ASTM D4464-15
(Test Method)Standard Test Method for Particle Size Distribution of Catalytic Materials by Laser Light Scattering
Standard Test Method for Particle Size Distribution of Catalytic Materials by Laser Light Scattering
SIGNIFICANCE AND USE
5.1 It is important to recognize that the results obtained by this test method or any other method for particle size determination utilizing different physical principles may disagree. The results are strongly influenced by physical principles employed by each method of particle size analysis. The results of any particle sizing method should be used only in a relative sense and should not be regarded as absolute when comparing results obtained by other methods. Particularly for fine materials (that is, average particle size 3
5.2 Light scattering theories (Fraunhofer Diffraction4 and Mie Scattering5) that are used for determination of particle size have been available for many years. Several manufacturers of testing equipment now have units based on these principles. Although each type of testing equipment utilizes the same basic principles for light scattering as a function of particle size, different assumptions pertinent to application of the theory and different models for converting light measurements to particle size, may lead to different results for each instrument. Furthermore, any particles which are outside the size measurement range of the instrument will be ignored, causing an increase in the reported percentages within the detectable range. A particle size distribution which ends abruptly at the detection limit of the instrument may indicate that particles outside the range are present. Therefore, use of this test method cannot guarantee directly comparable results from different types of instruments.
5.3 This test method can be used to determine particle size distributions of catalysts, supports, and catalytic raw materials for specifications, manufacturing control, and research and development work.
5.4 For fine materials (that is, average particle size 6
SCOPE
1.1 This test method covers the determination of the particle size distribution of catalyst, catalyst carrier, and catalytic raw material particles and is one of several found valuable for the measurement of particle size. The range of average particle sizes investigated was from 1 to 300 μm equivalent spherical diameter. The technique is capable of measuring particles above and below this range. The angle and intensity of laser light scattered by the particles are selectively measured to permit calculation of a volume distribution using light-scattering techniques.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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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Designation: D4464 − 15
Standard Test Method for
Particle Size Distribution of Catalytic Materials by Laser
1
Light Scattering
This standard is issued under the fixed designation D4464; 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 3. Terminology
3.1 Definitions and recommended nomenclature pertaining
1.1 Thistestmethodcoversthedeterminationoftheparticle
size distribution of catalyst, catalyst carrier, and catalytic raw to catalysts and to materials used in their manufacture can be
found in Terminology D3766.
material particles and is one of several found valuable for the
measurement of particle size. The range of average particle
3.2 Definitions of Terms Specific to This Standard:
sizes investigated was from 1 to 300 µm equivalent spherical
3.2.1 background—extraneous scattering of light by mate-
diameter. The technique is capable of measuring particles
rial present in the dispersion fluid other than the particles to be
above and below this range. The angle and intensity of laser
measured. It includes scattering by contamination in the
light scattered by the particles are selectively measured to
measurement path.
permit calculation of a volume distribution using light-
3.2.2 Fraunhofer Diffraction—the optical theory that de-
scattering techniques.
scribes the low-angle scattering of light by particles that are
1.2 The values stated in SI units are to be regarded as
large compared to the wavelength of the incident light.
standard. No other units of measurement are included in this
3.2.3 Mie Scattering—the complex electromagnetic theory
standard.
that describes the scattering of light by spherical particles. It is
1.3 This standard does not purport to address all of the
applied when the sample includes particles with diameters that
safety concerns, if any, associated with its use. It is the
are close to the wavelength of the incident light. The real and
responsibility of the user of this standard to establish appro-
imaginaryindicesoflightrefractionoftheparticlesareneeded.
priate safety and health practices and determine the applica-
3.2.4 multiple scattering—the re-scattering of light by a
bility of regulatory limitations prior to use.
particle in the path of light scattered by another particle. This
usually occurs in heavy concentrations of a particle dispersion.
