F
however, perishable organic implements and food that
FIELD GEOCHEMISTRY
Richard E. Terry
Plant and Wildlife Sciences Department, Brigham Young
University, Provo, UT, USA
Definition
Geochemical analysis: The chemical analysis of elements
associated with soils, rocks, and minerals.
Ethnoarchaeology: The application of archaeological
techniques to elucidate contemporary human activities.
Chelate: Complex organic molecules that surround
metallic ions to hold them in solution and prevent their
chemical precipitation.
Introduction
Examinations of the physical and chemical properties of
soils produce data that augment archaeological informa-
tion on the structures and artifacts left behind by ancient
peoples. In fact, the soil is a palimpsest of the physical
changes and chemical residues associated with both
ancient and contemporary human activities on the land
surface. The origin of the term palimpsest dates to classi-
cal times, but it commonly refers to medieval manuscripts
on parchment that were reused, because the medium was
valuable and more durable than papyrus or paper. The
old ink was partially effaced to clear the sheet for new
writing, and in most cases, vestiges of the previous text,
though faded and indistinct, could still be discerned. This
aptly describes the soil medium as a cumulative recorder
of human activities from ancient to contemporary times
(Bailey, 2007; Dore and López Varela, 2010). Soils can
store pollen, phytoliths, bones, architectural components,
and nonperishable artifacts over sequential occupations;
A.S. Gilbert (ed.), Encyclopedia of Geoarchaeology, DOI 10.1007/978-1-4020-4409-0,
© Springer Science+Business Media Dordrecht 2017
are readily decomposed and seldom survive to become
part of the artifactual record may have initially accounted
for as much as 90 % of an ancient household’s artifact
inventory (Cavanagh et al., 1988; Dahlin et al., 2007).
Such organic materials associated with food preparation
and consumption can lose their carbon and nitrogen com-
ponents, which decompose to gaseous and soluble sub-
stances, yet phosphorus (P) and certain trace nutrients –
including iron (Fe), copper (Cu), manganese (Mn), and
zinc (Zn) – are adsorbed onto soil particles or are precipi-
tated as insoluble compounds and remain for centuries at
the location of ancient use. These and other geochemical
residues of human activities serve as invisible artifacts.
Nonperishable artifacts associated with abandoned hab-
itations and public structures were often picked up and
moved and then reused at distant locations. In most cases,
the soils and earthen floors of former landscapes are not
transported, and thus the geochemical residues within soils
provide excellent in situ evidence of ancient use (Barba
et al., 1996; Wells et al., 2000; Parnell et al., 2001; Parnell
et al., 2002; Barba, 2007). Geochemical analyses of soils
and floors have become established archaeological
methods for locating ancient sites. The results further
define the types and extent of human activities within those
sites and help in the interpretation of those activities (see
reviews by Wilson et al., 2005; Wilson et al., 2006;
Holliday and Gartner, 2007; Walkington, 2010).
Anthropogenic chemical residues in soils
Phosphorus (P)
The application of phosphate analysis in archaeology was
first developed in Europe in the 1930s, where pioneering
efforts by Arrhenius (1931) and Lorch (1940) indicated
that areas of ancient occupation contained elevated
264 FIELD GEOCHEMISTRY
concentrations of soil P. Ethnographic studies likewise
illustrated the relationship of P concentration with domes-
tic activities (Barba and Ortiz, 1992; Middleton and Price,
1996; Fernández et al., 2002; Terry et al., 2004). Phospho-
rus is used by plant and animal cells in plasma membranes,
nucleic acids, and other organic molecules. When ancient
plant and animal foodstuffs were harvested and brought
into dwelling places, the P contained in the food was also
introduced into the settlement. As the food waste
decomposed, the mineralized P was readily fixed onto
the surface of soil particles and remained stable for long
periods of time (Barba and Ortiz, 1992; Holliday and
Gartner, 2007). Activities such as preparation, storage,
and disposal of food as well as the fertilizing of soil for
agriculture have left distinct chemical residues that remain
relatively in their original place within the soil for
centuries.
Soil samples collected prior to excavation can be ana-
lyzed and their chemical patterns determined and mapped,
in order to prospect for archaeological features of interest.
For instance, Parnell et al. (2001) reported a significant
positive correlation between sherd density discovered
within test pits and surface soil P concentrations. An area
that contains elevated soil P near architectural structures
may indicate locations of residential middens.
Floors with elevated P concentrations may indicate
kitchen and food consumption areas. Ethnoarchaeological
studies of indigenous households have demonstrated that
activities associated with high soil P concentrations
include gardening, food preparation, waste disposal, and
sweeping that pushes organic material to the peripheries
of patios and high-traffic areas (Barba and Ortiz, 1992;
Fernández et al., 2002). Combined with other lines of evi-
dence, geochemical data have helped identify areas used
as sleeping quarters and spaces in which ritual and funer-
ary activities were conducted (Barba et al., 1995; de
Pierrebourg, 1999). Thus, extraordinarily high
P concentrations in soils and on floors can be associated
with prehistoric food preparation, consumption, storage,
and disposal. Very low levels of P could indicate high-
traffic areas such as pathways and patio centers, as move-
ment and sweeping push organic debris to the outer
margins.
Several methods of P extraction have been used in geo-
chemical studies of ancient activity areas. Dilute acid
extraction procedures remove a portion of the
P adsorbed onto the surfaces of soil particles (e.g.,
Mehlich, 1978; Middleton and Price, 1996; Terry et al.,
2000; Rypkema et al., 2007). The concentrations of
extracted P vary with the type and strength of the acid.
In each extraction procedure, the portion of P analyzed is
affected by soil acidity or alkalinity, percentage of organic
matter, clay content and mineralogy, and other physical
and chemical properties of the soil. For these reasons,
the magnitude of extracted P concentration differs with
the extraction procedure, with the type of soil, and with
the geographic origin of the soil.
Trace elements
Anthropogenic metal and trace element residues have
proven useful in the identification of ancient activities.
Much of this work has focused on Cu, Fe, Mn, lead (Pb),
and Zn (Bintliff et al., 1990; Entwistle and Abrahams,
1997; Entwistle et al., 1998; Entwistle et al., 2000; Parnell
et al., 2002; Terry et al., 2004). Many of the metallic ions
remain stable in soils for long periods, as their ions are
readily adsorbed and precipitated onto clay surfaces, and
they can form insoluble oxides, sulfates, or carbonates
(Lindsay, 1979; Wells et al., 2000). Some pigments and
paints used by the pre-Hispanic Maya contained metallic
bases, such as hematite and cinnabar (Goffer, 1980;
Vázquez Negrete and Velázquez, 1996a; Vázquez Negrete
and Velázquez, 1996b), and thus, elevated values of trace
metals in soils may help to identify areas where pigments
were processed or applied and where craft workshops
were located (Terry et al., 2004). For example, evidence
of workshop activities was provided by trace metal extrac-
tion and inductively coupled plasma mass spectrometry
(ICP/MS) or atomic emission spectroscopy (ICP-AES)
analyses of soil and floor samples at Cancuén (Cook
et al., 2006), Piedras Negras, and Aguateca, Guatemala
(Parnell et al., 2002; Terry et al., 2004). Multivariate anal-
ysis of P and several trace metals has also proven useful
(Parnell et al., 2002; Abrahams et al., 2010; López Varela
and Dore, 2010).
Geochemical analysis in the field
Two problems arise when samples must be delivered from
the field to a distant formal laboratory setting with the
attendant lengthy wait for chemical analysis and data
processing. First, the process of moving samples from
field to laboratory and the analytical time required at
a busy soil laboratory mean that geochemical data are usu-
ally not available before the end of the field season.
Second, the permitting process for carrying soil samples
across international borders is time-consuming and often
both difficult and expensive. For these reasons, archaeo-
logical prospection benefits greatly from more rapidly
obtained results from analyses conducted in situ and in
a field laboratory. As geochemical techniques in archaeo-
logical research have developed and as analytical capabil-
ities have advanced, the demand has grown for relatively
quick data obtained at the time of excavation or at least
in a field laboratory so that within minutes or a couple of
days, results can be available to guide archaeological
investigations and to target features of interest.
Simple spot tests for soil P, amino acids, and lipids have
been developed (Eidt, 1973; Barba et al., 1991) for in situ
use. In the field laboratory, extractable P tests can be
conducted with relatively inexpensive equipment and
chemicals. Both Terry et al. (2000) and Rypkema
et al. (2007) have described such tests and equipment.
Much of the equipment needed for geochemical analysis
of archaeological soils in a field laboratory is available
 FIELD GEOCHEMISTRY 265

Field Geochemistry, Figure 1 A triangular grid was superimposed on the Conchita Plaza group near Caracol, Belize. Each grid point
was 10 m from adjacent grid points. North-south pathways through the dense vegetation were cut 8.67 m apart to allow
equidistance sampling at 10 m.

