ASTM D4464-00

Standard Test Method for Particle Size Distribution of Catalytic Material by Laser Light Scattering

SCOPE
1.1 This test method covers the determination of the particle size distribution of catalyst and catalyst carrier particles and is one of several found valuable for the measurement of particle size. The range of particle sizes investigated was 20 to 150-[mu]m 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 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Apr-2000
• ICS: 19.120 - Particle size analysis. Sieving
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.02 - Physical-Mechanical Properties

Relations

• Replaced By: ASTM D4464-00(2005) - Standard Test Method for Particle Size Distribution of Catalytic Material by Laser Light Scattering
• Effective Date: 01-Oct-2005
• Referred By: ASTM D5675-13(2018) - Standard Classification for Low Molecular Weight PTFE and FEP Micronized Powders
• Effective Date: 10-Apr-2000
• Referred By: ASTM D4441-20 - Standard Specification for Aqueous Dispersions of Polytetrafluoroethylene
• Effective Date: 10-Apr-2000
• Referred By: ASTM E3268-21 - Standard Guide for NAPL Mobility and Migration in Sediment—Sample Collection, Field Screening, and Sample Handling
• Effective Date: 10-Apr-2000
• Referred By: ASTM E3163-18 - Standard Guide for Selection and Application of Analytical Methods and Procedures Used during Sediment Corrective Action
• Effective Date: 10-Apr-2000
• Referred By: ASTM D8393-21 - Standard Guide for Determination of Pore Volume of Powdered Catalysts and Catalyst Carriers by Water Adsorption
• Effective Date: 10-Apr-2000

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4464–00
Standard Test Method for
Particle Size Distribution of Catalytic Material by Laser Light
Scattering
This standard is issued under the fixed designation D 4464; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.2.2 Fraunhofer Diffraction—the optical theory that de-
scribes the low-angle scattering of light by particles that are
1.1 Thistestmethodcoversthedeterminationoftheparticle
large compared to the wavelength of the incident light.
size distribution of catalyst and catalyst carrier particles and is
3.2.3 Mie Scattering—the complex electromagnetic theory
one of several found valuable for the measurement of particle
that describes the scattering of light by spherical particles. It is
size. The range of particle sizes investigated was 30 to 300 µm
usually applied to particles with diameters that are close to the
equivalent spherical diameter. The technique is capable of
wavelength of the incident light. The real and imaginary
measuring particles above and below this range. The angle and
indices of light refraction of the particles are needed.
intensity of laser light scattered by the particles are selectively
3.2.4 multiple scattering—the re-scattering of light by a
measured to permit calculation of a volume distribution using
particle in the path of light scattered by another particle. This
light-scattering techniques.
usually occurs in heavy concentrations of a particle dispersion.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Aprepared sample of particulate material is dispersed in
priate safety and health practices and determine the applica-
water or a compatible organic liquid and is circulated through
bility of regulatory limitations prior to use.
the path of a laser light beam or some other suitable source of
2. Referenced Documents light. The particles pass through the light beam and scatter it.
Photodetector arrays collect the scattered light which is con-
2.1 ASTM Standards:
verted to electrical signals to be analyzed using Fraunhofer
D 3766 Terminology Relating to Catalysts and Catalysis
Diffraction, or Mie Scattering, or both. Scattering information,
E 105 Practice for Probability Sampling of Materials
typically, is analyzed assuming a spherical geometry for the
E 177 Practice for Use of the Terms Precision and Bias in
particles. Calculated particle sizes are, therefore, presented as
ASTM Test Methods
equivalent spherical diameters.
E 456 Terminology Relating to Quality and Statistics
E 691 Practice for Conducting an Interlaboratory Study to
5. Significance and Use
Determine the Precision of a Test Method
5.1 It is important to recognize that the results obtained by
E 1617 Practice for Reporting Particle Size Characteriza-
3 this test method or any other method for particle size determi-
tion Data
nation utilizing different physical principles may disagree. The
3. Terminology results are strongly influenced by physical principles employed
by each method of particle size analysis. The results of any
3.1 Definitions and recommended nomenclature pertaining
particle sizing method should be used only in a relative sense
to catalysts and to materials used in their manufacture can be
and should not be regarded as absolute when comparing results
found in Terminology D 3766.
obtained by other methods.
3.2 Definitions of Terms Specific to This Standard:
5.2 Light scattering theories (Fraunhofer Diffraction and
3.2.1 background—extraneous scattering of light by mate-
Mie Scattering ) that are used for determination of particle size
rial present in the dispersion fluid other than the particles to be
has been available for many years. Several manufacturers of
measured. It includes scattering by contamination in the
testing equipment now have units based on these principles.
measurement path.
Although each type of testing equipment utilizes the same
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. Born, M., andWolf, E., Principles of Optics, Chptr 8, Pergamon Press, Oxford,
Current edition approved Apr. 10, 2000. Published June 2000. 1957.
2 5
Annual Book of ASTM Standards, Vol 05.05. van Hulst, H.C., Light Scattering by Small Particles, Chptr 9, John Wiley &
Annual Book of ASTM Standards, Vol 14.02. Sons, New York, 1908.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4464–00
basic principles for light scattering as a function of particle 8.2 The use of surfactant(s) is often recommended by
size, different assumptions pertinent to application of the equipmentmanufacturers.However,agentssuchassurfactants,
theory and different models for converting light measurements antifoams,andviscositymodifiersshouldbeusedwithcaution.
to particle size, may lead to different results for each instru- An interlaboratory study of this test method showed that the
ment. Furthermore, any particles which are outside the size use of different types and concentrations of surfactant can
measurement range of the instrument will be ignored, causing significantly affect the results. In calculating the precision of
an increase in the reported percentages within the detectable this test method, results obtained using surfactants were
range. A particle size distribution which ends abruptly at the excluded because they contributed disproportionately to the
detection limit of the instrument may indicate that particles scatter in results. Comparisons between laboratories should be
outsidetherangearepresent.Therefore,useofthistestmethod performed with liquid carriers which are identical in all
cannot guarantee directly comparable results from different respects.
types of instruments.
9. Sampling and Sample Size
5.3 This test method can be used to determine particle size
distributions of catalysts and supports for materials specifica-
9.1 Arepresentative test sample shall be obtained according
tions, manufacturing control, and research and development
to Practice E 105. The test portion shall be extracted from the
work.
test sample using a micro sample splitter according to Manual
32. Quartering shall not be used.
6. Interferences
9.2 Refer to the equipment manufacturer’s recommendation
6.1 Air bubbles entrained in the circulating fluid will scatter to ensure that the amount of the test portion is acceptable to
light and then be reported as particles. Circulating fluids, achieve optimum light scattering conditions. A wide range of
typically, do not require degassing, but should be bubble-free sample portions is acceptable depending upon median particle
on visual inspections. size, particle density, and the sample delivery system.
6.2 Contaminants, such as non-aqueous solvents, oil or 9.3 For liquid dispersed materials, redisperse as necessary
ot
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