ASTM C690-09(2014)
(Test Method)Standard Test Method for Particle Size Distribution of Alumina or Quartz Powders by Electrical Sensing Zone Technique
Standard Test Method for Particle Size Distribution of Alumina or Quartz Powders by Electrical Sensing Zone Technique
SIGNIFICANCE AND USE
3.1 This test method is useful to both sellers and purchasers of alumina and quartz powders for determining particle size distributions for materials specifications, manufacturing control, and development and research.
SCOPE
1.1 This test method, one of several found valuable for the measurement of particle size, covers the determination of the particle size distribution of alumina or quartz powders (0.6 to 56.0 μm) using electrical sensing zone particle size analyzers. These instruments use an electric current path of small dimensions which is modulated by individual particle passage through an aperture, and produces individual pulses of amplitude proportional to the particle volume.
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 problems, 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: C690 − 09 (Reapproved 2014)
Standard Test Method for
Particle Size Distribution of Alumina or Quartz Powders by
Electrical Sensing Zone Technique
This standard is issued under the fixed designation C690; 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* 4. Apparatus
1.1 This test method, one of several found valuable for the 4.1 Electrical Sensing Zone Particle Counter.
measurement of particle size, covers the determination of the
4.2 Aperture Tubes, diameter ranging from approximately
particle size distribution of alumina or quartz powders (0.6 to
30 to 140 µm. The diameter required is dependent upon the
56.0 µm) using electrical sensing zone particle size analyzers.
particle size distribution of the sample. Generally any given
These instruments use an electric current path of small dimen-
tube will cover a particle size range from 2 to 60 % of its
sions which is modulated by individual particle passage
aperture diameter.
through an aperture, and produces individual pulses of ampli-
NOTE 1—In certain cases, apertures up to 300 µm are usable.
tude proportional to the particle volume.
4.3 Sample Beaker, capable of maintaining all particles
1.2 The values stated in SI units are to be regarded as
uniformly in suspension (for example, round-bottom).
standard. No other units of measurement are included in this
standard.
4.4 Blender,capacity1-Lglasscontainer.Ameanstocontrol
speed is required.
1.3 This standard does not purport to address all of the
safety problems, if any, associated with its use. It is the
4.5 Beakers, 100, 500, and 1000-mL.
responsibility of the user of this standard to establish appro-
4.6 Pipet.
priate safety and health practices and determine the applica-
4.7 Wash Bottles.
bility of regulatory limitations prior to use.
4.8 Membrane Filtering Device, rated at 0.45-µm filters or
2. Summary of Test Method
finer.
2.1 A carefully dispersed, dilute suspension of the powder
5. Reagents
inabeakerfilledwithanelectrolyteisplacedontheinstrument
sample stand. The suspension is forced through a restricting
5.1 Purity of Reagents—Reagent grade chemicals shall be
aperture. Each particle passing generates an electric pulse that
used in all tests. Unless otherwise indicated, it is intended that
is recorded on an electronic counter.
all reagents shall conform to the specifications of the Commit-
2.2 The instrument response is essentially related to particle tee onAnalytical Reagents of theAmerican Chemical Society,
volume (liquid displacement). Equivalent spherical diameter is where such specifications are available. Other grades may be
commonly used to express the particle size. (Comparisons with used, provided it is first ascertained that the reagent is of
other techniques have been found to be good for spherical sufficiently high purity to permit its use without lessening the
particles; for non-spherical particles results may differ.) accuracy of the determination.
5.2 Dispersing Media—Ten percent solution of purified or
3. Significance and Use
reagent grade sodium hexametaphosphate in distilled water
3.1 This test method is useful to both sellers and purchasers
twice filtered through the membrane filtering device.
of alumina and quartz powders for determining particle size
NOTE 2—Deionized water may be substituted for distilled water.
distributions for materials specifications, manufacturing
NOTE 3—This liquid should not be retained longer than 1 month and
control, and development and research.
should not be pH modified or heated.
ThistestmethodisunderthejurisdictionofASTMCommitteeC21onCeramic
Whitewares and Related Productsand is the direct responsibility of Subcommittee Reagent Chemicals, American Chemical Society Specifications , American
C21.04 on Raw Materials. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved Dec. 1, 2014. Published December 2014. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
approved in 1971. Last previous edition approved in 2009 as C690 – 09. DOI: Chemicals, VWR International Ltd., U.K., and the United States Pharmacopoeia,
10.1520/C0690-09R14. USPC, Rockville, MD.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C690 − 09 (2014)
5.3 Electrolyte—Dissolve 10.0 g of reagent grade sodium 6.6 Place the sample beaker in position on the sample stand.
chloride (NaCl) in 1000 mL of distilled water and filter twice
6.7 Adjust the speed of the stirrer to furnish sufficient
through the membrane filtering device.
agitation to maintain a uniform particle suspension, but below
5.4 Wash Water—Distilled water twice filtered through the air bubble generation speeds.
membrane filtering device.
6.8 Use the apparatus control software to set the measure-
5.5 Calibration Particles—NIST or NIST traceable mono- ment parameters. Make three measurements in which each
sized particle standards. measurement counts and measures at least 5000 particles.
