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ISO Standardization in Particle Characterization

M. Stintz
Research Group Mechanical Process Engineering, Institute of Process Engineering and
Environmental Technology, TU Dresden, 01062 Dresden, Germany

ABSTRACT

An overview on published ISO standards and current projects of ISO Technical Committee 24 / Subcommittee 4
"Sieves, sieving and other sizing methods" is given.
Principles of the nearly complete basic representation standard series ISO 9276-1 …-6 and experience in first
revisions (every five years) is presented. It is intended to address especially the community of users, represented
rarely in the standard developing committees, for getting a feed back on the level of comprehensibility and
practicability of representation nomenclature and analysis methods.
Concerning the representation of analysis data, a general structure of particle shape descriptors is
introduced. With respect to applications in the field of nanotechnology the work program for aerosol
characterization is presented finally as well as contact addresses for possible contributions.

1 INTERNATIONAL ORGANIZATION organizations in which their participating experts work,


but of other stakeholders too.
FOR STANDARDIZATION
2 STANDARDIZATION IN
ISO - together with IEC (International Electrotechnical
Commission) and ITU (International ISO/TC24/SC4
Telecommunication Union) - has built a strategic
partnership with the WTO (World Trade Organization) The sub-committee SC4 „Sizing by methods other than
with the common goal of promoting a free and fair sieving“ of ISO /TC 24 „Sieves, sieving and other
global trading system. sizing methods“ is responsible for developing
The political agreements reached within the framework international standards for particle size analysis.
of the WTO require underpinning by technical
agreements. 16 nations are entitled to vote (P-members):
ISO standards are technical agreements which provide Australia, Austria, Belgium, China, Finland, France,
the framework for compatible technology worldwide. Germany, Italy, Japan, Republic of Korea,
Developing technical consensus on this international Netherlands, Norway, Sweden, Switzerland, USA,
scale is a major operation. United Kingdom.
In all, there are some 3 000 ISO technical groups
(technical committees, subcommittees, working groups
etc.) in which some 50 000 experts participate annually 15 nations are observing members (O-members):
to develop ISO standards. Brazil, Egypt, Greece, India, Ireland, Mexico,
ISO standards are developed by technical committees Pakistan, Poland, Portugal, Romania, Serbia and
(TC) comprising experts from the industrial, technical Montenegro, Slovakia, Spain, Turkey, Ukraine.
and business sectors which have asked for the
standards, and which subsequently put them to use. Members in Liaison:
These experts may be joined by others with relevant ISO/TC47 Chemistry, ISO/TC119 Powder metallurgy,
knowledge, such as representatives of government ISO/TC206 Fine ceramics, ISO/TC229 Nano-
agencies, testing laboratories, consumer associations, technologies.
environmentalists, academic circles and so on.
The experts participate as national delegations, chosen
The development of the standards is carried out in the
by the ISO national member institute for the country
working groups (WG):
concerned (DIN, BSI, ...). These delegations are
required to represent not just the opinions of the WG 1 "Representation of analysis data“ (convenor
Michael Stintz)
WG 2 "Sedimentation, Classification" (convenor
Dietmar Lerche) 2.2 Particle shape descriptors
WG 3 "Pore Size distribution, porosity" (convenor
Matthias Thommes)
The Draft International Standard ISO 9276-6 specifies
WG 5 "Electrical sensing zone methods" (convenor rules and a nomenclature for the description and
Billy Goransson) quantitative representation of particle shape and
WG 6 "Laser diffraction methods“ (convenor Ron morphology.
Iacocca) The relevance of any measure or method of shape
WG 7 "Dynamic light scattering" (convenor Robert representation to technological applications has to be
Finsy) the deciding factor for its selection and not the
WG 8 "Image Analysis methods„ (convenor Yoshio complete reconstruction of the geometric particle
Otani) shape.
WG 9 "Single Particle light interaction methods“ Therefore, this standard is restricted to
(convenor Kazuo Ichijo) characterization methods which can be correlated to
physical properties in industrial applications.
WG 10 "Small angle X-ray scattering" (convenor Jinyi
Chen)
WG 11 "Sample preparation" (convenor Kari The choice of an appropriate shape description method
Heiskanen) in Figure 1 depends on the measurement technique
available and the particle system (in particular its size
WG 12 "Differential electrical mobility analysis for
range) under examination.
aerosol particles“ (convenor Gilmore Sem)
Description methods based on mathematical operation
WG 14 "Acoustic methods" (convenor David Scott)
at the contour line (e.g. fractal dimension analysis or
WG 15 "Focussed scanning beam techniques„ Fourier analysis) require a relatively high resolution of
(convenor Gregor Hsiao) particle images which may be obtained by scanning
electron or light microscope.
20 Standards have been published, 14 Standards are
Particle Shape of an individual Particle
under development.
Verbal Shape Coefficients, Mathematical
Description e.g. Size or Proportion Parameters Shape Functions

