ASTM D4438-85(2007)
(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
SIGNIFICANCE AND USE
This test method can be used to determine particle size distributions for material specifications, manufacturing control, and research and development work in the particle size range usually encountered in fluidizable cracking catalysts.
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 m (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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Standards Content (Sample)
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Designation: D4438 − 85 (Reapproved2007)
Standard Test Method for
Particle Size Distribution of Catalytic Material by Electronic
Counting
This standard is issued under the fixed designation D4438; 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 position on the instrument sample stand. The suspension is
forced through a restricting aperture. Each passing particle is
1.1 This test method covers the determination of particle
recordedonanelectroniccounter,andthedataareaccumulated
size distribution of catalyst and catalyst carrier particles using
according to selected particle size intervals for subsequent
an electroconductive sensing method and is one of several
processing.
valuable methods for the measurement of particle size.
3.2 The instrument response is proportional to liquid dis-
1.2 The range of particle sizes investigated was 20 to 150
placement by the particle volume. Equivalent spherical diam-
µm(seeIEEE/ASTM SI 10)equivalentsphericaldiameter.The
eter is commonly used to express the particle size.
technique is capable of measuring particles above and below
this range. The instrument used for this method is an electric
4. Significance and Use
current path of small dimensions that is modulated by indi-
4.1 This test method can be used to determine particle size
vidual particle passage through an aperture, and produces
individual pulses of amplitude proportional to the particle distributionsformaterialspecifications,manufacturingcontrol,
and research and development work in the particle size range
volume.
usually encountered in fluidizable cracking catalysts.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Electronic Particle Counter, with sample stand and
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. stirring motor.
5.2 Aperture Tubes, with varying diameters. The diameter
2. Referenced Documents
required is dependent upon the particle size distribution of the
2.1 ASTM Standards:
sample. Generally, any given tube will cover a particle size
D1193 Specification for Reagent Water
range from 2 to 40 % of its aperture diameter.
E177 Practice for Use of the Terms Precision and Bias in
5.3 Ultrasonic Tank, 100 W.
ASTM Test Methods
5.4 Beaker, 100-mL.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
5.5 Graduated Glass Pipet, 5-mL.
IEEE/ASTM SI 10 Standard for Use of the International
5.6 Wash Bottles.
System of Units (SI): The Modern Metric System
5.7 Membrane Filtering Device with 0.22-µm filters.
3. Summary of Test Method
5.8 Round-Bottom Sample Beakers, 250-mL.
3.1 Acarefully dispersed, dilute suspension of the sample in
5.9 Micro-Riffler or Chute Riffler.
a beaker filled with an electrolyte is placed in the counting
6. Reagents
This test method is under the jurisdiction of ASTM Committee D32 on
6.1 Purity of Reagents—Reagent grade chemicals shall be
Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-
used in all tests. Unless otherwise indicated, it is intended that
Mechanical Properties.
all reagents shall conform to the specifications of the Commit-
Current edition approved April 1, 2007. Published April 2007. Originally
ϵ1
approved in 1985. Last previous edition approved in 2001 as D4438–85(2001) . tee onAnalytical Reagents of theAmerican Chemical Society,
DOI: 10.1520/D4438-85R07.
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 Supporting data have been filed at ASTM International Headquarters and may
the ASTM website. be obtained by requesting Research Report RR:D32-1011.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4438 − 85 (2007)
where such specifications are available. Other grades may be 7.4.3 During stirring, using a 5-mL pipet, transfer 2 mL of
used, provided it is first ascertained that the reagent is of the sample suspension (from 7.4.2) to another 250-mL round-
sufficiently high purity to permit its use without lessening the
bottom beaker containing 200 mLof clean electrolyte. Be sure
accuracy of the determination. all the contents in the pipet are transferred.
7.4.4 Remove the beaker (from 7.4.1) from the sampling
6.2 Purity of Water—Unless otherwise indicated, references
stand. Flush the outside of the aperture tube, the stirrer, and
towatershallbeunderstoodtomeanreagentwaterconforming
outer electrode. Place the sample and beaker from 7.4.3 in the
to Specification D1193, Type II.
sampling stand. Adjust the stirring blades close to the bottom
6.3 Electrolyte—Dissolve 10.0 g of reagent grade sodium
of the round-bottom beaker so that they effectively sweep the
chloride (NaCl) in 1 Lof distilled or deionized water and filter
bottom of the beaker again. Increase the stirrer speed moder-
twice through a 0.22-µm filter.
ately. Check for particle settling by visually observing the
NOTE 1—Commercially available Electrolyte solution of the same
stirring system with a flashlight and viewing the surface
concentration can also be used, but should be filtered for apertures smaller
perpendicular to the bottom. If particles are observed settling,
than 100 µm.
increase stirring rate without generating air bubbles or increase
6.4 WashWater—Distilled or deionized water, twice filtered
the electrolyte viscosity, or both.
through a 0.22-µm filter. Electrolyte may also be used as wash
NOTE 3—Electrolyte viscosity can be increased, for example, by adding
water.
filtered glycerol up to 30 % by volume.
6.5 CalibrationSpheres ,Nearmonosized,havingarelative
7.4.5 Initiate a preliminary count a
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