ASTM C1182-09(2014)
(Test Method)Standard Test Method for Determining the Particle Size Distribution of Alumina by Centrifugal Photosedimentation
Standard Test Method for Determining the Particle Size Distribution of Alumina by Centrifugal Photosedimentation
SIGNIFICANCE AND USE
5.1 Manufacturers and users of alumina powders will find this test method useful to determine the particle size distribution of these materials for product specification, quality control, and research and development testing.
SCOPE
1.1 This test method covers the determination of the particle size distribution of alumina in the range from 0.1 to 20 μm having a median particle diameter from 0.5 to 5.0 μm.
1.2 The procedure described in this test method may be successfully applied to other ceramic powders in this general size range. It is the responsibility of the user to determine the applicability of this test method to other material.
1.3 The values stated in SI units are to regarded as the standard. The values given in parentheses are for information only.
1.4 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: C1182 − 09 (Reapproved 2014)
Standard Test Method for
Determining the Particle Size Distribution of Alumina by
Centrifugal Photosedimentation
This standard is issued under the fixed designation C1182; 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. Summary of Test Method
4.1 A homogeneous aqueous dispersion of the powder is
1.1 This test method covers the determination of the particle
prepared. While kept in a thoroughly mixed condition, a small
size distribution of alumina in the range from 0.1 to 20 µm
aliquot is transferred to the analyzer sample cell, which is
having a median particle diameter from 0.5 to 5.0 µm.
placed in the instrument and subjected to a controlled centrifu-
1.2 The procedure described in this test method may be
gal acceleration at a known or controlled temperature. At
successfully applied to other ceramic powders in this general
predetermined times related to the sedimentation of specific
size range. It is the responsibility of the user to determine the
Stokes’ diameters (Note 1), the optical absorbance is recorded
applicability of this test method to other material.
and ratioed to the initial value to determine the fraction of the
1.3 The values stated in SI units are to regarded as the
total sample that has sedimented a specific distance.Avolume
standard. The values given in parentheses are for information
based size distribution is calculated from the absorbance-time
only.
data. Since alumina particles are not truly spherical, the results
are reported as equivalent diameters (spherical) (Note 2).
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
NOTE 1—This diameter in micrometres is referred to as D in the
responsibility of the user of this standard to establish appro-
equation:
priate safety and health practices and determine the applica-
18 n ~H/t!
2 8
bility of regulatory limitations prior to use. D 5 310 (1)
ρ 2 ρ u
~ !
s f
where:
2. Referenced Documents
2 n = viscosity of the fluid, P,
2.1 ASTM Standards:
H = height of the settling particles, cm,
C242 Terminology of Ceramic Whitewares and Related
t = time for particle to settle, s,
Products
ρ = particle density, g/cm ,
s
E691 Practice for Conducting an Interlaboratory Study to
ρ = fluid density, g/cm , and
f
Determine the Precision of a Test Method
u = the rotational velocity, cm/s.
E177 Practice for Use of the Terms Precision and Bias in
NOTE 2—Refer to Terminology C242 for the ASTM definition of this
ASTM Test Methods
term. Most equipment manufacturers refer to this as the equivalent
spherical diameter.
3. Terminology
4.2 The instruments that have been found suitable for this
test method incorporate microcomputers that control instru-
3.1 Definitions:
ment operation and perform all required data acquisition and
3.1.1 Refer to Terminology C242 for definitions of terms
computation functions.
used in this test method.
5. Significance and Use
5.1 Manufacturers and users of alumina powders will find
ThistestmethodisunderthejurisdictionofASTMCommitteeC21onCeramic
this test method useful to determine the particle size distribu-
Whitewares and Related Products and is the direct responsibility of Subcommittee
C21.04 on Raw Materials.
tion of these materials for product specification, quality
Current edition approved Dec. 1, 2014. Published December 2014. Originally
control, and research and development testing.
