Standard Guide for Measurement of Particle Size Distribution of Nanomaterials in Suspension by Photon Correlation Spectroscopy (PCS)

SIGNIFICANCE AND USE
PCS is one of the very few techniques that are able to deal with the measurement of particle size distribution in the nano-size region. This Guide highlights this light scattering technique, generally applicable in the particle size range from the sub-nm region until the onset of sedimentation in the sample. The PCS technique is usually applied to slurries or suspensions of solid material in a liquid carrier. It is a first principles method (that is, calibration in the standard understanding of this word, is not involved). The measurement is hydrodynamically based and therefore provides size information in the suspending medium (typically water). Thus the hydrodynamic diameter will almost certainly differ from other size diameters isolated by other techniques and users of the PCS technique need to be aware of the distinction of the various descriptors of particle diameter before making comparisons between techniques. Notwithstanding the preceding sentence, the technique is widely applied in industry and academia as both a research and development tool and as a QC method for the characterization of submicron systems.
SCOPE
1.1 This guide deals with the measurement of particle size distribution of suspended particles, which are solely or predominantly sub-100 nm, using the photon correlation (PCS) technique. It does not provide a complete measurement methodology for any specific nanomaterial, but provides a general overview and guide as to the methodology that should be followed for good practice, along with potential pitfalls.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E2490 − 09
StandardGuide for
Measurement of Particle Size Distribution of Nanomaterials
1
in Suspension by Photon Correlation Spectroscopy (PCS)
This standard is issued under the fixed designation E2490; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This guide deals with the measurement of particle size 3.1 Definitions of Terms Specific to This Standard:
distribution of suspended particles, which are solely or pre-
3.1.1 Some of the definitions in 3.1 will differ slightly from
dominantly sub-100 nm, using the photon correlation (PCS)
those used within other (non-particle sizing) standards (for
technique. It does not provide a complete measurement meth-
example, repeatability, reproducibility). For the purposes of
odology for any specific nanomaterial, but provides a general
thisGuideonly,weutilizethestateddefinitions,astheyenable
overview and guide as to the methodology that should be
the isolation of possible errors or differences in the measure-
followed for good practice, along with potential pitfalls.
ment to be assigned to instrumental, dispersion or sampling
variation.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.1.2 correlation coeffıcient, n—measure of the correlation
responsibility of the user of this standard to establish appro- (or similarity/comparison) between 2 signals or a signal and
priate safety and health practices and determine the applica-
itself at another point in time.
bility of regulatory limitations prior to use.
3.1.2.1 Discussion—If there is perfect correlation (the sig-
nals are identical), then this takes the value 1.00; with no
2. Referenced Documents
correlation then the value is zero.
2
2.1 ASTM Standards:
3.1.3 correlogram or correlation function, n—graphicalrep-
E177Practice for Use of the Terms Precision and Bias in
resentation of the correlation coefficient over time.
ASTM Test Methods
3.1.3.1 Discussion—This is typically an exponential decay.
E691Practice for Conducting an Interlaboratory Study to
3.1.4 cumulants analysis, n—mathematical fitting of the
Determine the Precision of a Test Method
correlation function as a polynomial expansion that produces
E1617Practice for Reporting Particle Size Characterization
some estimate of the width of the particle size distribution.
Data
F1877Practice for Characterization of Particles
3.1.5 diffusion coeffıcient (self or collective), n—a measure
2.2 ISO Standards:
of the Brownian motion movement of a particle(s) in a
ISO 13320-1 Particle Size Analysis—Laser Diffraction medium.
3
Methods—Part 1: General Principles
3.1.5.1 Discussion—After measurement, the value is be
ISO 14488Particulate Materials—Sampling and Sample
inputted into in the Stokes-Einstein equation (Eq 1, see
3
Splitting for the Determination of Particulate Properties
7.2.1.2(4)). Diffusion coefficient units in photon correlation
2
ISO 13321 Particle Size Analysis—Photon Correlation
spectroscopy (PCS) measurements are typically µm /s.
