Perfluorinated surfactants have been detected in widely distributed surface waters and
biological matrices. Due to these concerns at least one major manufacturer has started to phase
out their production. The possible routes of exposure to the environment include the water
supplies located near production plants. Hence, there is a need to monitor low concentrations of
these compounds in the environment. The United States Environmental Protection Agency
(EPA) and major manufactures have developed an approach to gather information on possible
health effects and routes of human exposure.
In 2003, the United States Environmental Protection Agency (USEPA) released a preliminary
risk assessment for the chemical perfluorooctanoic acid (PFOA) and began a process of meetings
to gather additional information on PFOA and any fluorinated telomers which may metabolize or
degrade to PFOA. At that time, enforceable consent agreements (ECA) were negotiated between
USEPA, the industry, and interested parties that required technical data regarding perfluorinated
surfactants to be generated and submitted on a specified schedule to USEPA.
One possible route for exposure of perfluorinated surfactants to the environment is through the
water supplies located near production plants. The surface waters close to the DuPont
Washington Works plant, a major producer of PFOA, were sampled for analysis of
perfluorinated surfactants. Samples from drinking water wells, wastewater treatment facilities,
and urban creeks were sent to the NEIC for analysis of three specific perfluorinated compounds:
perfluorooctanoic acid (PFOA), perfluoroheptanoic acid (PFHpA), and perfluorooctane sulfonate
(PFOS). Existing analytical methods were modified and optimized to accommodate the NEIC
instrumentation. The analytical method required the use of solid phase extraction (SPE) coupled
with liquid chromatography-negative ion electrospray/ion trap mass spectrometry (LC-
NIES/ITMS).
A contract laboratory, hired by DuPont, also performed analyses for PFOA on well water
samples located near the plant. A comparison of the NEIC data to the contract lab data, details
about the sampling (with photos), analysis (method specifications), and regulatory concerns
regarding perfluorinated surfactants will be included in the poster.
The National Enforcement Investigations Center (NEIC) joined a collaborative sampling and
analytical effort with the United States Geological Survey – Columbia Environmental Center
(USGS-CERC), the USEPA Office of Research and Development National Exposure Research
Laboratory – Environmental Sciences Division (ORD/NERL-ESD), and a USEPA regional
office. USGS-CERC developed a novel sampling device, the Polar Organic Chemical Integrative
Sampler (POCIS), for sequestering and concentrating waterborne polar organic chemicals. These
samples were collected at wastewater treatment facilities and urban creeks. NERL-ESD
analyzed sample extracts for pharmaceutical compounds, methamphetamine, and 3,4-
methylenedioxymethamphetamine (MDMA). The extracts were sent to the NEIC for analysis for
perfluorinated surfactants. PFOA and PFOS were qualitatively identified in the sample extracts
submitted to the NEIC.

573
 Field portable analysis
Donald J. Smith

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

The USEPA National Enforcement Investigations Center (NEIC) Laboratory Branch has
recently been developing a strategy for field analysis work. The goal of the analytical strategy is
to acquire and maintain the capability to provide rapid initial assessments of any type of sample
(solid, liquid, gas, or suspended particulates) prior to shipping to the laboratory for additional
testing (primary or confirmational analysis). Within this strategy, the NEIC is attempting to
provide as many analyses as possible with instruments that are easy to use, portable, and
lightweight. The instruments are part of a field-portable package that weighs less than 100
pounds and can be staged and ready for rapid response analytical support.
Some of the instruments included as part of the field-portable kit are a tube-excited X-ray
fluorescence spectrometer, an anodic stripping voltammeter, a Hazcat Chemical Identification
System, and a gamma spectrometer. Additional instrumentation, such as a HAPSITE gas
chromatograph/mass spectrometer, can be included with the kit when advance notice is provided
to the laboratory.
The tube-excited portable X-ray Fluorescence (XRF) spectrometer is a handheld energy
dispersive XRF analyzer that uses a miniature X-ray tube instead of a radioactive source and has
a high-resolution detector system (200 eV FWHM at 5.95 keV Mn spectral line). The instrument
has the capability to analyze for all of the USEPA RCRA and Priority Pollutant metals (Cr, Co,
Ni, Cu, Zn, As, Se, Ag, Cd, Sn, Sb, Ba, Pb, Hg, and Tl) in solid or liquid samples. The
spectrometer is equipped with X-ray tube filtering for enhanced detection limits on specific
metals. It also includes a light element analysis package that uses a combination of filtering and a
thin detector window to make light element detection possible. Additional improvements in light
element detection can be made by optimizing the tube current and voltage.
The portable anodic stripping voltammetry (ASV) system is designed for immediate on-site
identification of trace metals in water. The system can analyze for cadmium, arsenic, lead,
selenium, chromium, silver, and mercury at part per trillion levels in under three minutes. The
ASV system is very small (approximately 5” x 2” x 1”) and can be powered through the USB
port of a laptop computer.
The Hazcat Chemical Identification System is designed for immediate on-site identification of
hazardous materials using a variety of simple chemical tests. It also contains a Meth Kit option
for quickly identifying chemicals and wastes associated with the illegal manufacture of drugs.
The portable gamma spectrometer is used to identify gamma-emitting contaminants at sites
where radioactive substances may have been intentionally released. The portable gamma
spectrometer system provides analysis of radiological contaminants on-site in minutes. The
system is equipped with a 2” x 2” NaI detector to provide sufficient sensitivity for screening for
ambient levels of gamma radionuclides but does not require liquid nitrogen like germanium
detector systems. Signals are processed using quadratic compression conversion technology.
This optimizes the spectrum so that peaks are well separated at high, low and all energies in
between. Conventional spectroscopy requires a choice between optimizing either high or low
energy peaks. Since this system must be used for unexpected radiological contaminants,
optimization throughout the spectrum is needed.
Photos, specifications, and examples of on-site usage by NEIC personnel will be presented on
this poster.