Average the particle size distribution from the three measure-
6. Procedure
ments and report the statistical parameters from the averaged
6.1 Summary—Disperse the test powder in the electrolyte results.
with a blender. Transfer a representative portion to the sample
6.9 Precautions:
beaker that contains filtered electrolyte. Place sample beaker in
6.9.1 Before each analysis, using wash bottle and filtered
the apparatus and obtain particle size distribution in a chosen
wash water, wash all surfaces coming in contact with sample.
size range. Obtain relative weight fraction by assuming con-
6.9.2 Ensure that the calibration of the instrument is correct
stant particle density.
by checking the calibration factor at least once a week.
6.9.3 The number of particles per unit volume in the sample
6.2 Precalibrate the aperture and electrolyte combination
followi
...
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: C690 − 09 C690 − 09 (Reapproved 2014)
Standard Test Method for
Particle Size Distribution of Alumina or Quartz Powders by
Electrical Sensing Zone Technique
This standard is issued under the fixed designation C690; 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, one of several found valuable for the measurement of particle size, covers the determination of the particle
size distribution of alumina or quartz powders (0.6 to 56.0 μm) using electrical sensing zone particle size analyzers. These
instruments use an electric current path of small dimensions which is modulated by individual particle passage through an aperture,
and produces individual pulses of amplitude proportional to the particle volume.
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 problems, 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. Summary of Test Method
2.1 A carefully dispersed, dilute suspension of the powder in a beaker filled with an electrolyte is placed on the instrument
sample stand. The suspension is forced through a restricting aperture. Each particle passing generates an electric pulse that is
recorded on an electronic counter.
2.2 The instrument response is essentially related to particle volume (liquid displacement). Equivalent spherical diameter is
commonly used to express the particle size. (Comparisons with other techniques have been found to be good for spherical particles;
for non-spherical particles results may differ.)
3. Significance and Use
3.1 This test method is useful to both sellers and purchasers of alumina and quartz powders for determining particle size
distributions for materials specifications, manufacturing control, and development and research.
4. Apparatus
4.1 Electrical Sensing Zone Particle Counter.
4.2 Aperture Tubes, diameter ranging from approximately 30 to 140 μm. The diameter required is dependent upon the particle
size distribution of the sample. Generally any given tube will cover a particle size range from 2 to 60 % of its aperture diameter.
NOTE 1—In certain cases, apertures up to 300 μm are usable.
4.3 Sample Beaker, capable of maintaining all particles uniformly in suspension (for example, round-bottom).
4.4 Blender, capacity 1-L glass container. A means to control speed is required.
4.5 Beakers, 100, 500, and 1000-mL.
4.6 Pipet.
4.7 Wash Bottles.
4.8 Membrane Filtering Device, rated at 0.45-μm filters or finer.
This test method is under the jurisdiction of ASTM Committee C21 on Ceramic Whitewares and Related Productsand is the direct responsibility of Subcommittee C21.04
on Raw Materials.
Current edition approved Feb. 15, 2009Dec. 1, 2014. Published February 2009December 2014. Originally approved in 1971. Last previous edition approved in 20032009
as C690 – 03.C690 – 09. DOI: 10.1520/C0690-09.10.1520/C0690-09R14.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C690 − 09 (2014)
5. Reagents
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
5.2 Dispersing Media—Ten percent solution of purified or reagent grade sodium hexametaphosphate in distilled water twice
filtered through the membrane filtering device.
NOTE 2—Deionized water may be substituted for distilled water.
NOTE 3—This liquid should not be retained longer than 1 month and should not be pH modified or heated.
5.3 Electrolyte—Dissolve 10.0 g of reagent grade sodium chloride (NaCl) in 1000 mL of distilled water and filter twice through
the membrane filtering device.
5.4 Wash Water—Distilled water twice filtered through the membrane filtering device.
5.5 Calibration Particles—NIST or NIST traceable monosized particle standards.
6. Procedure
6.1 Summary—Disperse the test powder in the electrolyte with a blender. Transfer a representative portion to the sample beaker
that contains filtered electrolyte. Place sample beaker in the apparatus and obtain particle size distribution in a chosen size range.
Obtain relative weight fraction by assuming constant particle density.
6.2 Precalibrate the aperture and electrolyte combination following the manufacturer’s instruction manual.
NOTE 4—Calibration should be performed in accordance with the instruction manual. Monosized NIST or NIST traceable calibration standards should
be selected from Fig. A1.1. Mutual agreement on the source and size of calibration standards is necessary for interlaboratory comparisons.
6.3 Check background counts by filling the sample beaker with filtered electrolyte and taking counts without any sample added.
Follow 6.6, 6.7, and 6.8.
6.4 Disperse approximately 0.7 g of sample in 200 mL of electrolyte containing 5 drops of dispersing media, by mixing at high
speed on the blender or its equivalent for 5 min.
NOTE 5—The proper dispersion conditions for a given mixer or blender should be predetermined by obtaining a time-speed versus median diameter
curve (see typical curve in Fig. A1.2) while ensuring that grinding does not occur. The position of the plateau will indicate the proper dispersion conditions
for the sample. Experience has shown that full speed on th
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