in battery-powered form, including electronic balances,
timers, pH meters, and colorimeters. Deionization car-
tridges can be linked by flexible tubing in the field lab to
provide laboratory-quality water for chemical analyses.
Limitations inherent in a field laboratory setting likely
preclude the use of concentrated acids for sample diges-
tion in preparation for total elemental analysis. There are
the safety issues of toxic fumes and the necessity of safety
showers, eyewashes, and climate control that are cost pro-
hibitive in a field laboratory situation. In addition, the
inductively coupled plasma (ICP) spectrometer and the
atomic adsorption (AA) spectrophotometer necessary for
total element analysis are not available in a format that
would allow field laboratory use. However, recent
advances in the development of battery-operated, portable
X-ray fluorescence (pXRF) instruments may allow
researchers to obtain reliable total elemental analysis both
in situ and in the field laboratory.
Soil sampling
The key to excellent soil geochemical data is representa-
tive and statistically sound sampling. Only a few crumbs
or a couple of grams of soil end up in an extraction vessel
or an analysis vial. Those tiny amounts of soil must
therefore adequately represent the specific area of sam-
pling. Samples may be taken on a gridded system for
geospatial analysis of an area, or they may be taken at
intervals along a transect in search of “hot spots” for later
study. In many cases, the ancient occupation surface is at
the contemporary soil surface. Leaf litter should be
removed and approximately 500 g of soil collected. It is
recommended that this sample be obtained from three or
four spots within 0.5 m of a grid point or transect location.
The sample contains moisture, roots, and gravel that should
be removed during sample preparation. It is important to
collect sufficient sample for all of the planned analyses,
along with sufficient sample to allow procedures to be
repeated if necessary. In some cases, excavated occupation
surfaces are exposed and lend themselves well to sampling.
The archaeologist’s grid can help in the sampling. If there
are no excavation markers, a permanent reference point
with east-west and north-south lines can establish a grid.
Geospatial analysis is most effectively conducted if the
distance between adjacent samples is the same, and this
can be facilitated with an isosceles triangular grid
(Figure 1).
The type of sampling bag to be used should be carefully
considered. In either the field lab or the formal laboratory
266 FIELD GEOCHEMISTRY
setting, the analyst is going to remove either the full con-
tents or only part of the material repeatedly. We have
found heavy (0.064 mm thick) plastic bags to work best
if they must be opened and closed several times. Sandwich
bags or light-duty plastic bags tend to leak, they do not
stand up, they do not facilitate vigorous mixing, and they
generally do not survive a bank of soil preparation and
analysis procedures.
Soil sample preparation
For geochemical concentration data to be accurate, soil
samples need to be air-dried, crushed, and sieved to
remove rocks, roots, and non-soil debris. Soil samples
should be corrected for air-dry moisture content, which
can be done by weighing the sample and oven-drying it
at approximately 105
C to constant weight (generally
12–24 h depending on size of the sample). The field lab
is unlikely to have access to a drying oven; therefore, upon
return to the formal laboratory, the air-dry and oven-dry
weights should be determined so that moisture correction
factors can then be applied.
In a field lab, a few mortars and pestles can facilitate
crushing of dry soil aggregates, using care so as not to
crush stones and non-soil debris greater than 2 mm in
diameter. A 2-mm (#10-mesh) sieve is used to remove this
debris. No further grinding or sieving should be required
for field lab analyses. In our laboratory, samples are
air-dried for a couple of days on clean sheets of office
paper. Samples are either crushed and sieved at this time
or returned to the original bag to await further processing.
Field laboratory measurements
In all tests for soil P, care must be taken to avoid contam-
ination by hands, rubber stoppers, or detergents that might
contain phosphate. Phosphate-free detergent is used to
clean all glass and plasticware. In some cases, it may be
necessary to rinse laboratory ware with 1 M HCl to elim-
inate P contamination.
Spot tests
The spot test for field P analysis was described by Eidt
(1973). Briefly, the procedure calls for about 50 mg of
fresh or prepared soil to be placed in the center of a filter-
paper disk. Two drops of reagent A are added without
touching the soil with the dropper tip (Eidt, 1973). After
30 s, two drops of reagent B are added. A blue color
may appear after 2 min, and readings should be taken
before 8 min pass. Visual ratings of the lengths and inten-
sities of blue lines and rings are judged to give P ratings of
none, weak, regular, good, or strong. The phosphorus spot
test is simple and inexpensive, but the results are not quan-
titative. Values are affected by sample size, color percep-
tion of the analyst, and temperature, as well as other
environmental conditions in the field or the laboratory.
In addition, the dynamic range of P concentrations deter-
mined by the spot test is limited (Terry et al., 2000).
Mehlich III extractable phosphate procedure
Rypkema et al. (2007) adapted a Mehlich III (solution of
acetic acid, ammonium nitrate, nitric acid, and ammonium
fluoride) extraction method, for infield P prospection.
They used a 5-min extraction time and employed syringe
filtration with a glass fiber filter. They describe a two-part
color development process that mixes 3 ml of extractant
with 0.3 ml of a solution of ammonium molybdate and sul-
furic acid and 0.3 ml of a solution of malachite green and
polyvinyl acid. They reported that both reagent solutions
were stable over time and temperature ranges, making
them robust field materials. The extractant-reagent mix-
ture develops color from a light yellow-green to a dark
green with increasing P levels. Concentrations of P are
determined by a battery-operated colorimeter at
a wavelength of 620 nm.
Mehlich II extractable phosphate procedure
Terry et al. (2000) adapted a Mehlich II extraction proce-
dure (Mehlich, 1978) for use in a field laboratory for
P prospection at the ancient Maya site of Piedras Negras.
Ready-mixed Hach reagents (Loveland, CO) were conve-
nient for field laboratory extraction and molybdate-
phosphate color development. Phosphorus concentrations
were determined with the use of a battery-operated color-
imeter. A field laboratory setup is shown in Figure 2.
The following method was used: Two grams of
air-dried, sieved (<2-mm) soil sample were placed in
one of six 50-ml glass vials attached to a board that facil-
itated shaking and processing of multiple samples. Once
each soil sample was extracted with 20 ml of diluted
Mehlich II solution for 5 min, the extractant was filtered
and the filtrate collected in clean 50-ml vials. One millili-
ter of the extract was dispensed to a reaction vial and
diluted to 10 ml with deionized water, and the contents
of the PhosVer 3 powder pack were added to the vial.
The sample was shaken by hand for exactly 1 min, and
allowed to stand an additional 4 min for color develop-
ment. The concentration of P in the samples was deter-
mined on a Hach DR 850 colorimeter at a wavelength of
610 nm.
Precautions should be taken with P extraction and anal-
ysis in the field lab:
1. Both the P extraction and the phosphate-molybdate and
reductant reactions are temperature dependent. We
found that once the temperature of the laboratory and
the extractant solution exceeded 35
C, the blue molyb-
date color appeared even with no phosphate in solu-
tion. To resolve this problem in a hot climate region,
one should perform the analysis only in an
air-conditioned space or in the cool of the morning.
In the jungles of Guatemala, we finished our analysis
before about 11 AM, as, afterward, the temperatures
rose above 35
C.
2. Another source of error to be avoided is the auto-
reaction of the PhosVer 3 crystals. If the crystals are
allowed to settle to the bottom of the reaction vial and
 FIELD GEOCHEMISTRY
Field Geochemistry, Figure 2 The field laboratory set up near Tikal, Guatemala, for Olsen bicarbonate extraction and analysis of
soil P.
to remain in proximity to each other, they will auto-
react. The blue color will develop even if P is absent
from the solution. The way to avoid this potential prob-
lem is to dissolve the reagents immediately. The con-
tents of the PhosVer 3 packet can be added to one
sample at a time and shaken for 60 s.
The colorimeter reports the percent transmittance of
specific wavelengths of light. These transmittance values
are then converted to ppm in the reaction solution
according to a standard curve. The Mehlich II concentrate
solution that is available from Hach Co. contains hazard-
ous acids and thus is prohibited from transport within air-
line baggage. The reagent can be purchased in foreign
countries from Hach distributers, but our experience has
been that it takes about 1 year of difficult negotiations
before the reagent is imported. As an alternative for use
in calcareous soils and lime-stucco floors common to most
ancient Maya sites, the Olsen bicarbonate (Olsen and
Sommers, 1982) extraction can be successfully used in
the place of the Mehlich II extraction.
Olsen bicarbonate extraction
The Olsen procedure was developed for determination of
plant available P in neutral to alkaline soils that contain
calcium carbonate. The P concentrations extracted by
sodium bicarbonate from the soil tend to be lower than
with the dilute acid Mehlich extractant, but the results in
low P concentration samples compared to samples anthro-
pogenically enriched in P are relative. The advantage of
the bicarbonate extraction is that the reagent can be pur-
chased at local markets and pharmacies. The concentra-
tion of sodium bicarbonate is 0.5 M and the extraction
time with shaking is increased to 20 min. The samples
are filtered and dispensed, and color is developed as
267
indicated above. The PhosVer 3 reagents are acidic and
will cause effervescence. It is a good idea to relieve pres-
sure occasionally by cracking open the lid of the colorim-
eter vial and closing again for continued shaking.
Terry et al. (2000) subjected 35 soils of household mid-
dens, patios, and pathways from Piedras Negras, Guate-
mala, to the Eidt spot test, the Mehlich II extraction, the
Olsen bicarbonate extraction, and the nitric/perchloric
acid total P digestion procedures. While all four proce-
dures identified high soil P levels in household middens
and low P concentrations in patio and pathway soils, the
Mehlich II dilute acid and the Olsen bicarbonate extrac-
tion procedures provided the greatest ratios of midden
P concentrations to background P concentrations of 6.7
and 10.6, respectively (Table 1). The midden-background
concentration ratios obtained by total digestion and the
spot tests were 2.2 and 2.5, respectively.
Trace element analysis of soils
Elevated trace metal concentrations of Fe, Mn, and Cu
could be indicative of mineral paints and pigments used
in ancient times. Zinc is not a primary mineral pigment
but may be present as a contaminant of mineral ores.
A more likely source of Zn is the vegetable matter used
in households. While Fe, Mn, and Cu are also trace con-
stituents of foodstuffs, these minerals were also specifi-
cally collected and used in workshop activities.
Chelates are complex organic molecules that surround
and hold in solution metallic ions that would otherwise
quickly precipitate. The diethylenetriaminepentaacetic
acid (DTPA) chelate extraction method (Lindsay and
Norvell, 1978) can be used to solubilize surface adsorbed
and slightly soluble trace metals that may be plant avail-
able. This method is often used in determining heavy
268 FIELD GEOCHEMISTRY
Field Geochemistry, Table 1 Summary comparison of soil
P concentrations from 35 samples determined by four different
extraction and total digestion procedures. The samples were
obtained from groups O and N at Piedras Negras, Guatemala
(Terry et al., 2000)
Mehlich P Olsen P Total P Spot test
Rating
mg/kg mg/kg mg/kg 1–5
Maximum 125 65 2,949 5 X-ray fluorescence spectrometer contained in the device.
Minimum 17 5 1,042 2
Mean 33 19 1,854 4
STDEV 19 12 395 1 cific for each element (Bernick et al., 1995; Kalnicky
Background 19 6 1,132 2 and Singhvi, 2001; Jang, 2010), and the amount of radia-