2. Referenced Documents
2
4. Summary of Test Method
2.1 ASTM Standards:
D3766 Terminology Relating to Catalysts and Catalysis
4.1 Aprepared sample of particulate material is dispersed in
E105 Practice for Probability Sampling of Materials
water or a compatible organic liquid and is circulated through
E177 Practice for Use of the Terms Precision and Bias in
the path of a laser light beam or some other suitable source of
ASTM Test Methods
light. The particles pass through the light beam and scatter it.
E456 Terminology Relating to Quality and Statistics
Photodetector arrays collect the scattered light which is con-
E691 Practice for Conducting an Interlaboratory Study to
verted to electrical signals to be analyzed using Fraunhofer
Determine the Precision of a Test Method
Diffraction, or Mie Scattering, or both. Scattering information,
E1617 Practice for Reporting Particle Size Characterization
typically, is analyzed assuming a spherical geometry for the
Data
particles. Calculated particle sizes are, therefore, presented as
equivalent spherical diameters.
5. Significance and Use
1
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-
5.1 It is important to recognize that the results obtained by
Mechanical Properties.
this test method or any other method for particle size determi-
Current edition approved April 1, 2015. Published May 2015. Originally
nation utilizing different physical principles may disagree. The
approved in 1985. Last previous edition approved in 2010 as D4464 – 10. DOI:
10.1520/D4464-15.
results are strongly influenced by physical principles employed
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
by each method of particle size analysis. The results of any
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
particle sizing method should be used only in a relative sense
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. andshouldnotberegardedasabsolutewhencomparingresults
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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...
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: D4464 − 10 D4464 − 15
Standard Test Method for
Particle Size Distribution of Catalytic MaterialMaterials by
1
Laser Light Scattering
This standard is issued under the fixed designation D4464; 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 test method covers the determination of the particle size distribution of catalyst, catalyst and catalyst carrier carrier,
and catalytic raw material particles and is one of several found valuable for the measurement of particle size. The range of average
particle sizes investigated was from 1 to 300 μm equivalent spherical diameter. The technique is capable of measuring particles
above and below this range. The angle and intensity of laser light scattered by the particles are selectively measured to permit
calculation of a volume distribution using light-scattering techniques.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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:
D3766 Terminology Relating to Catalysts and Catalysis
E105 Practice for Probability Sampling of Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1617 Practice for Reporting Particle Size Characterization Data
3. Terminology
3.1 Definitions and recommended nomenclature pertaining to catalysts and to materials used in their manufacture can be found
in Terminology D3766.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 background—extraneous scattering of light by material present in the dispersion fluid other than the particles to be
measured. It includes scattering by contamination in the measurement path.
3.2.2 Fraunhofer Diffraction—the optical theory that describes the low-angle scattering of light by particles that are large
compared to the wavelength of the incident light.
3.2.3 Mie Scattering—the complex electromagnetic theory that describes the scattering of light by spherical particles. It is
applied when the sample includes particles with diameters that are close to the wavelength of the incident light. The real and
imaginary indices of light refraction of the particles are needed.
3.2.4 multiple scattering—the re-scattering of light by a particle in the path of light scattered by another particle. This usually
occurs in heavy concentrations of a particle dispersion.
1
This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-Mechanical
Properties.
Current edition approved Oct. 15, 2010April 1, 2015. Published January 2011May 2015. Originally approved in 1985. Last previous edition approved in 20052010 as
D4464–00(2005).D4464 – 10. DOI: 10.1520/D4464-10.10.1520/D4464-15.
2
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4464 − 15
4. Summary of Test Method
4.1 A prepared sample of particulate material is dispersed in water or a compatible organic liquid and is circulated through the
path of a laser light beam or some other suitable source of light. The particles pass through the light beam and scatter it.
Photodetector arrays collect the scattered light which is converted to electrical signals to be analyzed using Fraunhofer Diffraction,
or Mie Scattering, or both. Scattering information, typically, is analyzed assuming a spherical geometry for the particles. Calculated
particle sizes are, therefore, presented as equivalent spherical diameters.
5. Significance and Use
5.1 It is important to
...
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