ASTM D4438-85(1997)
(Test Method)Standard Test Method for Particle Size Distribution of Catalytic Material by Electronic Counting
Standard Test Method for Particle Size Distribution of Catalytic Material by Electronic Counting
SCOPE
1.1 This test method covers the determination of particle size distribution of catalyst and catalyst carrier particles using an electroconductive sensing method and is one of several valuable methods for the measurement of particle size.
1.2 The range of particle sizes investigated was 20 to 150 μm (see IEEE/ASTM SI 10) equivalent spherical diameter. The technique is capable of measuring particles above and below this range. The instrument used for this method is an electric current path of small dimensions that is modulated by individual particle passage through an aperture, and produces individual pulses of amplitude proportional to the particle volume.
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: D 4438 – 85 (Reapproved 1997)
Standard Test Method for
Particle Size Distribution of Catalytic Material by
Electronic Counting
This standard is issued under the fixed designation D 4438; 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 4. Significance and Use
1.1 This test method covers the determination of particle 4.1 This test method can be used to determine particle size
size distribution of catalyst and catalyst carrier particles using distributions for material specifications, manufacturing control,
an electroconductive sensing method and is one of several and research and development work in the particle size range
valuable methods for the measurement of particle size. usually encountered in fluidizable cracking catalysts.
1.2 The range of particle sizes investigated was 20 to 150
5. Apparatus
μm equivalent spherical diameter. The technique is capable of
5.1 Electronic Particle Counter, with sample stand and
measuring particles above and below this range. The instru-
ment used for this method is an electric current path of small stirring motor.
5.2 Aperture Tubes, with varying diameters. The diameter
dimensions that is modulated by individual particle passage
through an aperture, and produces individual pulses of ampli- required is dependent upon the particle size distribution of the
sample. Generally, any given tube will cover a particle size
tude proportional to the particle volume.
1.3 This standard does not purport to address all of the range from 2 to 40 % of its aperture diameter.
5.3 Ultrasonic Tank, 100 W.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.4 Beaker, 100-mL.
5.5 Graduated Glass Pipet, 5-mL.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 5.6 Wash Bottles.
5.7 Membrane Filtering Device with 0.22-μm filters.
2. Referenced Documents
5.8 Round-Bottom Sample Beakers, 250-mL.
2.1 ASTM Standards: 5.9 Micro-Riffler or Chute Riffler.
D 1193 Specification for Reagent Water
6. Reagents
E 177 Practice for Use of the Terms Precision and Bias in
6.1 Purity of Reagents—Reagent grade chemicals shall be
ASTM Test Methods
E 691 Practice for Conducting an Interlaboratory Study to used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
Determine the Precision of a Test Method
tee on Analytical Reagents of the American Chemical Society,
3. Summary of Test Method
where such specifications are available. Other grades may be
3.1 A carefully dispersed, dilute suspension of the sample in used, provided it is first ascertained that the reagent is of
a beaker filled with an electrolyte is placed in the counting sufficiently high purity to permit its use without lessening the
position on the instrument sample stand. The suspension is accuracy of the determination.
forced through a restricting aperture. Each passing particle is 6.2 Purity of Water—Unless otherwise indicated, references
recorded on an electronic counter, and the data are accumulated to water shall be understood to mean reagent water conforming
according to selected particle size intervals for subsequent to Specification D 1193, Type II.
processing. 6.3 Electrolyte—Dissolve 10.0 g of reagent grade sodium
3.2 The instrument response is proportional to liquid dis- chloride (NaCl) in 1 L of distilled or deionized water and filter
placement by the particle volume. Equivalent spherical diam- twice through a 0.22-μm filter. Commercially available Elec-
eter is commonly used to express the particle size. trolyte solution of the same concentration can also be used, but
should be filtered for apertures smaller than 100 μm.
This test method is under the jurisdiction of ASTM Committee D-32 on
Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-
Mechanical Properties. “Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
Current edition approved March 18, 1985. Published May 1985. cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
Annual Book of ASTM Standards, Vol 11.01. the American Chemical Society, see “Analar Standards for Laboratory U.K.
Annual Book of ASTM Standards, Vol 14.02. Chemicals,” BDH Ltd., Poole, Dorset, and the “United States Pharmacopeia.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4438
6.4 Wash Water—Distilled or deionized water, twice filtered 7.4.6 Initiate an analysis count, and accumulate and process
through a 0.22-μm filter. Electrolyte may also be used as wash
data in accordance with the manufacturer’s instructions. For
water.
increased precision take a total of three sets of data and average
6.5 Calibration Spheres, Near monosized, having a relative
them. If the resulting data in differential volume form show
standard deviation from the mean of less than 5 % as certified
more than a few percent in the smallest active channel,
by the manufacturer.
additional data may be obtained using a smaller aperture after
large particles are scalped from the sample. Data from both
7. Procedure
apertures may then be combined, as described in the instrument
7.1 Follow instrument manufacturer’s instruction manual
manufacturer’s instruction manual, although this step is be-
for instrument settings.
yond the scope of this test method.
7.2 Follow the manufacturer’s instructions for calibrating
each aperture and electrolyte combination that will be used.
8. Presentation of
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