574
 Toxicity Characteristic Leaching Procedure (TCLP)
and iron treatment of brass foundry waste
Douglas Kendall, Ph.D.

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

The Toxicity Characteristic Leaching Procedure (TCLP) is used by the United States
Environmental Protection Agency to determine if wastes contain extractable components subject
to hazardous waste regulations. This poster illustrates and examines the limitations of the TCLP
and the way it is used by studying a particular example.
Waste casting sand from brass foundries, to which iron metal has been added, passes the TCLP
test, but when placed in a landfill for several years may start to leach lead, copper and zinc.
Results of TCLP tests of waste sand alone, and with the additives iron metal, zinc metal, hydrous
ferric oxide and hematite, are reported.
Three processes were studied: reduction by metallic iron, sorption by hydrous ferric oxide, and
precipitation of hydroxides. Lead, copper and zinc behave differently with respect to these three
processes, and their measurement allows some deductions as to what is occurring in a TCLP test
or a landfill. Iron addition does not result in long term stabilization of a waste placed in the
ground.
The chemistry of a laboratory extraction can be very different from the chemistry of a waste
placed in the environment. Wastes which are treated to pass the TCLP test, but are not
permanently stabilized, are a threat to the environment.

575
 Environmental analysis of illicit drug laboratory wastes
John Fowler

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

Environmental hazards involved with methamphetamine (meth) production have brought the
U.S. Environmental Protection Agency (USEPA) into working relationships with local law
enforcement, prosecutors, and the Drug Enforcement Administration. Chemicals used in meth
production are hazardous and small producers routinely dump the chemical wastes and materials
contaminated with hazardous chemicals into streams, rivers, fields, and sewage systems, or the
hazardous material is left abandoned on-site as the suspects flee law enforcement.
The USEPA regulations established in the Resource Conservation and Recovery Act (RCRA)
provide the force to prosecute lab operators creating a situation harmful to human health and the
environment. RCRA hazardous wastes are tested for one or more of four “characteristics”:
ignitability, corrosivity, toxicity, and reactivity. This poster will detail chemicals involved in
methamphetamine production, the test methods used to determine the hazardous characteristics,
and include photos of some of the apparatus used in testing meth laboratory wastes.

576
 Electronic data analysis and laboratory fraud
Johnny Lee, Linda Johnson, and David Holzwarth

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

Environmental data integrity is a growing environmental concern for the USEPA. The accuracy
and truthfulness of environmental data is a cornerstone for environmental enforcement and
compliance, and is essential to the protection of public health and the environment.
The National Enforcement Investigations Center (NEIC) has developed an innovative approach
in investigations by merging electronic data analysis (EDA) techniques, also known as computer
forensics, with analytical chemistry and environmental science and engineering.
The NEIC capabilities in laboratory fraud investigations are enhanced by the unique combination
of EDA seizure and recovery, a modern state-of-the-art analytical laboratory, and multi-media
field inspections.
The EDA team works closely with experienced chemists, environmental scientists, and engineers
to trace the origins of data fraud. This multidisciplinary approach has been recently been applied
across the country on criminal and civil data integrity investigations involving:
● reformulated fuel
● environmental analytical laboratories
● automated waste water treatment plants
The EDA fraud poster will illustrate the unique niche being filled by the NEIC and the impact on
data integrity and laboratory fraud.