Midden sample N6–7 125 65 2,476 5 tion released is related to the concentration of an element
Midden: background 6.7 10.6 2.2 2.5
ratio
The “background” levels of P were determined by averaging 10 %
of the samples lowest in concentration. The midden-background
ratio was determined by dividing the P concentration of the soil at
a known kitchen midden by the background concentration deter-
mined by each P analysis method
Spot test rating: 1 ¼ no blue color development; 5 ¼ a continuous
ring of strong blue color development
metal contamination of environmental samples, and it is
useful in characterizing the metal ions associated with
human activities such as food use and mineral use in work-
shop activities. Unfortunately, the method does not lend
itself well to the field laboratory, but if samples are
returned to a formal laboratory possessing the necessary
equipment, the procedure could be used. The concentra-
tions of Cu, Fe, Mn, Pb, strontium (Sr), Zn, and other ele-
ments of interest can be determined simultaneously on the
inductively coupled plasma atomic emission spectrometer
(ICP-AES).
Portable X-ray fluorescence
The cutting-edge technology of portable X-ray fluores-
cence (pXRF) could be used to facilitate soil chemical
analysis of total mineral elements in a field laboratory
(Koester et al., 2003; Hou et al., 2004; Melquiades and
Appoloni, 2004; Marwick, 2005; Jozic et al., 2009;
Donais et al., 2010; Donais et al., 2011; Coronel
et al. 2014). The pXRF instrument not only makes the
work of elemental analysis possible in situ or in a field lab-
oratory (Bernick et al., 1995; Radu and Diamond, 2009),
but the analysis can be performed more economically
and much faster than sending samples to an ICP laboratory
facility for analysis. The pXRF is a battery-operated,
handheld device that determines total elemental content
for elements heavier than calcium. The instrument is about
one-fifth of the cost of an ICP-AES and is fully functional
in a field laboratory. The device is equipped with a probe
window and an X-ray tube that irradiates the sample.
The high-energy X-rays can either scatter or be absorbed
by atoms in the sample and reradiated as X-rays of specific
lower energy in a photoelectric effect. A rearrangement of
electrons happens as a consequence of X-ray irradiation,
which can cause ionization, or the ejection of an electron
from an inner orbital. X-ray fluorescence is the emission
of high-energy photons as an electron from a higher orbital
replaces the one ejected, allowing the atom to return to
normal energy levels. Using this method, concentrations
of specific elements of interest can be measured by an
The determined X-ray energy of the fluorescence is spe-
in the sample (Juvonen et al., 2009).
Unfortunately, the pXRF analysis of soil P is not ade-
quate to differentiate soils with subtle differences in
anthropogenic P within activity areas. The energy emitted
by P is low, and therefore, the error in P analysis by pXRF
is large. In addition, the X-ray energy of P shows up on the
shoulder of the energy peak for silicon (Si), so that the
large Si content of soils increases the error in
P concentration measurement (Coronel, 2011; Coronel
et al., 2014). For this reason, it is recommended that one
of the extractable P analyses be performed in the field
lab. Several scientists are developing protocols for the
use of pXRF in situ and in the field laboratory (e.g., Bernick
et al., 1995; Kalnicky and Singhvi, 2001; Carr et al., 2008;
Jang 2010; Martín Peinado et al., 2010; Coronel, 2011; Zhu
et al., 2011; Davis et al., 2012; Weindorf et al., 2012a;
Weindorf et al., 2012b; Coronel et al., 2014).
For pXRF analysis under ideal laboratory conditions, it
is recommended that dry soil samples be ground to pass a -
100-mesh (<0.149-mm) sieve and that the sample be
contained behind 0.0036-mm plastic film (USEPA,
2007; Jang, 2010). In the field lab, it is more feasible to
air-dry, crush, and sieve soils to 10 mesh (<2 mm) than
to spend the time and labor to grind the samples to
100 mesh. Coronel and colleagues (2014) found no signif-
icant difference in the pXRF analyses of Ti, Fe, Cu, and Zn
in samples crushed to pass either 10-mesh or 100-mesh
sieves. Concentrations of Sr and Zr were attenuated by
approximately 10 % when samples passed only a 10-mesh
sieve. Prepared samples can be poured onto a 0.0036-mm
film atop the pXRF window to a depth of 1–2 cm for an
analysis time of 120 s. Compared to oven-dry samples,
the X-ray signals from air-dry soil (about 96 % solids)
were reduced by approximately 8 %, while elemental con-
centrations in field-moist soils (about 82 % solids) at
approximately 33-kPa (0.33-bar) moisture potential
were attenuated by 11 %.
Further improvements of in situ protocols are needed,
and more robust and less cumbersome pXRF instruments
should be developed. Soil moisture and soil heterogeneity
of in situ samples increase the error rate of pXRF measure-
ments, but these error rates do not preclude the use of
pXRF for qualitative and semiquantitative comparisons.
In situ measurements could prove useful in initial
 FIELD GEOCHEMISTRY
screening of samples or in prospection for archaeological
features. Deposition of workshop minerals, stucco floor
materials, and the leveling of land surfaces by ancient peo-
ple often change the elemental content of surface soils and
of deposition horizons sufficiently that in situ measure-
ments could prove useful. Sample preparation and pXRF
measurement in the field laboratory produce reliable data
for activity area analysis of ancient human activities.
Summary
The high surface area and chemical properties of soil par-
ticles allow the soil medium to preserve a geochemical
record of human activities from ancient times to the pre-
sent. The carbon and nitrogen components of perishable
food and other household and workshop items decompose
and are lost as gaseous and soluble substances, but P and
certain trace nutrients, including Fe, Cu, Mn, and Zn, are
adsorbed onto soil particles or precipitated as insoluble
compounds and can remain for centuries. These geochem-
ical residues serve as invisible artifacts. Soil geochemical
methods are used in archaeology to locate ancient sites
based on geochemical concentrations and help in the inter-
pretation of ancient human activities. Spot tests, chemical
extraction, and sample digestion procedures have been
used to determine areas enriched in phosphate by ancient
activities.
Protocols for portable X-ray fluorescence (pXRF) use
in the field are being developed to facilitate soil chemical
analysis of total mineral elements. In situ pXRF measure-
ments could prove useful in initial screening of samples
and in prospection for archaeological features. Unfortu-
nately, the low-energy X-ray fluorescence from P and
the interference of X-rays from soil Si render high-error
and low-quality data for total soil P concentrations. How-
ever, chemical extraction procedures and battery-operated
balances and colorimeters facilitate the collection of use-
ful, high-quality P data from archaeological soils and
floors in the field laboratory. The combination of appropri-
ate sample preparation, chemical extraction of soil P, and
pXRF measurement of metallic elements in the field labo-
ratory produces reliable data for activity area analysis of
ancient human behavior.
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FIELD SURVEY
John Bintliff
School of Archaeology, Classics and History, Edinburgh
University, Edinburgh, UK
Definition and introduction
Archaeological field survey refers to the systematic study
of the surface traces of past human activity in the land-
scape (see also entry Landscape archaeology). The most
common forms of such evidence are broken pottery and
stone tools, but in protohistoric and historic societies, vis-
ible remains range from fragments of art through house
foundations to standing monuments such as hillforts and
temples.
Field survey
During the fifteenth to nineteenth centuries, landscape
mapping of the more substantial forms of surface remains
was the dominant aspect of archaeology, with excavation
being much rarer and less sophisticated. Even after the
development of scientific forms of excavation by the early
twentieth century, wider research in the total landscape has
remained of equal importance for compiling maps of past
human activity in the countryside. This is due to the early
recognition that the density of archaeological sites is far
greater than the capacity of archaeologists to excavate
them, especially in areas where human society has a long
record of intensive settlement – such as Mesoamerica,
the American Southwest, large parts of the Mediterranean
and Near East, and Japan. Early collaboration with geog-
raphers, especially in the first half of the twentieth century,
led to a lasting interest in settlement patterns, their evolu-
tion over time, and their relationship to the physical char-
acteristics of a region. This also required a spatially wider
271
investigation of human activity foci than targeted excava-
tion or chance discoveries could provide (e.g., Fox, 1923).
The methodology of field survey has continuously
improved in complexity over time, and practitioners are
still in the process of evolving a rigorous and agreed-upon
set of practices. It is typical even today for field survey
projects to continue experimenting each year and for con-
siderable diversity in approaches to occur among projects.
Initially, “topographers” travelled extensively into the
countryside, often with ancient texts in hand when historic
sites were mentioned or with advice from local villagers as
to where “remains” of all kinds were known. Recording
began with ruins and earthworks in the early centuries,
supplemented by coins and sculpture, but by the late nine-
teenth century, the importance of the everyday, and far
more plentiful, human traces such as potsherds and stone
tools was realized, as such finds allowed a far greater
range of sites to be discovered while providing the pri-
mary means – still true today – of dating the periods of
time in the past during which a given findspot was in use.
This new phase of survey history, with its focus on pot-
tery and lithics backed up by the evidence of ruined struc-
tures where preserved, was practiced with what today
would be called “grab samples”: small collections of hope-
fully diagnostic artifacts that would provide chronological
information and some idea of site function for a findspot
(e.g., settlement, burial, temporary activity in the land-
scape such as a hunting stand, or seasonal farming base).
Moreover, the coverage of a region was still “extensive,”
and surveyors ranged over large areas in vehicles or on
foot, gaining a general impression of the kinds of site to
be encountered and the overall balance of activities from
phase to phase. By the 1950s, major programs of regional
survey were set in motion in different parts of the world,
each conceived with a conscious intention to tackle spe-
cific historical problems. What set these projects apart
from most earlier endeavors was their large scale, the
deliberate inclusion of a range of complementary disci-
plines in addition to archaeology, and the “problem orien-
tation” planned within a regional framework. Among the
most noteworthy, during which chosen sites were also
excavated on occasion, were (1) the team led by Robert
Braidwood (Braidwood, 1937; Braidwood et al., 1983)
researching the origins of agriculture in the Fertile Cres-
cent of the Near East, followed by (2) Robert McCormick
Adams’s (1965, 1981) studies of the long-term settlement
development of later prehistoric to historic Southern Mes-
opotamia, (3) the Valley of Tehuacán project of Richard
MacNeish (1967–1972) (also particularly focused on the
development from hunter-gatherers through the earliest
maize farmers to the rise of civilization), (4) the South
Etruria Survey led by John Ward-Perkins (Potter, 1979),
and (5) the Messenia Project directed by William
McDonald and Richard Hope Simpson (McDonald and
Rapp, 1972) (see entry Minnesota Messenia Expedition
(MME)). As these pioneering major projects proceeded,
experiments were conducted with more systematic site-
mapping and artifact collection procedures commensurate
272 FIELD SURVEY
with the quantitative emphasis of the “New Archaeology,”
which in the 1960s–1970s urged that survey be brought
within the model of experimental science (e.g., Redman
and Watson, 1970; Flannery, 1976).
During the 1980s and 1990s, a new generation of
regional projects adopted a more complete, “intensive”