approved in 1991. Last previous edition approved in 2009 as C1182 – 09. DOI:
10.1520/C1182-09R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Apparatus
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Centrifugal Particle Size Distribution Analyzer—The
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. analyzer shall incorporate a centrifuge capable of subjecting a
*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
C1182 − 09 (2014)
homogeneous dispersion of the sample to centrifugal accelera- mLof 0.1 % sodium hexametaphosphate solution and mix well
tion in specially designed sample cells. A collimated beam of by stirring. Disperse by either of the following methods:
visible light (either monochromatic or broad-band) shall tra- 8.1.1.1 Ultrasonic Bath—Place the beaker in the bath with
verse the sample cell at a defined distance from the top of the the bottom of the beaker suspended above the bottom of the
cell. The change in photo extinction resulting from sedimen- bath. In the ideal position, the top of the fluid in the beaker is
tation of the sample shall be measured by a photo detector and even with the liquid level in the bath. Apply ultrasonic energy
appropriate electronic circuits, and used to calculate the for 15 min with frequent stirring. Remove beaker from bath.
volume-based sized distribution of the sample. 8.1.1.2 Ultrasonic Probe—Insert the probe into the beaker
containing the sample and apply power for 30 s. Make sure the
6.2 Ultrasonic Probe, consisting of power unit, ultrasonic
sample is well suspended during this step. Remove probe from
transducer, and 13-mm ( ⁄2-in.) diameter probe, 200 to 250 W.
the beaker.
6.3 UltrasonicWaterBath,powerdensityapproximately0.3
8.1.2 Add a 25-mm (1-in.) stirring bar to the beaker and
2 2
W/cm (2 W/in. ).
place on a magnetic stirrer. Stir for approximately 3 min in a
6.4 Balance, top-loading, accurate to 60.1 g. cold water bath to bring the sample to ambient temperature.
Continue stirring at constant temperature.
6.5 Stirrer, magnetic, with 25-mm (1-in.) and 19-mm ( ⁄4-
in.) stirring bars. NOTE 4—The concentration of the sample may require dilution with
0.1 % sodium hexametaphosphate solution to meet the optical absorbance
6.6 Thermometer, 0 to 50°C, accurate to 0.5°C. May also be
tolerance specified in the instrument operating manual. Thorough mixing
an electronic temperature measuring device, properly
must accompany any dilution of the sample.
calibrated, that meets the given specifications.
8.2 Analyzer Preparation:
6.7 Sample Cells, as supplied by the instrument manufac-
8.2.1 To warm up the analyzer, apply power a minimum of
turer.
10 min prior to testing. Conduct the warm-up with the sample
compartment closed. Make certain that ventilation airflow is
7. Reagents
not restricted by adjacent equipment, papers, or other materi-
als. Check the printer to ensure a sufficient supply of paper.
7.1 Purity of Reagents—Reagent grade chemicals shall be
Clean a pair of sample cells and caps, rinse with the 0.1 %
used in all tests. Unless otherwise indicated, it is intended that
sodium hexametaphosphate solution and store inverted on
all reagents shall conform to the specifications of
...
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: C1182 − 09 C1182 − 09 (Reapproved 2014)
Standard Test Method for
Determining the Particle Size Distribution of Alumina by
Centrifugal Photosedimentation
This standard is issued under the fixed designation C1182; 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 alumina in the range from 0.1 to 20 μm having
a median particle diameter from 0.5 to 5.0 μm.
1.2 The procedure described in this test method may be successfully applied to other ceramic powders in this general size range.
It is the responsibility of the user to determine the applicability of this test method to other material.
1.3 The values stated in SI units are to regarded as the standard. The values given in parentheses are for information only.
1.4 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
2.1 ASTM Standards:
C242 Terminology of Ceramic Whitewares and Related Products
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
3. Terminology
3.1 Definitions:
3.1.1 Refer to Terminology C242 for definitions of terms used in this test method.
4. Summary of Test Method
4.1 A homogeneous aqueous dispersion of the powder is prepared. While kept in a thoroughly mixed condition, a small aliquot
is transferred to the analyzer sample cell, which is placed in the instrument and subjected to a controlled centrifugal acceleration
at a known or controlled temperature. At predetermined times related to the sedimentation of specific Stokes’ diameters (Note 1),
the optical absorbance is recorded and ratioed to the initial value to determine the fraction of the total sample that has sedimented
a specific distance. A volume based size distribution is calculated from the absorbance-time data. Since alumina particles are not
truly spherical, the results are reported as equivalent diameters (spherical) (Note 2).