577
 Nuclear Magnetic Resonance (NMR) spectrometry in environmental applications
Jon Beihoffer and Jimmy Seidel, Ph.D.

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

Nuclear magnetic resonance (NMR) spectroscopy is a powerful analytical technique which can
be used to determine chemical structures and provide information on the amount of a given
chemical present in environmental samples.
Like its close cousin, the magnetic resonance imaging (MRI) scanner found in hospitals, NMR
relies upon the use of a powerful electromagnet. A NMR spectrum is unique, like a fingerprint,
and can be used to identify constituents present in a sample. Each signal in the resulting NMR
spectrum is proportional to the concentration of the atoms in a sample, and as such, can be used
to determine the amount of each constituent present in a sample.
The NEIC has used NMR as an analytical technique in environmental enforcement cases to
provide complimentary data to supplement traditional analytical techniques used for
environmental samples. At times, NMR has been a key technique for resolving analytical issues
in environmental enforcement cases.
Three recent uses of the NMR spectrometer for environmental enforcement cases will be
presented.
The identification of alcohols and glycols in environmental and process samples from an
antifreeze recycling facility.
The identification and measurement of low levels (<2%) of impurities in pesticide formulations.
The identification and measurement of a cobalt complex in waste samples from a facility that
manufactures automobile air bag inflators.

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 White river fish kill
Laurence Strattan, Ph.D.

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

Personnel at the National Enforcement Investigations Center (NEIC) in Denver, Colorado used a
variety of scientific tools to assist the environmental enforcement action and investigation of a
facility which had caused a large fish kill on the White River upstream of Indianapolis, Indiana.
The White River is the source of about 60% of the drinking water for the city of Indianapolis.
The cause of the fish kill was sodium dimethyldithiocarbamate, a short-lived, but toxic, chemical
used in water treatment at an electroplating facility.
Scientists and engineers from NEIC provided authoritative scientific advice to the enforcement
case on short notice:
Interpreted scientific and technical information available at the time in order to properly plan the
enforcement activities.
Provided knowledge of the environmental behavior of the toxic compound in order to select the
samples for analysis that would the best evidence of what happened in the river.
Performed analyses on the critical sample proving that the compound was present in a discharge
from the facility and the compound was present in concentrations capable of causing the
observed harm to the environment.
The most important analyses were performed by liquid chromatography/tandem mass
spectrometry and by nuclear magnetic resonance (NMR) spectroscopy. This poster will illustrate
the science and technology used to assist with this investigation as well as the scope of this
significant environment enforcement case.

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 The Davold investigation – Illegal asbestos removal and disposal
Peggy Forney, Susan S. Helbert, Joyce Kopatich, and Richard Martinez

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

Asbestos is the name for a group of natural fibrous silicate materials. The three most common
types of asbestos are chrysotile, amosite, and crocidolite; of these three, it is estimated that
chrysotile makes up more than 90% of the asbestos in buildings in the United States. Asbestos-
containing materials (ACM) have been used in products that require the thermal insulation,
chemical and thermal stability, and high tensile strength provided by asbestos fibers.
Generally, if ACM are intact and undisturbed, the asbestos does not pose any health problem.
Problems can occur if these materials are damaged in such a way as to expose the microscopic
asbestos fibers to the air. If distributed through the air, asbestos fibers may be inhaled into the
lungs and the greater the exposure to the fibers (time and quantity), the greater the risk of
developing an asbestos-related disease (asbestosis, mesothelioma, or lung cancer).
The Clean Air Act is the United States federal law that regulates air emissions and tasks the US
Environmental Protection Agency with developing and enforcing regulations to protect the
public from exposure to hazardous airborne contaminants. Asbestos was one of the first
hazardous air pollutants to be listed and regulated under the National Emissions Standards for
Hazardous Air Pollutants (NESHAP).
Because of the potential health hazards involved with damaging asbestos-containing materials
and the frequent need for renovation or demolition of older, asbestos-containing buildings, the
Asbestos NESHAP regulation was developed. Within this regulation are the specific work
practices required by law for minimizing the release of asbestos fibers during the during
demolition and renovation activities. Included in these work practices are requirements to wet
the ACM (preventing airborne distribution of the fibers) and to provide asbestos-removal
(remediation) training and personal protective equipment to employees involved in the activities.
This poster will provide step-by-step details of an investigation where the NESHAP regulations
were not followed. This investigation required the combined efforts of criminal investigators,
field personnel, and qualified asbestos microscopists. Photos will detail the interior of the
building undergoing the asbestos removal and obvious contamination by the fibrous material.
Additional photos will show the excavation by field personnel in an area where the suspects
illegally dumped bags of ACM. Specifics of the investigation and prosecution will be covered
including the sentencing results for the defendants.