survey procedure, where each field or artificial study
block (sometimes called a transect) in the landscape was
walked at close intervals (5–20 m usually between
fieldwalkers) so that even small artifact concentrations
would be encountered (what this writer dubbed in 1994
the “New Wave” surveys). Visibility measurements were
taken in order to control for differential recognition of sites
due to the variable density of surface vegetation, and geo-
morphologists were increasingly deployed on the team to
identify areas of likely loss or burial of artifacts due to ero-
sion or colluvial-alluvial processes (e.g., Cherry et al.,
1988). In the latter part of this phase, the concept of
“non-site” survey emerged in the United States and was
more generally adopted; it recognized that the landscape
between the activity concentrations termed “sites” often
contained significant numbers of dispersed artifacts. It
became common to refocus surface survey onto the map-
ping of individual artifacts across the landscape, with
a secondary stage being the identification of the patterns
in these total distributions and the variable processes that
might have created them. Besides the effects of weather,
cultivation, or construction activities, which could shift
artifacts out of sites into their immediate surroundings,
more distant scatters could be shown to reflect
“taskscapes” in the countryside: temporary bases for hunt-
ing or farming, mining, etc. An additional category was
given prominence by the Near Eastern regional surveys
of Wilkinson, where intensive agricultural manuring in
certain periods of the past, using undifferentiated domestic
rubbish, had resulted in extensive carpets of artifacts
across the landscape radiating from settlement sites
(Bintliff and Snodgrass, 1988a; Wilkinson, 1989).
Although criticized by some, subsequent exhaustive
investigations leave little doubt that in some landscapes
and usually for restricted periods, massive manuring did
indeed occur, with major implications, as Wilkinson
argued, for detecting population pressure and ecological
sustainability (e.g., Bintliff et al., 2007). Finally, moti-
vated by the pioneer survey of the New World’s largest
pre-Columbian agglomeration, Teotihuacan (Millon,
1964), it proved possible to survey large urban sites in
a relatively short period of one or several seasons (e.g.,
Bintliff and Snodgrass, 1988b; Bintliff, 2014).
As the shift from a non-site approach to regional survey
occurred, awareness was growing that even if conducted
on a field-by-field basis, intensive surveys detected only
a certain sample of past activity in the landscape. The
problem lay in evaluating what was missed and whether
there were ways to compensate for such omissions. One
filter was already noted: the geomorphological constraints
that determined whether surface artifacts and sites could
be seen at the present day (van Leusen et al., 2011).
Advice from project geoarchaeologists could sensitize
surveys to those localities unlikely to provide “windows”
into past landscapes, and these might be omitted from
study or alternatively (but rarely) probed by coring if
remains were expected to be buried. Vegetation cover –
grassland or forest – posed seemingly equal hindrances
to effective surface survey, but coping methods have
included focusing on areas temporarily opened by fire as
well as shovel-pit testing, in which numerous small units
one or a few meters square are stripped to the subsoil to
evaluate buried finds (reviewed by Shott, 1985). On
a more archaeological front, the relative survival and visi-
bility of artifacts themselves have been raised as limiting
factors in site recognition, i.e., the “hidden landscape”
concept (Bintliff et al., 1999), which implies that for some
eras of the past, even a handful of surface finds may repre-
sent a significant former activity focus.
In the heyday of “New Archaeology” in the
1960s–1970s, it appeared attractive to limit overall land-
scape coverage, the area of a located site to be studied,
or the amount of artifacts to be collected, through an
explicit sampling strategy linked to statistical methodolo-
gies, such as stratified sampling in which homogeneous
subareas (strata) would be identified and sampled inde-
pendently (cf. Cherry et al., 1978; Renfrew and Wagstaff,
1982). Warnings about such procedures (already in
Flannery, 1976) have not prevented their continued use,
the central failing being the concept of designing
a reliable sample of a larger whole whose properties are
unknown. More experiments are required where samples
are compared with complete spatial coverage and artifact
samples with total surface collection, before such short-
cuts can be recommended.
Since the late 1990s and early 2000s, a wider process of
rethinking the methodology and interpretative potential of
surface surveys has been in operation as a form of “source
criticism.” Comparative survey analysis, where practi-
tioners review each other’s methods, theories, and inter-
pretations and attempt to amalgamate data from separate
surveys, is one aspect of this reevaluation (cf. Bintliff
et al., 2000; Alcock and Cherry, 2004). Two practical
examples are Farinetti’s integration of site data from all
forms of surface research since the nineteenth century
for the central Greek province of Boeotia (Farinetti,
2011) and Gkiasta’s overview of the history and results
of survey on the island of Crete (Gkiasta, 2008). Another
aspect of rethinking survey approaches is the publication
of surface survey manuals (e.g., Banning, 2002).
Finally, one can mention a number of extra dimensions
to traditional survey which are being increasingly featured
in published projects. Some surveys have deliberately
worked in terrain not considered ideal for surface survey,
such as mountain zones, tropical forests, pastoral low-
lands, or dune environments, where a range of additional
techniques have been necessary to deal with problems of
site detection. Problem periods, or past intervals for which
it has proved difficult to find significant numbers of activ-
ity foci, have led to predictive modeling based on
 FIELD SURVEY
compiled evidence that isolates landscape characteristics
where survey is more likely to recover adequate data
(e.g., Paleolithic-Mesolithic sites in semiarid environ-
ments, Runnels et al., 2005). Scientific aids have become
more frequently used as additional means to study past
settlements, such as a battery of geophysical methods to
map subsurface features, geochemical soil testing to detect
human activity zones, aerial photography, and satellite
imaging (e.g., Philip et al., 2005) (see entries Remote
Sensing in Archaeology; Geophysics; Electrical Resistiv-
ity and Electromagnetism). Geographical information sys-
tems (GIS) have brought two contrasting advantages to
field survey. First, GIS using palmtops and GPS links
can allow accurate and speedy plotting of landscape units
under study in the field as well as recording data in real
time, and second, GIS can assist the recent interest in the
phenomenology of landscape through estimating human
navigation potential and the sensory perception of
a particular terrain. There remains, however,
a considerable lack of experimental evidence on the
effects of using different methodologies on the data pro-
duced through survey, and many key issues are still uncer-
tain. These issues include (1) the desired size and
composition of artifact samples to achieve reliable repre-
sentativeness for an activity focus (Bintliff, 2012),
(2) the best way to reconstruct demographic estimates
from survey data, and (3) whether regional surface survey
can move from generalized pictures of the long and
medium term (thousands to hundreds of years) to detect
the dynamism of human settlement at the historical scale
of decades or even individual years.
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McNeish, R. S. (ed.), 1967–1972. The Prehistory of the Tehuacán
Valley, vols. 1–5. Austin: University of Texas.
Millon, R., 1964. The Teotihuacan Mapping Project. American
Antiquity, 29(3), 345–352.
Philip, G., Abdulkarim, M., Newson, P., Beck, A., Bridgland, D. R.,
Bshesh, M., Shaw, A., Westaway, R., and Wilkinson, K., 2005.
Settlement and landscape development in the Homs region,
Syria. Report on work undertaken during 2001–2003. Levant,
37: 21–41.
Potter, T. W., 1979. The Changing Landscape of South Etruria.
London: Elek.
Redman, C. L., and Watson, P. J., 1970. Systematic, intensive
surface collection. American Antiquity, 35(3), 279–291.
Renfrew, C., and Wagstaff, J. M. (eds.), 1982. An Island Polity. The
Archaeology of Exploitation in Melos. Cambridge: Cambridge
University Press.
Runnels, C., Panagopoulou, E., Murray, P., Tsartsidou, G., Allen, S.,
Mullen, K., and Tourloukis, E., 2005. A Mesolithic landscape in
Greece: testing a site-location model in the Argolid at Kandia.
Journal of Mediterranean Archaeology, 18(2), 259–285.
Shott, M., 1985. Shovel-test sampling as a site discovery technique:
a case study from Michigan. Journal of Field Archaeology,
12(4), 457–468.
Van Leusen, M., Pizziolo, G., and Sarti, L. (eds.), 2011. Hidden
Landscapes of Mediterranean Europe. Cultural and
Methodological Biases in Pre- and Protohistoric Landscape
Studies: Proceedings of the International Meeting, Siena, Italy,
May 25–27, 2007. British Archaeological Reports, International
Series 2320. Oxford: Archaeopress.
274 FISSION TRACK DATING
Wilkinson, T. J., 1989. Extensive sherd scatters and land-use
intensity: some recent results. Journal of Field Archaeology,
16(1), 31–46.
Cross-references
Alluvial Settings
Colluvial Settings
Electrical Resistivity and Electromagnetism
Field Geochemistry
Geophysics
Geographical Information Systems (GIS)
Landscape Archaeology
Minnesota Messenia Expedition (MME)
Paleoenvironmental Reconstruction
Soils, Agricultural
FISSION TRACK DATING
Barry Kohn
School of Earth Sciences, University of Melbourne,
Melbourne, VIC, Australia
Definition
Fission track dating is a radiometric method of age
determination based on the accumulation within insulating
solids of damage trails formed by the spontaneous nuclear
fission decay of the uranium isotope 238U.
Principles
The main mode of radioactive decay for the 238U nucleus is
a-particle emission; however, about one in every two mil-
lion decays is by nuclear fission. During fission, the heavy,
unstable nucleus splits into two uneven, positively charged
fragments. The two fragments are propelled in opposite
directions from the reaction site, dissipating their consider-
able excess kinetic energy in the host crystal lattice. This
interaction disrupts the crystal structure creating a single
linear damage trail at the atomic scale. The trails cannot
be observed optically, but because they are very reactive,
they can be enlarged with chemical etchants to become vis-
ible under an optical microscope. The maximum size of an
etched fission track depends on the physical and chemical
properties of the host mineral but is typically about
11–17 mm long and 1–2 mm wide. Although spontaneous
fission occurs in other naturally occurring heavy isotopes
(e.g., 235U and 232Th), their half-lives are too long to pro-
duce a significant number of tracks. The time span over
which fission track dating can be applied is very broad
and is essentially determined by the areal density of fission
tracks preserved in the material of interest. Cultural objects
only several decades in age to minerals and glasses, some
over a billion years old, have been dated by this method.
Materials and analysis
Uranium is present as a trace element in many of the minor
rock-forming minerals, e.g., apatite (calcium phosphate),
zircon (zirconium silicate), and titanate (calcium titanium
silicate), as well as volcanic glass. As for any radioactive
decay process, spontaneous fission occurs with a specific
decay rate constant, so that the measurement of the num-
ber of tracks and 238U content – determined by either neu-
tron irradiation in a nuclear reactor or by laser ablation
inductively coupled plasma mass spectrometry
(LA-ICP-MS) – can be used to calculate a fission track
age for a mineral grain or glass fragment. Precision of
the dating depends mainly on the number of fission tracks
counted in mineral grains, as well as in standard glass
monitors (where 238U content is determined by neutron
irradiation) or from calculated analytical uncertainties
(where 238U content is measured by LA-ICP-MS).
Applications
Fission track ages can be applied in two ways.
First, where mineral samples have cooled rapidly and
remained thermally “undisturbed” relatively close to or