2.1 Representation of analysis data


Standard shapes Macro, Meso- and Microshape descriptors - Radius-Angle-Function
(e.g. rod, disc) (e.g. geometrical descriptors like Feret- e.g. Fourieranalysis
flat, edged) diameters, Aspect Ratio)

ISO 9276 (responsible WG 1) consists of the following


parts, under the general title Dynamic (Physical) Shape Parameters (e.g.
sedimentation velocity, pressure drop)
Line-Angle –Function
e.g. Slip Chording

„Representation of Results of Particle Size analysis“


Other Parameters (e.g. electrical Tangents-Angle-Funct.
Part 1: Graphical representation, resistance) e.g. Angularity Factors

Part 2 : Calculation of average particle sizes and


moments from particle size distributions,
Figure 1 — Classification of some methods for particle
Part 3: Adjustment of an experimental curve to a shape description [1]
reference model,
Apart from such factors, the result of shape analysis
Part 4: Characterization of a classification process, may also be significantly affected by sample
Part 5: Methods of calculation relating to part. size preparation (sample size and whether it is
analysis using log. normal prob. distribution, representative, particle orientation in 2-d-analysis,..).
Part 6: The descriptive and quantitative representation This standard defines the necessary parameter set for
of particle shape and morphology. comparison of shape analyzing methods and devices.

Part 1 was published in 1998 and revised with an The properties in Figure 2 may not suffice for a
corrigendum in 2004. complete description of the shape of one particle and
Parts 2 and 4 were published in 2001 and are under may be differently defined by other authors.
revision now. But these particle shape properties give a good idea
Part 5 was published in 2001. how shape parameters can be measured at different
size levels.
Parts 3 and 6 are now circulated to the national ISO
bodies for voting. Three corresponding levels of shape can thus be
distinguished - macroshape, mesoshape and
A new work item NWIP Particle characterization of microshape.
particulate systems – terminology was established
actually.
ISO 15901-1:2005 Pore size distribution and porosity
of solid materials by mercury porosimetry and gas
adsorption -- Part 1: Mercury porosimetry
ISO 20998-1:2006 Measurement and characterization
of particles by acoustic methods -- Part 1: Concepts
and procedures in ultrasonic attenuation spectroscopy

2.4 Work program for ISO/TC 24/SC 4

PWI 9277 (WG3) “Determination of the specific surface


area of solids by gas adsorption using BET and
alternative methods”.
ISO/FDIS 15901-2 (WG 3) Pore size distribution and
porosity of solid materials by mercury porosimetry and
gas adsorption -- Part 2: Analysis of meso-pores and
Figure 2 – Illustration of surface texture, roundness macro-pores by gas adsorption
and form [2]
ISO/DIS 15901-3 (WG 3) Pore size distribution and
porosity of solid materials by mercury porosimetry and
2.3 Other already published ISO-Standards gas adsorption -- Part 3: Analysis of micro-pores by
gas adsorption