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 Use of the HAPSITE field-portable GC/MS for on-site analysis
Stephanie Volz

U.S. Environmental Protection Agency – National Enforcement Investigations Center

P.O. BOX 25227, Denver Federal Center Denver, Colorado 80225 (USA)

The INFINICON HAPSITE Chemical Identification System is a field-portable, temperature

programmable gas chromatograph equipped with a mass spectrometer (GC/MS). This innovative
new instrument allows for rapid analysis of air, water, and soil samples on-site. The system has a
microtrap concentrator for low parts-per-billion (ppb) detection limits, runs on a rechargeable
battery pack, and can be easily adapted for headspace and purge-and-trap analysis.
The National Enforcement Investigation Center (NEIC) has utilized the HAPSITE in the field for
the analysis of reactive gases that are too reactive to ship, for sample screening, and for facility
leak detection.
Samples screened in the field can improve on-site decision-making by the investigative team.
Screening data can be used to determine if further analysis of a particular sample is warranted. It
can also assist in determining if additional samples must be taken in order to support the
environmental crime case. If the area suspected for pollutant contamination is large, sample
screening may prove useful in “mapping” clean sections and sections of the site that actually
contain the hazardous material. Decisions made in the field regarding samples can dramatically
improve the support to an investigation or inspection without requiring additional site visits or
excessive sampling for full laboratory analysis—a savings of time and money.
Analysis results from the HAPSITE are comparable to laboratory analysis of collocated samples.
The USEPA Environmental Technology Verification program approved the HAPSITE for use
with USEPA methods after comparing data generated by the HAPSITE to that generated by a
reference laboratory.
Examples of the use of the HAPSITE by NEIC personnel for environmental investigations will
be presented in this poster. Photos, logistical information, and a comparison of HAPSITE and
NEIC laboratory data for collocated samples will be included.

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 COMPUTER CRIME

An algorithm of digital evidence search process

Kadir OZKAN

Organization: Crime Laboratory of Police in Istanbul, TURKEY

Kriminal Polis Laboratuvarõ, Vatan Cd. A Blok Kat:7 Fatih, ISTANBUL
Telephone: + 90 212 636 17 77, + 90 505 213 23 19 Fax: + 90 212 636 23 97,
kadir.ozkan@kpl.gov.tr , ykadir_ozkan@hotmail.com

“Crime”, as a general concept, is changing its style, host, target etc. every moment. It is a living
mechanism of its very culture and is affected by other mechanisms of the culture it exists in.
Because of that, digital culture of global world brought a new kind of crime to our lives: “digital
crime” with the other face of the medal, investigating techniques of such crimes.
A 40 GB harddisk, if full of text files, can include “42.949.672.960 letters” and it makes
approximately “10 billions words”. It is not easy to comprehend this number but a man with a
reading speed of 10 words\second can read this amount in “1 billion seconds”. 1 Billion seconds
make 32 years. That’s why; one can read a 40 GB harddisk in 32 years without a breath or sleep
however digital crime investigators must conduct searches on harddisks, CDs etc. to reach digital
evidences.
Noticing the difficulties of such search processes, IACIS (International Association for
Computer Information Systems - www.iacis.org) announced a document saying: “In many
instances a complete examination of all of the data on media may not be authorized, possible,
necessary or conducted for various reasons. In these instances, the examiner should not conduct
a complete search and document the reasons for not conducting”.
Because of mentioning a crucial problem, this document is an important one however is not
offering a solution for the problem although such a solution is needed much.
Digital crime investigation procedure can be itemized mainly into three: 1- Seizure and
preservation of data which may contain evidence, 2- Finding the “valuable data” among many
from storage devices etc., 3- Making “evidence-criminal connections” and reporting discoveries
before the court of law.
Among them the second item is becoming more and more difficult every day and requiring a
good solution because the problem is lacking even a rough, worldwide standard. A general
algorithm may enable investigators to document local, detailed documents and conduct more
effective search.
For that reason a “detail levels list of digital crime investigation” should be documented first and
delivered to all police departments. Police departments, when a crime is committed involving
digital machines, should decide the importance of digital evidence among other evidences
(fingerprint, handwriting, DNA, retina etc.) and using this list, they should mark the case with a
number indicating the level of importance.
If the police needs digital evidence -in storage devices- much, a complete search process must be
conducted but if it is relatively unimportant for the police, list of detail levels will not make the
search process -in digital crime laboratory- a waste of time.
At important cases, police officers from involving department should assist digital crime
investigators because it is difficult for a digital crime investigator to update himself with a new
codes of law, new kinds of crime, diverse “modus operandi” etc. and involvement of police to
this search process do not harm the reliability of evidence because the consistency of the digital
evidences is provable.

