ASTM E159-00
(Test Method)Standard Test Method for Hydrogen Loss of Cobalt, Copper, Tungsten, and Iron Powders
Standard Test Method for Hydrogen Loss of Cobalt, Copper, Tungsten, and Iron Powders
SCOPE
1.1 This test method covers the determination of oxygen due to the presence of hydrogen-reducible oxides in copper, tungsten, and iron powders. This test method consists of subjecting a sample of powder to the action of a hydrogen-containing gas under standard conditions of temperature and time and measuring the resulting loss of weight. This test method is useful for copper and iron powders in the range from 0.05 to 3.0% oxygen and for tungsten powder in the range from 0.01 to 0.50% oxygen. This test method does not measure the oxygen contained in oxides such as silicon oxide (SiO2), aluminum oxide (Al2O3), magnesium oxide (MgO), calcium oxide (CaO), titanium dioxide (TiO2), etc. that are not reduced by hydrogen at the test temperatures. For total oxygen content, vacuum or inert gas fusion methods are available.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information only.
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:E159–00
Standard Test Method for
Hydrogen Loss of Cobalt, Copper, Tungsten, and Iron
Powders
This standard is issued under the fixed designation E159; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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. Terminology
1.1 Thistestmethodcoversthedeterminationofthemassof 3.1 Definitions—Definitions of powder metallurgy terms
hydrogen-reducible constituents in the following metal pow- can be found in Terminology B243. Additional descriptive
ders: cobalt, copper, iron, and tungsten. This test method information on powder metallurgy is available in the Related
consists of subjecting a sample of powder to the action of a Material section of Vol 02.05 of the Annual Book of ASTM
hydrogen-containinggasunderstandardconditionsoftempera- Standards.
ture and time and measuring the resulting loss of mass. This
4. Significance and Use
testmethodisusefulforcobalt,copper,andironpowdersinthe
4.1 The oxygen content of a powder affects both its green
range from 0.05 to 3.0% oxygen and for tungsten powder in
the range from 0.01 to 0.50% oxygen. This test method does and sintered properties.
4.2 Hydrogen loss is a term widely used in the powder
not measure the oxygen contained in oxides such as silicon
oxide (SiO ), aluminum oxide (Al O ), magnesium oxide metallurgy industry even though the measurement represents
2 2 3
an approximate oxygen content of the powder.
(MgO), calcium oxide (CaO), titanium dioxide (TiO ), and so
forththatarenotreducedbyhydrogenatthetesttemperatures. 4.3 Oxygen is the most common hydrogen-reducible con-
stituent of the metal powders, and this procedure may be used
For total oxygen content, vacuum or inert gas fusion methods
are available. as a measure of oxygen, reducible under test conditions, if
other interfering elements are absent.
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are provided for
5. Interferences
information only.
5.1 If carbon or sulfur, or both, is present, they will be
1.3 This standard does not purport to address all of the
largelyremovedinthetest.Theirlossinmassisincludedinthe
safety concerns, if any, associated with its use. It is the
total loss in mass measurement and must be subtracted from
responsibility of the user of this standard to establish appro-
the total mass loss.
priate safety and health practices and determine the applica-
5.2 If metals or compounds are present that vaporize at the
bility of regulatory limitations prior to use.
test temperature (such as cadmium, lead, zinc, and so forth),
2. Referenced Documents
their effect is included in the loss of mass measurement and
must be subtracted from the total mass loss.
2.1 ASTM Standards:
B215 Practices for Sampling Finished Lots of Metal Pow- 5.3 If some components are present that are oxidized or
hydrided during the test, there is a gain in mass that must be
ders
B243 Terminology of Powder Metallurgy added to the total mass loss.
E691 Practice for Conducting an Interlaboratory Study to
3 6. Apparatus
Determine the Precision of a Test Method
6.1 Furnace, capable of operating at the prescribed tem-
perature.
1 6.2 Temperature Control, capable of maintaining tempera-
This test method is under the jurisdiction of ASTM Committee B09 on Metal
tures to 615°C (627°F).
Powders and Metal Powder Products and is the direct responsibility of Subcom-
mittee B09.02 on Base Metal Powders.
6.3 Gastight Ceramic or Metallic Combustion Tube.
Current edition approved Oct. 10, 2000. Published January 2001. Originally
6.4 Flow Meter, to measure flow of hydrogen.
published as E159–86. Last previous edition E159–98.
6.5 Supply of Hydrogen and Nitrogen, having dew point
Annual Book of ASTM Standards, Vol 02.05.
Annual Book of ASTM Standards, Vol 14.02. lower than −40°C (−40°F).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E159
6.6 Combustion Boat, composed of abundum, quartz, or 9.5 At the end of the prescribed time, discontinue the flow
nickel, depending on test conditions. The boat shall be of such of hydrogen and restart the flow of nitrogen into the tube.
dimensions,forexample75mmlongand12mmwide,thatthe
9.6 Afternitrogenhasbeenflowingthroughthecombustion
thickness of powder, when uniformly distributed, does not
tube for at least 1 min, open the tube and withdraw the boat
exceed 3 mm ( ⁄8 in.).
undernitrogenatmospheretothecoolerpartofthecombustion
6.7 Balance, suitable for determining mass to the nearest
tube.
0.001 g.
9.7 Allow the specimen to cool in the nitrogen atmosphere
for 15 to 30 min, then remove the specimen from the tube and
7. Reagents
permit it to cool to room temperature in a desiccator.
7.1 Purity of Reagents—Reagent grade chemicals shall be
9.8 Whentheboathascooledtoroomtemperature,reweigh
used in all tests. Unless otherwise indicated, it is intended that
it to the nearest 0.001 g.
all reagents shall conform to the specifications of the Commit-
9.9 Alternative Test Method—The following alternative test
tee onAnalytical Reagents of theAmerican Chemical Society,
method may be used satisfactorily if the use of nitrogen is
where such specifications are available. Other grades may be
impractical.
used, provided it is first ascertained that the reagent is of
9.9.1 Bring the furnace with the combustion tube inserted
sufficiently high purity to permit its use without lessening the
up to the prescribed temperature.
accuracy of the determination.
9.9.2 Spread the test specimen to a uniform depth in the
7.2 Dissociated Ammonia, having a dew point better
preweighed combustion boat. The depth of powder in the boat
than−40°C (−40°F). May be used interchangeably with 7.3.
should be approximately 3 mm ( ⁄8 in.). Then weigh the boat
7.3 Hydrogen, having an oxygen content less than 20 ppm
and specimen to the nearest 0.001 g.
and a dew point lower than −40°C (−40°F).
9.9.3 Placetheboatcontainingthespecimeninthecombus-
7.4 Nitrogen, having an oxygen content less than 20 ppm
tion tube through
...
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