at the Earth’s surface, they may be used to determine abso-
lute ages, e.g., volcanic units, meteorite impact events, and
kimberlite emplacement.
Second, at elevated temperatures, tracks may be par-
tially or entirely erased by thermal annealing (repair of
track damage), during which they are gradually restored
to the ordered structure of the crystalline matrix by pro-
gressive shrinkage from each end. For apatite,
a commonly studied mineral, most track annealing pro-
ceeds progressively between about 60 and 110
C (but this
varies with heating time and chemical composition), with
the fission track clock being reset to zero with total track
erasure. The annealing temperature range is equivalent to
depths between about 2 and 6 km in the uppermost part
of the Earth’s crust. By analyzing fission track age and
track length information, the thermal history of samples
collected at the Earth’s surface or in deep boreholes can
be determined. This provides unique information for
reconstructing geological histories in terms of processes
such as tectonism, fluid flow, and landscape evolution.
Fission track thermal history studies have been applied
to a wide range of geological problems, e.g., sedimentary
basin evolution, sedimentary provenance, structural
development of orogenic belts, and continental denuda-
tion patterns (e.g., Gallagher et al., 1998; Dumitru, 2000;
Gleadow et al., 2002).
Archaeological applications have been related mostly
to dating of man-made glasses, ceramics, obsidian, and
heated stones (e.g., Wagner and van den Haute, 1992).
Because of the long half-life of spontaneous uranium fis-
sion and the relative youthfulness of archaeological mate-
rials, this often requires large samples with relatively high
uranium concentrations. Such circumstances are rare,
which limits the archaeological application of fission track
dating. Probably the best application to address archaeo-
logical questions is where the age of hominin or artifact-
bearing strata can be constrained by their stratigraphic
relation to datable volcanic units, particularly using zircon
 FLUORINE DATING
(e.g., Gleadow, 1980; Morwood et al., 1998). Fission track
dating of unheated obsidian artifacts and their uranium
content may be characteristic of a particular source area
which, if matched, may provide information on ancient
trade routes. Alternatively, if heat has been applied to an
obsidian artifact resulting in track annealing, then study
of the diameter of etched tracks can be used to determine
whether the fission track clock was partially or totally
reset, allowing the age of the artifact’s manufacture or
use to be constrained (e.g., Miller and Wagner, 1981).
Bibliography
Dumitru, T. A., 2000. Fission-track geochronology. In Noller, J. S.,
Sowers, J. M., and Lettis, W. R. (eds.), Quaternary
Geochronology: Methods and Applications. Washington, DC:
American Geophysical Union. American Geophysical Union
Reference Shelf, Vol. 4, pp. 131–156.
Gallagher, K., Brown, R., and Johnson, C., 1998. Fission track
analysis and its applications to geological problems. Annual
Review of Earth and Planetary Sciences, 26, 519–572.
Gleadow, A. J. W., 1980. Fission track age of the KBS Tuff and
associated hominid remains in northern Kenya. Nature,
284(5753), 225–230.
Gleadow, A. J. W., Belton, D. X., Kohn, B. P., and Brown, R. W.,
2002. Fission track dating of phosphate minerals and the
thermochronology of apatite. In Kohn, M. J., Rakovan, J., and
Hughes, J. M. (eds.), Phosphates – Geochemical, Geobiological
and Material Importance. Reviews in Mineralogy and Geo-
chemistry, Vol. 48, pp. 579–630.
Miller, D. S., and Wagner, G. A., 1981. Fission-track ages applied to
obsidian artifacts from South America using the plateau-
annealing and the track-size age-correction techniques. Nuclear
Tracks, 5(1–2), 147–155.
Morwood, M. J., O’Sullivan, P. B., Aziz, F., and Raza, A., 1998.
Fission-track ages of stone tools and fossils on the east
Indonesian island of Flores. Nature, 392(6672), 173–176.
Wagner, G. A., and van den Haute, P., 1992. Fission-Track Dating.
Dordrecht: Kluwer.
Cross-references
40
Ar/39Ar and K–Ar Geochronology
Cosmogenic Isotopic Dating
Glass
Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)
Optically Stimulated Luminescence (OSL) Dating
Paleomagnetism
Radiocarbon Dating
U-Series Dating
Volcanoes and People
FLUORINE DATING
Matthew R. Goodrum
Department of Science and Technology in Society,
Virginia Tech, Blacksburg, VA, USA
Synonyms
Fluoride dating; Fluorine absorption dating
275
Definition
Fluorine dating is a method that measures the amount of
fluoride absorbed by bones in order to determine their rel-
ative age. Unlike radiometric dating methods, it cannot
provide a chronometric (or calendrical) date. Fluorine dat-
ing provides only a relative date for bone, revealing
whether specimens are older or younger than one another
or if they are of the same age (Berger and Protsch, 1991;
Lyman et al., 2012).
Fluorine dating relies on the discovery that bone min-
eral, calcium hydroxyapatite, will absorb fluoride ions if,
during burial, it is exposed to groundwater that contains
fluoride. Groundwater and soil in most parts of the world
contain small amounts of fluoride, and these ions can
replace the hydroxyl ions in bone mineral to form
fluorapatite. In this way, the chemically unstable Ca10
(PO4)6(OH)2 is gradually replaced by the more stable
Ca5(PO4)3F. Bones absorb fluoride over time, and as
a result, those that were buried long ago will contain more
fluoride than those buried more recently. However, since
fluoride concentrations vary significantly in different geo-
graphical areas because of sediment chemistry as well as
sediment hydrology, this method is reliable only when
bones from the same location are compared. Furthermore,
bone density and size also affect fluorine absorption, so
not all types of bone in a skeleton will absorb fluorine at
the same rate. Thus, caution is required when employing
this method, and for these reasons, as well as the develop-
ment of other dating methods, fluorine dating fell out of
common use over the last half century.
History
In the 1890s, the French paleontologist Emile Rivière
solicited the assistance of Adolphe Carnot, a chemist at
the School of Mines in Paris, to test human bones he had
excavated along with Pleistocene animal fossils in caves
near the town of Menton in southern France in order to
determine if the human and animal bones were of the same
age. Carnot developed techniques for measuring the fluo-
rine content of fossil bones and conducted tests to demon-
strate the validity of his new fluorine dating method.
Carnot’s method was successfully used in the 1890s to set-
tle questions about the relative ages of contested human
fossils found with Pleistocene animals, but the method
soon fell into disuse. The English geologist Kenneth Oak-
ley reintroduced the method in 1947 and later used it to
resolve the contentions problem of the Piltdown Man fos-
sils. Charles Dawson originally collected the skull frag-
ments and partial jaw bone of Piltdown Man in southern
England between 1908 and 1912. This presumed ancient
hominin was greeted with great excitement in Britain,
yet from the start there were doubts about the antiquity
of the fossils and whether the jaw and skull bones
belonged to the same creature. Oakley collaborated with
chemist Randall Hoskins to test the Piltdown finds and
eventually showed that the jaw was significantly younger
than the skull bones and that both were younger than the
276 FORENSIC GEOARCHAEOLOGY
Pleistocene animal fossils found nearby. The fluorine dat-
ing method contributed to other evidence that convinc-
ingly demonstrated that the Piltdown fossils were
a forgery. More importantly, Oakley used this method to
settle disputes over other contested prehistoric human fos-
sils (Goodrum and Olson, 2009).
Bibliography
Berger, R., and Protsch, R., 1991. Fluorine dating. In Göksu, H. Y.,
Oberhofer, M., and Regulla, D. (eds.), Scientific Dating
Methods. Dordrecht: Kluwer, pp. 251–270.
Goodrum, M. R., and Olson, C., 2009. The quest for an absolute
chronology in human prehistory: anthropologists, chemists and
the fluorine dating method in palaeoanthropology. British Jour-
nal for the History of Science, 42(1), 95–114.
Lyman, R. L., Rosania, C. N., and Boulanger, M. T., 2012. Compar-
ison of fluoride and direct AMS radiocarbon dating of black bear
bone from Lawson Cave, Missouri. Journal of Field Archaeol-
ogy, 37(3), 226–237.
Cross-references
40
Ar/39Ar and K–Ar Geochronology
Archaeomagnetic Dating
Dendrochronology
Fission Track Dating
Paleomagnetism
Radiocarbon Dating
U-Series Dating
FORENSIC GEOARCHAEOLOGY
J. M. Adovasio
Research Programs/Services, Florida Atlantic
University–Harbor Branch, Fort Pierce, FL, USA
Definition
Forensic Geoarchaeology: The application of multidis-
ciplinary, high-resolution analytical techniques from geol-
ogy, archaeology, physical science, and earth science in
the examination, recovery, and interpretation of outdoor
crime scenes.
Introduction
Prior to the early 1980s, forensic geoarchaeology essen-
tially did not exist. While the geological “context” of out-
door crime scenes had been scrutinized to varying degrees
for more than a century, the use of high-resolution,
geoarchaeological analytical protocols in forensic applica-
tions was unknown. The genesis of forensic
geoarchaeology as a subdiscipline took place as a result
of an unusual turn of events. A particular series of
geoarchaeological evaluations of criminal evidence, nar-
rowly circumscribed in time, illustrated their power in
revealing information useful in a court of law.
In the late spring of 1984, the author was contacted by
the then state archaeologist of Utah, D. Brigham Madsen,
who inquired into the excavation protocols and attendant
analyses conducted during the excavations at
Meadowcroft Rockshelter, Washington County, Pennsyl-
vania, in the 1970s. The protocols had been initiated and
refined by James Adovasio, Jack Donahue, and Gary
Cooke as tools in the investigation of the deeply stratified,
multicomponent closed site located on an unglaciated por-
tion of the Allegheny Plateau approximately 46 km south-
west of Pittsburgh (Figure 1). From its first season in 1973
to the present, this locality has been the focal point of an
intensive multidisciplinary, research project that has gen-
erated hundreds of publications and technical papers.
Long famous, or infamous, for the controversial dating
of its early occupational components, the site is equally
well known, albeit in much smaller circles, for the extreme
rigor and great precision of the excavation, analytical, and
documentary methodologies employed. Unlike the age of
the earliest deposits, these protocols were never the sub-
ject of any debate.
Of greatest interest to the Utah state archaeologist were
the techniques used to excavate and characterize the many
microstrata which composed most of the 11 major deposi-
tional units at the site (Figure 2). In some cases, these
microstrata were thinner than a trowel blade (1.35 mm)
and were often tediously excavated with single-edged
razor blades. Moreover, they represented, in depositional
terms, just moments in time. By 1984, many of these
microstrata had been subjected to a battery of macro-
and micro-sedimentological analyses involving both con-
ventional (i.e., sieve based) grain size study and rigorous
instrumental compositional analyses. Among the latter
were Coulter counter-based quantification of silt-sized
materials (which represented the first use of this technique
in North American closed site archaeology), a variety of
geochemical assays, and even scanning electron micros-
copy (SEM) of individual sand grains. The original pur-
pose of these analyses was to provide objective
verification of the subjectively perceived differences
between these microstrata in order to elucidate subtle
changes in the depositional history of the site. Each
microstratum had a distinctive suite of physical and geo-
chemical attributes, i.e., each had a unique
microsedimentary signature.
The Utah state archaeologist was interested to know
whether the rigorous and detailed analyses conducted at
Meadowcroft Rockshelter could be applied to legal cases
in a forensic evidentiary capacity, and the results of several
first “trials” represented the “birth” of forensic
geoarchaeology.
Forensic applications
The main task in 1984 was to exploit the analytical
techniques used to discriminate the Meadowcroft
microstrata in the cause of helping to adjudicate
ARPA violations. ARPA refers to the Archaeological
 FORENSIC GEOARCHAEOLOGY 277