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Moreover, digital crime can be ended whenever enough evidence is found and this information
must be used to minimize the time that is used to find the digital evidence. For example, the
search process should begin with storage devices which use faster ports, which are of newer
technology, bigger capacity and stop with storage devices that use slower ports, that are of older
technology and smaller capacity.
Shoving this information and the some more details of it will be easier and better if transferred to
an algorithm and presented visually.

583
 Critical issues in computer forensics
Krishnia S PENDYALA*, Dr.M.S RAO**

*Assistant government examiner, computer forensic division, %GEPD, Ramanthpur,

hyderabad, India -500013
** Director & chief forensic scientist, Directorate of Forensic Science, Ministry of
Homeaffairs New Delhi (India)

THE IT- REVOLUTION SWEEPING THE GLOBE in communications and information

technology has truly made the world a smaller village. In this ever-evolving age of information
technology, the requirements of law enforcement are shifting, as well. Some conventional
crimes, continue to become ever more technologically sophisticated. Paper trails have given way
to electronic trails. Digital evidence replaced the physical evidence. Computer forensics is a
new and fast growing field that involves carefully collecting and examining digital evidence to
prosecute a criminal. The four steps in any computer forensic investigation are acquiring,
authenticating, analysis of digital evidence and documentation. Acquiring the data mainly
involves creating a bit-by-bit copy of the hard drive. Authentication is to ensure that the copy
used to perform the investigation/analysis is an exact replica of the original and contents of the
original hard drive has not been altered during the acquisition process. Analysis of the data is the
most important part of the investigation since this is where incriminating evidence may be found.
In this paper the authors discussed about the various critical issues involved in computer
forensics like choosing a right tool for right job; operating system independent imaging tool;
source and destination media for imaging; hashing the drive; loss-less compression of imaging;
rapid increase in storage media capacity; different types of storage media; analysis of application
software’s; cryptoanalysis; steganoanalysis; password cracking; key word search; vernacular
language problems etc and how data mining, neural network, fuzzy logic can help in the forensic
analysis of the suspected computer system.

* Author to whom all correspondence should be made. :

584
 INTERPRETATION

Bayesian networks and the assessment of scientific evidence: the use of qualitative
probabilistic networks and sensitivity analyses.

A. Biedermann1,2,*, F. Taroni1,3,†

The University of Lausanne, School of Criminal Sciences, Institut de Police Scientifique,

Bâtiment de Chimie, 1015 Lausanne-Dorigny, Switzerland
Federal Department of Justice and Police, Federal Office of Police, Nussbaumstrasse 29,
3003 Berne, Switzerland
Institut de Médicine Légale, The University of Lausanne, 21, rue du Bugnon, 1005
Lausanne, Switzerland
*
alex.biedermann@fedpol.admin.ch; alex.biedermann@esc.unil.ch
†
franco.taroni@esc.unil.ch; franco.taroni@inst.hospvd.ch

Bayesian networks (BNs) are models that formally combine elements of graph and probability
theory. BNs are a mathematically and statistically rigorous technique allowing their user to
define a pictorial representation of assumed dependencies and influences among a set of
variables deemed to be relevant for a particular inferential problem. Moreover, newly acquired
evidence can be processed in a way that complies with the rules of probability calculus.
However, only few forensic scientists currently seem to accept BNs as a general framework for
representing and evaluating sources of uncertainties associated with scientific evidence. Notably,
BNs are widely thought of as an essentially numerical method, requiring “exact” numbers with a
high “accuracy”.
The aim of the document is to show that the availability of hard numerical data is not a necessary
requirement for using BNs in forensic science. An abstraction of quantitative BNs, known as
Qualitative probabilistic networks (QPNs), and sensitivity analyses are thus presented and their
potential applications discussed. As a main difference to their quantitative counterpart, i.e. BNs,
QPNs contain qualitative probabilistic relationships instead of numerical relations. Sensitivity
analyses consist of, for example, varying the assessment of one variable and studying the effect
on the model’s outcome.
Both QPNs and sensitivity analyses can be useful concepts that permit forensic scientists to work
in contexts with acute lack of numerical data and where reasoning in agreement with the laws of
probability should nevertheless be performed.

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