NOTE 1—This diameter in micrometres is referred to as D in the equation:
18 n ~H/t!
2 8
D 5 310 (1)
ρ 2 ρ u
~ !
s f
where:
n = viscosity of the fluid, P,
H = height of the settling particles, cm,
t = time for particle to settle, s,
This test method is under the jurisdiction of ASTM Committee C21 on Ceramic Whitewares and Related Products and is the direct responsibility of Subcommittee C21.04
on Raw Materials.
Current edition approved Jan. 1, 2009Dec. 1, 2014. Published February 2009December 2014. Originally approved in 1991. Last previous edition approved in 20072009
as C1182–91(2007).C1182 – 09. DOI: 10.1520/C1182-09.10.1520/C1182-09R14.
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.
*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
C1182 − 09 (2014)
ρ = particle density, g/cm ,
s
ρ = fluid density, g/cm , and
f
u = the rotational velocity, cm/s.
NOTE 2—Refer to Terminology C242 for the ASTM definition of this term. Most equipment manufacturers refer to this as the equivalent spherical
diameter.
4.2 The instruments that have been found suitable for this test method incorporate microcomputers that control instrument
operation and perform all required data acquisition and computation functions.
5. Significance and Use
5.1 Manufacturers and users of alumina powders will find this test method useful to determine the particle size distribution of
these materials for product specification, quality control, and research and development testing.
6. Apparatus
6.1 Centrifugal Particle Size Distribution Analyzer—The analyzer shall incorporate a centrifuge capable of subjecting a
homogeneous dispersion of the sample to centrifugal acceleration in specially designed sample cells. A collimated beam of visible
light (either monochromatic or broad-band) shall traverse the sample cell at a defined distance from the top of the cell. The change
in photo extinction resulting from sedimentation of the sample shall be measured by a photo detector and appropriate electronic
circuits, and used to calculate the volume-based sized distribution of the sample.
6.2 Ultrasonic Probe, consisting of power unit, ultrasonic transducer, and 13-mm ( ⁄2-in.) diameter probe, 200 to 250 W.
2 2
6.3 Ultrasonic Water Bath, power density approximately 0.3 W/cm (2 W/in. ).
6.4 Balance, top-loading, accurate to 60.1 g.
6.5 Stirrer, magnetic, with 25-mm (1-in.) and 19-mm ( ⁄4-in.) stirring bars.
6.6 Thermometer, 0 to 50°C, accurate to 0.5°C. May also be an electronic temperature measuring device, properly calibrated,
that meets the given specifications.
6.7 Sample Cells, as supplied by the instrument manufacturer.
7. Reagents
7.1 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 precision of the determination.
7.2 Sodium Hexametaphosphate Solution , 0.1 %—Tare a 50-mL beaker on the balance. Weigh 1.0 6 0.1 g of sodium
hexametaphosphate into the beaker. Add 30 to 40 mL of distilled or deionized water and dissolve the salt. Pour the solution into
the volumetric flask, rinse the beaker twice with water, and pour into the flask. Make up the volume to 1000 mL and mix
thoroughly. Store in a stoppered glass or polyethylene reagent bottle labeled with the contents and date of preparation. Discard any
solution after six weeks of storage.
NOTE 3—These reagents are adequate to cover the range of samples up to a maximum diameter of 20 μm.
8. Procedure
8.1 Sample Preparation and Dispersion :
8.1.1 Withdraw approximately 1 g of a thoroughly mixed powdered sample (or an equivalent amount of a slurried sample) and
place into a 250-mL beaker. If the sample is received in a plastic or glass vial containing about 1 g (60.25 g), transfer the entire
contents to the 250-mL beaker. Add 200 mL of 0.1 % sodium hexametaphosphate solution and mix well by stirring. Disperse by
either of the following methods:
8.1.1.1 Ultrasonic Bath—Place the beaker in the bath
...
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