Forensic Geoarchaeology, Figure 1 General view of the new protective structure/visitors platform at Meadowcroft Rockshelter. The
work here has directly led to the development of the forensic geoarchaeological techniques discussed in this entry.

Forensic Geoarchaeology, Figure 2 General view of some of the microstratigraphy at Meadowcroft Rockshelter.

Resources Protection Act of 1979, enacted to protect applications was USA versus Earl K. Shumway,
sites and other cultural remains on public and Indian a notorious and, to some, a near mythic figure in the his-
lands from vandalism and theft. The “test case” that tory of archaeological looting in the Greater American
would become the template for all future Southwest.
278 FORENSIC GEOARCHAEOLOGY
Horse Rock Ruin litigation
In April of 1984, E. K. Shumway of Blanding, Utah, plun-
dered a cache of 28–32 Pueblo III coiled and plaited bas-
kets from Horse Rock Ruin, in the Monticello Ranger
District of the Manti-La Sal National Forest, San Juan
County, Utah. Horse Rock Ruin lies within an area locally
known as Jack’s Pasture. The USDA Forest Service
recovered about one half of the collection, which was used
along with other evidence in the subsequent indictment of
Shumway on 14 November 1984.
Shumway maintained that the baskets in question were
ethnographic materials and did not derive from a site on
federal property but rather from a site or sites on private
land (which would not have been an ARPA violation).
This claim has become the standard alibi in virtually all
similar ARPA cases. The baskets were sent to the author
for evaluation, and our collective cooperation was
solicited in demonstrating that these items did, in fact,
derive from Horse Rock Ruin (Donahue and Adovasio,
1986). The procedures are described in the following
paragraphs.
Detailed attribute analysis of the basketry clearly dem-
onstrated that, contrary to Shumway’s claim, the items
were all of Pueblo III Anasazi (or, in contemporary jargon,
Ancestral Pueblo) ascription and, in fact, probably
represented a single aboriginal caching event from the
thirteenth century (Adovasio and Andrews, 1990).
In order to establish the provenience of the baskets,
a wide range of sediment samples was obtained and ana-
lyzed. These samples included sediments from the Horse
Rock Ruin itself, the roof and walls of the alcove immedi-
ately contiguous to the suspected location of illicit dig-
ging, and other nearby alcoves. Small samples were
extracted from the recovered baskets, and additional sur-
face samples taken from federal and private lands were
also included for comparison.
Eighty-five sediment samples were analyzed in all,
including 9 from the baskets, 58 from the Horse Rock
Ruin site and contiguous alcove, 8 from four other
alcoves, and 2 from open locations in the Jack’s Pasture
area. Interestingly, though Shumway had carefully
cleaned the baskets, sufficient sediment remained under
the stitches or between the plaiting elements to permit
removal of enough material for analytical purposes.
Indeed, the great advantage to some of these analytical
techniques is that they require less sediment than normally
accumulates under a gardener’s fingernails.
All bulk samples were sieved through a 1 mm screen to
remove coarse sand and pebbles, and the sifted fraction
was then passed through a riffle sample splitter to obtain
a representative subsample weighing less than 10 g.
These samples were then crushed via mortar and pestle
and transferred to sample cups covered with Mylar for
analysis by energy dispersive X-ray fluorescence (XRF).
The X-ray fluorescence analysis detects elements
heavier than aluminum and was performed on a Tracor
Northern Spectrace 440 spectrometer. Two scans were
made: one at 20 kV and 0.1 mA and the other at 35 kV
and 0.1 mA with a thin molybdenum window to block
out most of the direct signal from the molybdenum
X-ray tube. The spectrum at each setting was recorded
for 100 s. The individual spectral lines for the elements
were identified, and their intensities were recorded. United
States Geological Survey standards were also analyzed to
provide calibration coefficients for the calculation of ele-
ment concentrations from the intensity data. Selected sam-
ples were also analyzed by X-ray diffraction (XRD),
a method which identifies the mineral phases in which
the elements occur. The diffraction analysis was run on
a General Electric XRD-5 unit with a copper X-ray tube
at 35 kV and 15 mA. Medium resolution slits were used
and a scanning rate of 2.2 was employed.
The XRF analysis detected the presence of the follow-
ing elements: aluminum, silicon, sulfur, chlorine, potas-
sium, calcium, titanium, manganese, iron, copper, zinc,
bromine, arsenic, rubidium, strontium, and zirconium
(Table 1). Copper, bromine, and arsenic were detected in
only a few (less than ten) samples and seemed to show
no specific trend in their occurrence. Aluminum was
detected in about one third of the samples but is probably
present in all of them; the detection capability of XRF for
aluminum (and light elements such as magnesium,
sodium, and carbon) is extremely poor, and because of
this, no attempt was made to determine the actual amount
of aluminum present in the samples. Zirconium concentra-
tions were also not determined exactly. Imprecision in the
analysis of the latter element results from the interface of
the molybdenum X-ray tube peaks with the zirconium
peaks.
Concentrations of elemental silicon, potassium, cal-
cium, sulfur, chlorine, manganese, titanium, iron, zinc,
strontium, and rubidium were also used to calculate their
oxide content. The difference between the sum of these
elements and oxides and 100 % represents the missing ele-
ments: carbon, sodium, magnesium, and aluminum,
which were not included due to poor detection.
The XRD analysis showed quartz (SiO2) to be the dom-
inant mineral in all samples together with various clay
minerals (containing potassium, magnesium, silicon, alu-
minum, oxygen, and hydrogen), K-feldspar (KAlSi3O8),
calcite (CaCO3), and gypsum (CaSO4 2H2O) present in
lesser amounts. The mineral dolomite (CaMg(CO3)2), var-
ious iron oxides, halite, and polyhalite may also be present
in some of the samples in very small amounts. The XRD
analysis combined with examination of bivariate cross
plots of the elemental data allowed the determination of
which elements were associated with the various mineral
phases (Table 1). These were as follows: silicon
(associated with quartz, feldspar, and clays); potassium
(associated with clays, feldspar, and polyhalite); calcium
(associated with calcite, gypsum, and dolomite); iron
(associated with clays and iron oxides); titanium
(associated with clays and iron oxides); chlorine
(associated with halite); sulfur (associated with gypsum
 FORENSIC GEOARCHAEOLOGY 279

