ASTM E2490-09(2015)

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

SIGNIFICANCE AND USE
5.1 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.

General Information

• Status: Historical
• Publication Date: 31-Mar-2015
• ICS: 71.100.01 - Products of the chemical industry in general
• Technical Committee: E56 - Nanotechnology
• Drafting Committee: E56.02 - Physical and Chemical Characterization

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 (Reapproved 2015)
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 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 2.2 ISO Standards:
ISO 13320-1 Particle Size Analysis—Laser Diffraction
1.1 This guide deals with the measurement of particle size
3
Methods—Part 1: General Principles
distribution of suspended particles, which are solely or pre-
ISO 14488Particulate Materials—Sampling and Sample
dominantly sub-100 nm, using the photon correlation (PCS)
3
Splitting for the Determination of Particulate Properties
technique. It does not provide a complete measurement meth-
ISO 13321 Particle Size Analysis—Photon Correlation
odology for any specific nanomaterial, but provides a general
3
Spectroscopy
overview and guide as to the methodology that should be
followed for good practice, along with potential pitfalls.
3. Terminology
1.2 This standard does not purport to address all of the
3.1 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.1.1 Some of the definitions in 3.1 will differ slightly from
responsibility of the user of this standard to establish appro-
those used within other (non-particle sizing) standards (for
priate safety, health, and environmental practices and deter-
example, repeatability, reproducibility). For the purposes of
mine the applicability of regulatory limitations prior to use.
thisGuideonly,weutilizethestateddefinitions,astheyenable
1.3 This international standard was developed in accor-
the isolation of possible errors or differences in the measure-
dance with internationally recognized principles on standard-
ment to be assigned to instrumental, dispersion or sampling
ization established in the Decision on Principles for the
variation.
Development of International Standards, Guides and Recom-
3.1.2 correlation coeffıcient, n—measure of the correlation
mendations issued by the World Trade Organization Technical
(or similarity/comparison) between 2 signals or a signal and
Barriers to Trade (TBT) Committee.
itself at another point in time.
3.1.2.1 Discussion—If there is perfect correlation (the sig-
2. Referenced Documents
nals are identical), then this takes the value 1.00; with no
2
2.1 ASTM Standards:
correlation then the value is zero.
E177Practice for Use of the Terms Precision and Bias in
3.1.3 correlogram or correlation function, n—graphicalrep-
ASTM Test Methods
resentation of the correlation coefficient over time.
E691Practice for Conducting an Interlaboratory Study to
3.1.3.1 Discussion—This is typically an exponential decay.
Determine the Precision of a Test Method
3.1.4 cumulants analysis, n—mathematical fitting of the
E1617Practice for Reporting Particle Size Characterization
correlation function as a polynomial expansion that produces
Data
some estimate of the width of the particle size distribution.
F1877Practice for Characterization of Particles
3.1.5 diffusion coeffıcient (self or collective), n—a measure
of the Brownian motion movement of a particle(s) in a
1
This guide is under the jurisdiction of ASTM Committee E56 on Nanotech-
medium.
nology and is the direct responsibility of Subcommittee E56.02 on Physical and
3.1.5.1 Discussion—After measurement, the value is be
Chemical Characterization.
inputted into in the Stokes-Einstein equation (Eq 1, see
Current edition approved April 1, 2015. Published April 2015. Originally
approved in 2008. Last previous edition in 2009 as E2490–09. DOI: 10.1520/
7.2.1.2(4)). Diffusion coefficient units in photon correlation
2
E2490-09R15.
spectroscopy (PCS) measurements are typically µm /s.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 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

---------------------- Page: 1 ----------------------
E2490 − 09 (2015)
3.1.6 Mie region, n—in this region (typically where the size reportedresults.VariationinpHislikelytoaffectthedegreeof
of the particle is greater than half the wavelength of incident agglomeration and so forth.
light), the light scattering behavior is complex a
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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 − 09 E2490 − 09 (Reapproved 2015)
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 E2490; 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 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.
2. Referenced Documents
2
2.1 ASTM Standards:
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1617 Practice for Reporting Particle Size Characterization Data
F1877 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:
3.1.1 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.
3.1.2 correlation coeffıcient, n—measure of the correlation (or similarity/comparison) between 2 signals or a signal and itself
at another point in time.
1
This guide is under the jurisdiction of ASTM Committee E56 on Nanotechnology and is the direct responsibility of Subcommittee E56.02 on Physical and Chemical
Characterization.
Current edition approved April 1, 2009April 1, 2015. Published June 2009April 2015. Originally approved in 2008. Last previous edition in 20082009 as
E2490 – 08.E2490 – 09. DOI: 10.1520/E2490-09.10.1520/E2490-09R15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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.
3.1.2.1 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.
3.1.3 correlogram or correlation function, n—graphical representation of the correlation coefficient over time.
3.1.3.1 Discussion—
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2490 − 09 (2015)
This is typically an exponential decay.
3.1.4 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.
3.1.5 diffusion coeffıcient (self or collective), n—a measure of the Brownian motion movement of a particle(s) in a medium.
3.1.5.1 Discussion—
After measurement, the value is be inputted into in the Stokes-Einstein equation (Eq 1, see 7.2.1.2(4)). Diffusion coefficient units
2
in photon correlation spectroscopy (PCS) measurements are typically μm /s.
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 interpreted with a more rigorous and exact (and all-encompassin
...