3
Spectroscopy
3.1.6 Mie region, n—in this region (typically where the size
of the particle is greater than half the wavelength of incident
light), the light scattering behavior is complex and can only be
1
This guide is under the jurisdiction of ASTM Committee E56 on Nanotech-
interpreted with a more rigorous and exact (and all-
nology and is the direct responsibility of Subcommittee E56.02 on Physical and
encompassing) theory.
Chemical Characterization.
Current edition approved April 1, 2009. Published June 2009. Originally
3.1.6.1 Discussion—This more exact theory can be used
approved in 2008. Last previous edition in 2008 as E2490–08. DOI: 10.1520/
instead of the Rayleigh and Rayleigh-Gans-Debye approxima-
E2490-09.
2
tions described in 3.1.8 and 3.1.9. The differences between the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approximations and exact theory are typically small in the size
Standards volume information, refer to the standard’s Document Summary page on
range considered by this standard. Mie theory is needed in
the ASTM website.
3
order to convert an intensity distribution to one based on
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. volume or mass.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2490
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:E2490–08 Designation: E 2490 – 09
Standard Guide for
Measurement of Particle Size Distribution of Nanomaterials
1
in Suspension by Photon Correlation Spectroscopy (PCS)
This standard is issued under the fixed designation E 2490; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 Thisguidedealswiththemeasurementofparticlesizedistributionofsuspendedparticles,whicharesolelyorpredominantly
sub-100 nm, using the photon correlation (PCS) technique. It does not provide a complete measurement methodology for any
specific nanomaterial, but provides a general overview and guide as to the methodology that should be followed for good practice,
along with potential pitfalls.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
E 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E 1617 Practice for Reporting Particle Size Characterization Data
F 1877 Practice for Characterization of Particles
2.2 ISO Standards:
3
ISO 13320-1 Particle Size Analysis—Laser Diffraction Methods—Part 1: General Principles
3
ISO 14488 Particulate Materials—Sampling and Sample Splitting for the Determination of Particulate Properties
3
ISO 13321 Particle Size Analysis—Photon Correlation Spectroscopy
3. Terminology
3.1 Definitions of Terms Specific to This Standard— Some of the definitions in 3.1 will differ slightly from those used within
other (non-particle sizing) standards (for example, repeatability, reproducibility). For the purposes of this Guide only, we utilize
the stated definitions, as they enable the isolation of possible errors or differences in the measurement to be assigned to
instrumental, dispersion or sampling variation.
3.1.1 correlation coeffıcient, n—measure of the correlation (or similarity/comparison) between 2 signals or a signal and itself
at another point in time.
3.1.1.1 Discussion—If there is perfect correlation (the signals are identical), then this takes the value 1.00; with no correlation
then the value is zero.
3.1.2 correlogram or correlation function, n—graphical representation of the correlation coefficient over time.
3.1.2.1 Discussion—This is typically an exponential decay.
3.1.3 cumulants analysis, n—mathematical fitting of the correlation function as a polynomial expansion that produces some
estimate of the width of the particle size distribution.
3.1.4 diffusion coeffıcient (self or collective), n—a measure of the Brownian motion movement of a particle(s) in a medium.
3.1.4.1 Discussion—After measurement, the value is be inputted into in the Stokes-Einstein equation (Eq 1, see 7.2.1.2 (4)).
2
Diffusion coefficient units in photon correlation spectroscopy (PCS) measurements are typically µm /s.
3.1.5 Mie region, n—in this region (typically where the size of the particle is greater than half the wavelength of incident light),
the light scattering behavior is complex and can only be interpreted with a more rigorous and exact (and all-encompassing) theory.
1
This guide is under the jurisdiction ofASTM Committee E56 on Nanotechnology and is the direct responsibility of Subcommittee E56.02 on Characterization: Physical,
Chemical, and Toxicological Properties.
Current edition approved Oct. 1, 2008. Published November 2008.
Current edition approved April 1, 2009. Published June 2009. Originally approved in 2008. Last previous edition in 2008 as E 2490–08.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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E2490–09
3.1.5.1 Discussion—T
...

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