Forensic Geoarchaeology, Table 1 XRF analysis results for sediment samples collected from Horse Rock Ruin, Monticello Ranger
District, Manti-La Sal National Forest, San Juan County, Utah

Associated with
Element Comment Quartz Feldspar Clays Polyhalite Halite Gypsum Dolomite Calcite Iron oxides Carbonates

Al (aluminum) Poor detection

Zr (zirconium) Poor detection
Si (silicon) Oxide calculated x x x
K (potassium) Oxide calculated x x x
Ca (calcium) Oxide calculated x x x
S (sulfur) Oxide calculated x x
Cl (chlorine) Oxide calculated x
Mn (manganese) Oxide calculated x x
Ti (titanium) Oxide calculated x x
Fe (iron) Oxide calculated x x
Zn (zinc) Oxide calculated x
Sr (strontium) Oxide calculated x x x
Rb (rubidium) Oxide calculated x
Cu (copper) Variable
Br (bromine) Variable
As (arsenic) Variable

and polyhalite); zinc (associated with carbonates); stron-
tium (associated with clays, calcite, and gypsum); rubid-
ium (associated with feldspar); and manganese
(associated with quartz and feldspar).
Further examination of the bivariate plots of the ele-
mental data showed that the sediment samples from the
various sample groups tended to cluster in relatively tight
configurations. This clustering is caused by the degree of
similarity within each sample group. Examination of the
bivariate plots for different elements demonstrated that
the degree, or tightness, of clustering was best demon-
strated by the elements calcium, potassium, chlorine, and
sulfur. All these elements were present in mineral phases
associated with the soluble portion of the sediment
(calcite, gypsum, and polyhalite). These minerals precipi-
tate within any pore space, and one would expect their
abundance to be controlled primarily by the groundwater
chemistry of the specific location from which they were
collected. The abundance of the four elements (calcium,
potassium, chlorine, and sulfur) was used in
a computerized multivariate statistical analysis to deter-
mine the degree of similarity among the various sample
groups.
The four variables (calcium, potassium, chlorine, and
sulfur) were converted to standardized scores by
subtracting the mean of a variable from each value for that
variable and dividing the result by the standard deviation
of that variable. These standardized scores were the basis
for calculating a Euclidean distance between each pair of
the 85 sediment samples analyzed. These Euclidean dis-
tances represented how like or unlike each pair of samples
was in terms of the four variables measured. Because their
values were first standardized, each of the four variables
contributed equally to the distance measurement.
Results of the statistical analysis clearly indicated that
the sediment adhering to the interstices of the coiled and
plaited baskets was most similar, if not identical, to the
sediment samples from the Horse Rock Ruin site and con-
tiguous alcove. The sediment samples from the other
alcoves and open sites were clearly dissimilar. On 17 Janu-
ary 1986, Shumway pleaded guilty to the ARPA violations
in federal court in Salt Lake City, Utah.
Tin Cave litigation
In a second and, in some ways, more egregious case (USA
vs. Ralph Cortiana), R. Cortiana was indicted in 1987 for
attempting to sell a Native American infant mummy to an
undercover federal agent for $35,000. Cortiana had looted
the mummy with a wealth of accompanying grave goods
from Tin Cave on the Tonto National Forest near Roose-
velt Lake, northeast of Phoenix, Arizona (Donahue and
Cooke, 1987).
At the request of the US Attorney’s office in Phoenix,
the author and the late R. L. Andrews examined the
mummy and associated grave goods and determined that
they were either of Hohokam or Salado ascription. Addi-
tionally, a radiocarbon assay was processed on
a fragment of deerskin (Odocoileus sp.) associated with
the mummy. This assay yielded a date of 1350  2514C
yr BP.
In order to obtain a definite link between the despoiled
remains and the suspected site of vandalism, sediment
samples adhering to the body and the mummy’s grave
goods were removed, and three additional sediment sam-
ples were collected by the author from the floor of Tin
Cave itself. Each Tin Cave sample was collected from
a different location within the cave, including the alleged
280 FORENSIC GEOARCHAEOLOGY
burial pit, in order to ascertain if different portions of the
surface evidenced distinctive geochemical signatures
(Donahue and Cooke, 1987).
The samples initially were examined via optical binoc-
ular microscopy. Microscopic examination revealed that
the larger size fraction of each sample consisted of highly
variable amounts of organic detritus and rock fragments.
In order to eliminate this highly variable coarse material,
the samples were dry-sieved, and the fraction containing
particulate sizes smaller than 63 m – that is, 63 micrometers
(mm) or 0.063 mm – was retained for further analysis. Two
analytic methods were then employed to characterize the
samples.
Mineral composition of the samples was determined by
X-ray diffraction (XRD) analysis. The diffraction analysis
was again run on a General Electric XRD-5 unit with
a copper X-ray tube at 35 kV and 15 mA. Medium resolu-
tion slits were used, and a scanning rate of 2.2 was
employed. Bulk mineralogy was determined from a 63
m-or-smaller sample that was mixed with an aluminum
metal internal standard and ground to a finer grain size with
a mortar and pestle. Each sample was sifted onto a Vaseline-
coated glass slide and was then X-rayed using standard ana-
lytical procedures. Clay mineralogy was determined by
examining an organic-free, oriented mount of a less than
3 m size fraction from each sample. The organics were
removed from each sample by digestion in sodium hypo-
chlorite. The less than three micron size fraction was
obtained from each sample by gravity settling in an aqueous
medium. A slurry of this <3 m size fraction was then placed
on a glass slide. After drying, the sample was saturated with
ethylene glycol and X-rayed using standard procedures.
The samples were then heated to 300
C and 500
C, with
X-ray patterns obtained after each heating.
Chemical composition of the samples was determined
by X-ray fluorescence (XRF) analysis. The fluorescence
analysis, which as noted above identifies elements heavier
than aluminum, was run on the same Tracor Northern
Spectrace 440 unit. Splits of the <63 m size samples were
treated by ignition of the sample to 1000
C in order to
decompose organic and inorganic carbon. During ignition,
weight loss of each sample was determined at 110
C,
550
C, and 1000
C. These values indicate the mass of
absorbed water, organic carbon, and inorganic carbon con-
tent, respectively, that had been lost through ignition. Each
sample was then crushed in a mortar and pestle and trans-
ferred to sample cups covered with Mylar. For XRF anal-
ysis, two scans were run for each sample, one at 20 kVand
0.1 mA and the other at 35 kVand 0.1 mA, each with a thin
molybdenum window to block out most of the direct sig-
nal from the molybdenum X-ray tube. The spectrum at
each setting was recorded for 200 s. The individual spec-
tral lines for each element were identified, and their inten-
sities were recorded. United State Geological Survey
standards were also analyzed to provide calibration coeffi-
cients for the intensity data in order to determine element
concentrations. These concentrations were then normal-
ized to 100 % of the <63 m size ignited sample.
Analysis by XRD determined that the following min-
erals were present in all four samples: quartz, calcite, feld-
spar, apatite, whewellite, and the clay minerals, smectite,
illite, and chlorite. After identification of mineral phases,
the amount of each mineral was estimated from the inten-
sity of major peaks and the internal standard method of
calculation. Correction factors to convert from peak inten-
sities to mineral percentage were determined by running
pure mineral/aluminum mixtures. The resulting percent-
ages were normalized to 100 %. Because no pure sample
of the rare mineral whewellite (hydrous calcium oxalate
or CaC2O4·H2O) was available, a ratio value was deter-
mined by comparing the whewellite peak to the aluminum
internal standard peak. In addition, clay mineral percent-
ages were determined by using clay standards to derive
correction factors in order to calculate the amount of each
clay mineral.
Although some difference occurred in the percentage
values, the mineral composition of all four samples was
the same. All of the samples contained quartz, feldspar,
calcite, and the clay minerals, smectite, illite, and chlorite.
This is not surprising as these minerals are commonly
found in sediments. Detailed analysis of the clay minerals,
however, revealed several distinctive characteristics that
all four samples had in common.
The dominant clay mineral assemblage was a mixture of
illite and smectite. Lesser amounts of chlorite were present.
No kaolinite, a relatively common clay mineral, was
detected in any of the samples. During XRD analysis of
the bulk sample (<63 m fraction) from each of the four sam-
ples, the position of the smectite 001 reflection suggested
that this clay predominantly contains calcium rather than
sodium in the exchange positions. This indicates a calcium-
rich environment for both the Tin Cave sediments and the
sediment collected from the mummified infant.
In the detailed clay mineral XRD analysis (<3 m sam-
ples) of all four sediments, the smectite also showed
unusual behavior when it was heated. Smectite,
a swelling clay, usually loses its water and collapses when
heated to 300
C for 1 h. In the four samples, however, the
smectite only partially collapsed at 300
C. Complete col-
lapse of the smectite occurred only upon additional
heating to 500
C. Although the precise cause for this
unusual behavior was not determined, it is very likely that
it is identical in all four samples. This further suggests
a common source for all four samples.
The occurrence of apatite in all of the samples is also
suggestive of a common origin for all of them. Apatite is
frequently found in association with organic material,
especially bones and teeth, and thus it can be expected in
the Tin Cave setting. Most unusual, however, is the occur-
rence of the mineral whewellite, which is extremely rare.
We have found only two documented occurrences in the
USA. These are in concretions in the Devonian Huron
black shales of Ohio and in some modern peat bogs
located in Florida. Whewellite appears to be associated
with the alteration of woody organic detritus in a neutral
to basic, calcium-rich environment.
 FORENSIC GEOARCHAEOLOGY
The XRF analysis detected the presence of the follow-
ing elements: silicon, calcium, aluminum, iron, potassium,
manganese, titanium, zinc, strontium, copper, and rubid-
ium. Examination of both the mineral and chemical data
makes it possible to assign the elements and their oxides
to the minerals in which they occur. The chemical data,
coupled with their associations, provided the basis for
a statistical analysis of the Tin Cave and mummified infant
soil samples. In particular, the association of the trace ele-
ments (Rb, Sr, Zn, Cu, K, Ti, Fe, and Mn) with the clay
minerals formed the basis for generating a series of ratios
to be used in statistical analysis. Once again, Euclidean
distances were calculated between the samples, and the
results conclusively showed that the soil adhering to the
mummified infant was essentially identical to the samples
from Tin Cave.
Cortiana elected not to plead out in this case, though the
defense inexplicably stipulated to the damning
geoarchaeological evidence. He was eventually found
guilty in the first ARPA case involving forensic sedimen-
tology to be argued before a jury.
Site 206 litigation
Since these first forays into the use of forensic sedimentol-
ogy both involved closed sites (i.e., a cave, rock-shelter, or
architectural alcove), it was decided that the logical exten-
sion of this line of evidence collecting and analysis was to
employ the same protocols in a case involving open site
vandalism. This posed special problems that required the
use of additional highly sensitive techniques not
employed in earlier cases.
The suspect in the first open-site case, W. E. Sherman,
was alleged to have removed artifacts from a Pueblo-style
aboriginal surface structure on an archaeological site des-
ignated AR-03-06-07-206 (hereafter called Site 206)
located in the Gila National Forest in New Mexico
(Donahue et al., 1990). Sherman claimed the seized
materials derived from private land located very close to
the suspected locus of looting. This parcel of property
contained two prehistoric sites (hereafter called
Sites 1 and 2) which had also been looted. Later, Sherman
changed his story and suggested the seized material
came from a third site also located on private land
a considerable distance from Site 206. This site was
designated XSX.
In order to tie Sherman’s artifacts to Site 206, the
suspected location of the theft, evidence was sought and
scrutinized from four compositional classes of samples.
These included bedrock samples, soil samples, daub sam-
ples, and fired aboriginal potsherds. Bedrock and soil sam-
ples were provided by the USDA Forest Service and/or
collected by the author from a series of archaeological
locations within or adjacent to the Gila National Forest,
New Mexico. Soil was also removed from the hand tools
and clothing found in Sherman’s possession and possibly
used in the vandalizing of Site 206. Finally, soil was col-
lected from the inner surfaces of ceramics also found in
281
Sherman’s possession, and the ceramics were seized
as well.
The soil samples specifically include four samples
manually collected by USDA Forest Service personnel
from a vandal’s pit, which was designated as Hole 6 and
located within an aboriginal structure on Site 206. One
sample derived from the subfloor of floor feature #7, while
three samples were extracted from the modern ground sur-
face and at depths of 30 cm and 61 cm below the modern
ground surface of Hole 6, respectively.
Soils collected by the author from Site 206 included
three samples from the same room sampled by USDA For-
est Service personnel, but these were obtained from the
buried undisturbed walls rather than the mechanically
turbated fill of this structure. The samples were manually
removed by trowel at depths of 50–60 cm, 60–70 cm,
and 80–90 cm below modern ground surface,
respectively.
The USDA Forest Service also provided soil samples
from three other locations, including one each from Site
AR-03-06-07-205 (hereafter called Site 205) on federal
property and two sites designated Sites 1 and 2 on private
land. The USDA Forest Service Site 205 sample was col-
lected from an aboriginal structure fill at a depth of 20 cm
below modem ground surface as were the general soil (i.e.,
non-structure fill) samples from Sites 1 and 2. In addition,
the author collected two samples from the site designated
as XSX and located on private land directly adjacent to the
Gila National Forest. These samples were taken via trowel
from gravel fill at depths of 10 cm and 14 cm below mod-
ern ground surface, respectively.
The samples provided by the USDA Forest Service
from Sherman’s hand tools and clothing include soil sam-
ples from an ice pick, a shovel, and a pick ax. The sample
from the clothing was principally derived from the pockets
of a pair of coveralls.
The last suite of soils included three samples
provided by the USDA Forest Service representing scrap-
ings of fill derived from the inner surfaces of aboriginal
ceramic vessels found in the possession of the alleged
pothunter.
A number of daub samples were collected by the
USDA Forest Service personnel and the author;
they include two specimens from Site 206, one from
Site 1 and one found in the possession of the alleged
pothunter.
Finally, the ceramic samples provided by the USDA
Forest Service included two conjoining ceramic sherds
from Site 206. The two sherds conjoin a third sherd recov-
ered in the possession of the alleged pothunter.
Six different techniques were employed on the samples
from New Mexico. These included:
1. Grain size analysis (using sieves for the sand-sized
fraction of each sample and Coulter counter analysis
for the silt- and clay-sized fractions)
2. Flame emission spectrophotometry to determine abun-
dances of exchangeable and extractable metallic
282 FORENSIC GEOARCHAEOLOGY
cations of both major and trace elements including bar-
ium, cadmium, calcium, cobalt, copper, iron, lead,
magnesium, manganese, nickel, potassium, sodium,
strontium, and zinc
3. Flow injection and high-performance liquid chroma-
tography to determine the type and amount of organic
material present in the samples
4. Water leach atomic absorption (WLAA) via a Varian
SpectrAA 300 unit to determine the type and amount
of more water-soluble cations present in the samples
5. X-ray diffraction analysis via a General Electric
XRD-5 unit with a copper X-ray tube at 35 kV and
15 mA to determine bulk mineralogy for five mineral
phases (quartz, feldspar, orthoclase, microcline, and
plagioclase)
6. Computer-controlled scanning electron microscopy
(CCSEM)
CCSEM is an analytic technique used to acquire infor-
mation on the size, shape, and both chemical and mineral
composition of individual sediment grains in a soil sample
in an automated manner. It is performed by combining
three analytic tools under the control of a computer:
(1) the scanning electron microscope (SEM), which is
widely used in materials science because of its high reso-
lution and depth of field; (2) energy dispersive X-ray spec-
troscopy (EDS), which adds to the SEM the extra
dimension of X-ray microanalysis; and (3) the electron
beam control via the digital scan generator, which allows
rapid measurement of the size and shape of individual soil
grains found in the SEM image.
Finally, thin sections were prepared from the two
conjoining ceramic sherds and examined with a Leitz pet-
rographic microscope. This examination allowed charac-
terization and identification of coarser-grained temper
(inclusions) as well as characterization of both paste and
void space within each sherd.
After a somewhat lengthy jury trial in which, for the
first time, the defense produced its own expert witness,
Sherman was convicted on all counts.
More recent cases
Since these initial cases in forensic sedimentology, the
author and his associates have been involved in a series
of ARPA prosecutions, all of which have resulted in plea
bargains or convictions. As in the three cases summarized
above, in each instance, the accused had vandalized a site
or sites on federal property. Additionally, all claimed the
purloined artifacts were ethnographic in origin and
derived from nearby private land, or they denied culpabil-
ity completely. Space and time constraints preclude any
in-depth discussion of the post W. E. Sherman cases; how-
ever, certain salient facts about several of them are worth
noting. In the celebrated and highly publicized Polar Mesa
case, actually a series of many separate ARPA prosecu-
tions, a group of individuals was charged with vandalizing
a number of closed and open localities in the Manti-La Sal
National Forest in Utah. The author’s participation in
these prosecutions was fourfold. Together with the late R. -
L. Andrews, we analyzed, described, and validated the
prehistoric age of the archaeological materials recovered
from two closed sites (42GR383 and 42ML3169) and/or
seized from the indicted suspects. Subsequently, the
author personally collected sediment samples from one
of the vandalized closed site localities and, finally, over-
saw the processing, analysis, and interpretation of sedi-
ment recovered from the seized artifacts as well as those
collected from the location of the theft (Adovasio and
Andrews, 1990; Donahue and Adovasio, 1986).
The mineralogical and chemical analysis conducted for
these prosecutions involved XRD, CCSEM (with 500 or
1000 particle samples), and water leach chemical analysis
employing a SpectrAA 300 Atomic Absorption unit for
dissolved cations and a Dionex 2120i Ion Chromatograph
for anions. These analyses were performed on two sediment
samples from each site and 18 sediment samples from
seized artifacts. The results of these analyses indicated that
the sediments from both sampled closed sites on Polar
Mesa could be readily distinguished from one another
and, further, that 12 of the seized artifacts could be matched
to site 42GR383. One artifact was matched with site
42ML3169 while another most closely corresponded to that
locality. The sediment from four other artifacts derived
from other, unsampled, looted localities. As a result of these
analyses, a series of plea bargains or convictions were
obtained.
In USA versus Tony Maschler and John D. Price, the
accused, two Coconino County Sheriff’s deputies, alleg-
edly vandalized several locations within Kinnikinnick
Pueblo (AR-03-04-05-45) on Anderson Mesa within the
Coconino National Forest, ca. 30 miles southeast of Flag-
staff, Arizona (Cooke and Adovasio, 2000). In this case,
24 sediment samples of three types were scrutinized:
13 of these derived from tools, gloves, or clothing seized
from the suspects; 3 came from seized Conus sp. shell
“tinklers” (small perforated and truncated cone-shaped
shell ornaments); and 7 derived from vandalized rooms
at the Pueblo. Analytical methodologies included manual
scanning electron microscopy (MSEM) of aggregated par-
ticulate using an SEM equipped with an EDS and the
capacity to examine the sediment in BEI (backscatter elec-
tron imaging) mode. Selected sediments were also
subjected to bulk mineralogy analysis via XRD with
a Phillips XR6 3100 XRD unit, and then the same samples
were subjected to sequential chemical leaches for carbon-
ates, sulfates, and iron oxide/hydroxide. The clay-sized
samples from the sequential leaches were also examined
for clay mineralogy via XRD.
The results of all these analyses were mutually support-
ive and conclusively linked the two suspects to the seized
artifacts and the location of the vandalism. Both submitted
guilty pleas.
The last case to be summarized here, USA versus Jerry
Lee Young, represents one of the boldest examples of site
vandalism on a grand scale (Adovasio and Illingworth,
2001; Cooke et al., 2001). Young operated a for-profit
 FORENSIC GEOARCHAEOLOGY 283

museum in Jackpot, Nevada, which contained thousands
of artifacts, many of which were allegedly removed from
federal property in at least three states. In August of
1998, the author and J. E. Thomas collected sediment
samples from three of the vandalized properties and subse-
quently removed sediments from artifacts found in seven
seized display cases. Also collected were sediments adher-
ing to a bucket confiscated from Young’s property. Young
claimed that the bucket was used to mix cement.
In total, 20 samples were analyzed in two stages. In
stage I, sediment from one of the vandalized locations was
compared to sediment from the seized bucket. XRD was
employed to determine crystalline phases in the samples,
and CCSEM with EDS was used to determine the chemistry
of individual sediment particles. A third sample, also from
the seized bucket, was examined via MSEM with EDS to
determine if it was cement as claimed by the suspect. In
the second stage, the same analytical techniques employed
in stage I were used with sediments extracted from selected
seized artifacts from the Young Museum. Once again, the
results of all of these analyses were conclusive. Sediments
from the vandalized sites were readily distinguishable from
one another. The bucket samples were not cement and
directly linked Young to one of the vandalized sites; five