ISO 9277:1995 Determination of the specific surface


area of solids by gas adsorption using the BET method ISO/CD 13319 (WG 5) Determination of particle
size distributions -- Electrical sensing zone method
ISO 13317-1:2001 Determination of particle size
(Revision of ISO 13319:2000)
distribution by gravitational liquid sedimentation
methods -- Part 1: General principles and guidelines
ISO 13317-2:2001 Determination of particle size ISO/DIS 22412 (WG 7) Particle size analysis --
distribution by gravitational liquid sedimentation Dynamic light scattering (DLS)
methods -- Part 2: Fixed pipette method NWIP (WG 12) Validation and Calibration of Aerosol
ISO 13317-3:2001 Determination of particle size Particle Number Counters
distribution by gravitational liquid sedimentation
methods -- Part 3: X-ray gravitational technique ISO/FDIS 13322-2 (WG 8) Particle size analysis --
ISO 13318-1:2001 Determination of particle size Image analysis methods -- Part 2: Dynamic methods
distribution by centrifugal liquid sedimentation methods
-- Part 1: General principles and guidelines
ISO/CD 21501-1 (WG 9) Determination of particle
ISO 13318-2:2001 Determination of particle size size distribution -- Single particle light interaction
distribution by centrifugal liquid sedimentation methods methods -- Part 1: Light scattering aerosol
-- Part 2: Photocentrifuge method spectrometer
ISO 13318-3:2004 Determination of particle size ISO/DIS 21501-2 (WG 9) Determination of particle
distribution by centrifugal liquid sedimentation methods size distribution -- Single particle light-interaction
-- Part 3: Centrifugal X-ray method methods -- Part 2: Light-scattering liquid-borne particle
ISO 13319:2000 Determination of particle size counter
distributions -- Electrical sensing zone method ISO/DIS 21501-3 (WG 9) Determination of particle
ISO 13320-1:1999 Particle size analysis -- Laser size distribution -- Single particle light-interaction
diffraction methods -- Part 1: General principles methods -- Part 3: Light-extinction liquid-borne particle
ISO 13321:1996 Particle size analysis -- Photon counter
correlation spectroscopy ISO/DIS 21501-4 (WG 9) Determination of particle
ISO 13322-1:2004 Particle size analysis -- Image size distribution -- Single particle light-interaction
analysis methods -- Part 1: Static image analysis methods -- Part 4: Light-scattering airborne particle
methods counter for clean spaces
ISO 13323-1:2000 Determination of particle size
distribution -- Single-particle light interaction methods -- ISO/DIS 14488 (WG 11) Particulate materials --
Part 1: Light interaction considerations Sampling and sample splitting for the determination of
ISO/TS 13762:2001 Particle size analysis -- Small particulate properties
angle X-ray scattering method
ISO 14887:2000 Sample preparation -- Dispersing
procedures for powders in liquids
ISO/CD 15900 (WG 12) Determination of particle
size distribution -- Differential electrical mobility
analysis for aerosol particles

ISO/PRF 20998-1 (WG 14) Particle characterization by


acoustic methods -- Part 1: Ultrasonic attenuation
spectroscopy

2.5 Work program for aerosol characterization

Aerosol measurement techniques range from the


characterization of dry dispersion of powders (WG 6),
image analysis (WG 8) up to single particle
measurement techniques (WG 9 and 12) or clean
room monitoring (in WG 9).
A new Preliminary Work Item (PWI) with title
“Validation and Calibration of Aerosol Particle Number
Counters” will be started by WG12. The proposed work
item should cover calibration and verification from the
nm to µm region and to a particle concentration of up
to 105 cm-3. The motivation was ISO 14644-1 (Section
8.2.2) and ASTM F328-98 plus FDIA 21501-4.

2.6 How can new experts contribute to ISO


standardization?

You can contact the convenor of the responsible


Working group or
the Secretariat of ISO/TC24/SC4 (ANSI)
Dr. Kevin Powers, E-mail: kpowers@erc.ufl.edu ,
Fax: 352-846-1196

Further Information, Searching for Standards


World Standards Services Network, a network of
publicly accessible Web servers
of standards organizations around the world:
http://www.wssn.net

ISO Catalogue which can be accessed online:


http://www.iso.ch

REFERENCES:
[1] ISO/Dis 9276-6: 2006
[2] Bowman, E.T.; Soga, K.; Drummond, W.: Particle
shape characterisation using Fourier descriptor
analysis. Geotechnique 51 (2001) 545-554.

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