a 16000

12000
Counts

8000

4000

0
10 20 30 40 50 60
Degrees 2-Theta
b 16000

12000
Counts

8000

4000

0
10 20 30 40 50 60
Degrees 2-Theta

Forensic Geoarchaeology, Figure 3 XRD plots from the Bob’s Cave case, showing: (a) the relative frequency of mineral components
in a sediment sample from one of the looted localities and (b) the relative frequency of mineral components in sediment removed
from a bucket found at Young’s house. Peaks are unlabeled as to mineral phase represented, but the figure intends to demonstrate
only the remarkable similarity between the two sample plots.
284 FORENSIC GEOARCHAEOLOGY
of the artifact-derived samples were congruent with an ori-
gin in one of the vandalized sites (Figure 3). Young was sub-
sequently convicted of multiple ARPA violations.
Summary
According to local authorities, the successful prosecution
of the cases summarized above had an immediate, if per-
haps only temporary, dampening effect on pothunting
activities in their respective areas. Unfortunately, they also
probably led to increased attention by pothunters and
dealers to such hitherto ignored considerations as the thor-
ough cleaning of looted artifacts. Tying soil residues to
site earth may become more challenging in the future,
but the science of proving looted objects to be ancient as
opposed to recent ethnographic items and documenting
their origin will continue to offer avenues to conviction
for illicit collectors. The basic utility of the forensic tech-
niques discussed here remains valid and valuable in the
prosecution of antiquities theft.
All of the cases discussed here clearly demonstrate the
extreme resolution possible with forensic
geoarchaeological analyses, generally, and forensic sedi-
mentology, in particular. In so doing, they also provide
in many cases – especially where no other probative
Forensic Geoarchaeology, Figure 4 A USDA Forest
Service employee “facing” a looter’s hole in preparation for
sampling.
information may be available – a very potent weapon in
the armamentarium of law enforcement agents.
In retrospect, certain conclusions should be stressed.
First, as with the seminal investigations at Meadowcroft
Rockshelter, the collection of samples to be retrieved, ana-
lyzed, and compared in ARPA prosecutions must be rigor-
ous and very carefully executed. Twenty-five years of
experience have demonstrated that mechanically or bio-
logically turbated sediments frequently produce mislead-
ing or erroneous results when compared to samples from
carefully excavated, undisturbed contexts. Thus, as
stressed previously (Adovasio et al., 1991), it is critical
that “fresh” (i.e., newly cut) surfaces of walls, profiles,
and “floors” be sampled by trained professionals inti-
mately familiar with the nuances of depositional processes
(Figures 4 and 5). Second, it is clear from the foregoing
that these kinds of laboratory analyses are very time con-
suming and require sophisticated instrumentation and
highly experienced personnel. Hence, they are invariably
relatively expensive and should be employed judiciously.
Nonetheless, it is clear that the expenditures of time and
money have been justified by the success rates in these
types of ARPA prosecutions. Third, though the basic field
protocols and attendant laboratory analyses have
Forensic Geoarchaeology, Figure 5 Clear, labeled stratigraphic
sequence within a looter’s hole ready for geoarchaeological
sampling.
 FOURIER TRANSFORM INFRARED SPECTROSCOPY (FTIR)
remained strategically constant over the past 25 years, the
tactics of recovery and analysis have evolved exponen-
tially. Instrumentation in both field and laboratory con-
texts is now many technological generations removed
from what was employed in 1985–1986, and, if anything,
the precision and reliability has only increased. So has the
portability of some very potent analytical tools. For exam-
ple, now there are handheld XRF devices which function
essentially like hair dryer-sized implements that permit
analysis of sediments and sediment profiles in the field
with virtually the same accuracy and reliability as tabletop
instruments.
It is pertinent to reiterate (and time has corroborated)
the author’s final comments in Adovasio and Andrews
(1990) which described the earliest applications of foren-
sic sedimentology in ARPA prosecutions. It is now
possible to detect the equivalent of “fingerprints in the
sand,” and this capability has become a powerful
weapon in the unfortunately unending conflict with those
who would destroy the archaeological legacy, not just of
Native Americans, but of all people of every cultural
heritage.
Despite the proven probity of forensic geoarchaeology
in the cases cited above, these techniques have not become
common in North America or anywhere else. The author
has been the principal investigator of all such cases prose-
cuted to date in North America. The failure of forensic
geoarchaeology to encourage a larger audience of service
providers may be attributed to several causes. (1) Thus far
all but one of its applications have been in the arcane arena
of ARPA cases – a sphere of law enforcement known lit-
tle, if at all, outside of its practitioners. (2) Even to the ini-
tiated, forensic geoarchaeology, it seems overly complex,
time consuming, and therefore daunting to many potential
practitioners. This is often the case in situations where
carefully collected data by qualified, credentialed archae-
ologists is available for potential analysis. (3) The applica-
tion of forensic geoarchaeological field and laboratory
protocols is not inexpensive. This is compounded by the
fact that few field-workers, even in archaeology, have
the requisite battery of skills to assess and prepare a site
for sampling, and almost none exist in traditional law
enforcement agencies. Additionally, the analytical equip-
ment needed for geoarchaeological research is not cheap
to acquire and maintain, and it requires expertise to oper-
ate and interpret the results of analysis. Perhaps, as the
oftentimes spectacular results of geoarchaeological analy-
sis in forensic applications become better known, the
problems of poor participation will diminish.
Bibliography
Adovasio, J. M., and Andrews, R. L., 1990. The Horse Rock Ruin
(42SA10550) Basketry Cache: An Unparalleled View of
Regional Pueblo Perishable Technology. Paper presented at the
55th annual meeting of the Society for American Archaeology,
Las Vegas, April 18–22, 1990.
285
Adovasio, J. M., Donahue, J., Cooke, G. A., and Quigley, M. N.,
1991. Forensic Geoarchaeology: Three Case Studies. Paper
presented at the 56th Annual Meeting of the Society for Ameri-
can Archaeology, New Orleans, April 23–28, 1991.
Adovasio, J. M., and Illingworth, J. S., 2001. Report on the Artifact
Technology for USAO No. 01-015-S-BLW, U.S. v. Jerry Lee
Young. Manuscript on file, Mercyhurst Archaeological Institute,
Mercyhurst University, Erie.
Cooke, G. A., and Adovasio, J. M., 2000. Report on the Forensic
Sedimentology Analysis of Selected Soil Samples for USAO
No. 2000R02203: U.S. v. Tony Maschler and John D. Price.
Manuscript on file, Mercyhurst Archaeological Institute,
Mercyhurst University, Erie.
Cooke, G. A., Adovasio, J. M., and Illingworth, J. S., 2001. Foren-
sic Sedimentologic Analysis of Sediment Samples, U.S. v. Jerry
Lee Young. Manuscript on file, Mercyhurst Archaeological Insti-
tute, Mercyhurst University, Erie.
Donahue, J., and Adovasio, J. M., 1986. Notes on the Analysis of the
Horse Rock Ruin (42SA10550) Basket Cache Sediments. Manu-
script on file, Department of Anthropology, University of Pitts-
burgh, Pittsburgh.
Donahue, J., and Cooke, G. A., 1987. Mineral, Chemical, and Sta-
tistical Analysis of Soil Samples from Tin Cave, AR-03-12-06-
104, Arizona, and from a Mummified Infant. Manuscript on file,
Departments of Anthropology, Geology and Planetary Sciences,
University of Pittsburgh, Pittsburgh.
Donahue, J., Adovasio, J. M., Cooke, G. A., and Quigley, M. N.,
1990. Report on the Mineralogical, Chemical and Statistical
Analyses of Selected Soil, Daub and Pottery Samples from the
Gila National Forest, New Mexico. Manuscript on file, Depart-
ments of Anthropology, Geology and Planetary Sciences, Uni-
versity of Pittsburgh, Pittsburgh.
Cross-references
Electron Probe Microanalyzer
Scanning Electron Microscopy (SEM)
X-ray Fluorescence (XRF) Spectrometry in Geoarchaeology
FOURIER TRANSFORM INFRARED SPECTROSCOPY
(FTIR)
Francesco Berna
Department of Archaeology, Simon Fraser University,
Burnaby, BC, Canada
Synonyms
FT-IR; Fourier transform infrared spectroscopy; Infrared
spectroscopy
Definition
FTIR (Fourier transform infrared spectroscopy) is an
instrumental technique used to identify the functional
groups present in organic and inorganic compounds by
measuring their absorption of infrared radiation over
a range of wavelengths (Smith, 2011; Margaris, 2014).
The FTIR method first collects an interferogram of
a sample signal using an interferometer, and then it per-
forms a Fourier transform (a mathematical algorithm) on
286 FOURIER TRANSFORM INFRARED SPECTROSCOPY (FTIR)
the interferogram to obtain the infrared spectrum. An
FTIR spectrometer, thus, collects and digitizes the inter-
ferogram, performs the Fourier transform, and displays
the FTIR spectrum. Modern FTIR spectrometers obtain
infrared spectra in absorption, total and diffuse reflec-
tance, attenuated total reflectance (ATR), and
photoacoustic modes from solid, liquid, or gaseous sam-
ples. Typically, only tens of micrograms of a sample are
required, and spectrometers can be coupled to micro-
scopes for the analysis of particles as small as 10 mm in
diameter. Infrared spectrometers are also available as por-
table devices and can therefore be used reliably and conve-
niently on-site.
The Uses
Infrared spectroscopy can identify and characterize both
inorganic and organic materials of geoarchaeological
interest (Weiner, 2010). This analytical technique, in fact,
has the major advantage of being able to identify both
crystalline and amorphous minerals (e.g., quartz and opal)
as well as many organic materials, including crystalline
and “amorphous” inorganic compounds (such as silicates,
carbonates, phosphates, sulfates, and nitrates) and organic
compounds (such as fatty and humic acids, oxalates, pro-
teins, lignin, cellulose, and graphite). FTIR is very sensi-
tive to compositional and structural changes such as
crystallinity and atomic disorder. It is thus particularly
useful for the identification of authigenic minerals; the
study of biomaterials such as bone, shells, and endo- and
exoskeletons of cell tissues (e.g., phytoliths) and microor-
ganisms; and the characterization of charcoal and bone
collagen. FTIR is also uniquely suitable for the identifica-
tion and characterization of pyrogenic calcite and high-
temperature silicates; thus, it can be extremely useful for
the reconstruction of ancient pyrotechnological activities.
FTIR is therefore a very valuable technique for the identi-
fication and characterization of the geogenic and biogenic
components of the archaeological record, stratigraphic
correlations, and the reconstruction of human activities,
diagenetic transformations, and site formation processes.
By using FTIR microspectroscopy, which couples an
FTIR spectrometer to a petrographic microscope, it is pos-
sible to perform FTIR analysis directly upon thin sections
of intact archaeological materials and sediments, thus
allowing the integration in real time of micromorphologi-
cal, petrographic, chemical, and mineralogical analyses
(Goldberg and Berna, 2010). In turn, the data produced
by integrating soil micromorphology and FTIR
microspectroscopy can yield high-resolution, contextual-
ized information about technology, activities, and site for-
mation processes.
Bibliography
Goldberg, P., and Berna, F., 2010. Micromorphology and context.
Quaternary International, 214(1–2), 56–62.
Margaris, A. V., 2014. Fourier Transform Infrared Spectroscopy
(FTIR): applications in archaeology. In Smith, C. (ed.), Encyclo-
pedia of Global Archaeology. New York: Springer,
pp. 2890–2893.
Smith, B. C., 2011. Fundamentals of Fourier Transform Infrared
Spectroscopy, 2nd edn. Boca Raton, FL: CRC Press.
Weiner, S., 2010. Microarchaeology: Beyond the Visible Archaeo-
logical Record. New York: Cambridge University Press.
Cross-references
Site Formation Processes
Soil Micromorphology