ASTM C1408-98(2004)
(Test Method)Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
SIGNIFICANCE AND USE
Uranium dioxide is used as a nuclear-reactor fuel. Gadolinium oxide is used as an additive to uranium dioxide. In order to be suitable for this purpose, these materials must meet certain criteria for impurity content. This test method is designed to determine whether the carbon content meets Specifications C 753, C 776, C 888, and C 922.
SCOPE
1.1 This test method covers the determination of carbon in nuclear-grace uranium oxide powders and pellets to determine compliance with specifications.
1.2 Gadolinium oxide (Gd2O3) and gadolinium oxide-uranium oxide powders and pellets may also be analyzed using this test method.
1.3 This test method covers the determination of 5 to 500 µg of residual carbon.
1.4 This test method describes an induction furnace carrier gas combustion system equipped with an infrared detector. It may also be applied to a similar instrument equipped with a thermal conductivity detector.
1.5 The preferred system of units is micrograms carbon per gram of uranium (µg/g U).
1.6 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.
General Information
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Standards Content (Sample)
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Designation:C1408–98 (Reapproved 2004)
Standard Test Method for
Carbon (Total) in Uranium Oxide Powders and Pellets By
Direct Combustion-Infrared Detection Method
This standard is issued under the fixed designation C 1408; 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 C 922 Specification for Sintered Gadolinium Oxide-
Uranium Dioxide Pellets
1.1 This test method covers the determination of carbon in
nuclear-grade uranium oxide powders and pellets to determine
3. Summary of Test Method
compliance with specifications.
3.1 The powered or crushed test specimen and an appropri-
1.2 Gadolinium oxide (Gd O ) and gadolinium oxide-
2 3
ate accelerator (metal flux) are added to a crucible, placed
uranium oxide powders and pellets may also be analyzed using
within an induction-heated furnace and burned at a nominal
this test method.
temperature of 1600 to 1700°C in a stream of oxygen. A
1.3 Thistestmethodcoversthedeterminationof5to500µg
catalyst converts the carbon monoxide (CO) to carbon dioxide
of residual carbon.
(CO ) and the products of combustion are scavenged free of
1.4 This test method describes an induction furnace carrier
sulfur compounds, halogens, and water vapor. The CO is
gas combustion system equipped with an infrared detector. It
swept into an infrared cell detector. The amount of carbon is
may also be applied to a similar instrument equipped with a
automatically determined from stored calibration data, and is
thermal conductivity detector.
displayed or printed out, or both, by the carbon analyzer.
1.5 The preferred system of units is micrograms carbon per
3.2 The actual configuration of the system may vary with
gram of sample (µg/g sample) or micrograms carbon per gram
vendor and model. Typical systems include columns of mate-
of uranium (µg/g U).
rials such as copper oxide, platinized silica gel, magnesium
1.6 This standard does not purport to address all of the
perchlorate, sodium hydroxide, and cellulose to purify the CO
safety concerns, if any, associated with its use. It is the
stream.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use.
4.1 Uranium dioxide is used as a nuclear-reactor fuel.
Gadolinium oxide is used as an additive to uranium dioxide. In
2. Referenced Documents
2 order to be suitable for this purpose, these materials must meet
2.1 ASTM Standards:
certain criteria for impurity content. This test method is
C 753 Specification for Nuclear-Grade, Sinterable Uranium
designed to determine whether the carbon content meets
Dioxide Powder
Specifications C 753, C 776, C 888, and C 922.
C 776 Specification for Sintered Uranium Dioxide Pellets
C 888 Specification for Nuclear-Grade Gadolinium Oxide
5. Interferences
(Gd O ) Powder
2 3
5.1 Contamination of carrier gas, crucibles, or samples with
extraneous sources of carbon may cause a positive bias. The
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
blankcorrectionwillhelptominimizethebiasfromcarriergas
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
and crucibles. Interference from absorbed carbon on samples
Test.
may be eliminated by keeping the sample in an inert atmo-
CurrenteditionapprovedJune1,2004.PublishedJuly2004.Originallyapproved
in 1998. Last previous edition approved in 1998 as C 1408 - 98.
sphere or vacuum.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.2 PowderedGd O samplesmayadsorbCO/CO fromthe
2 3 2
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
atmosphere. Sample preheating to 120° for2his recom-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. mended in this case.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1408–98 (2004)
5.3 The purification system typically associated with the 8. Carbon Standard Materials
recommended combustion and detection equipment is de-
8.1 NIST SRM steel standards or equivalent:
signed to minimize other expected sources of interferences,
8.1.1 The 101, 131, 133, 339, and 343 series, ranging from
such as sulfur, halogens, and water.
approximately 20 µg/g sample to 1500 µg/g sample have been
found satisfactory.
6. Apparatus
6.1 Low-Carbon Analyzer, consisting of an induction-
9. Hazards and Precautions
heated furnace suitable for operation at 1600 to 1700°C, an
9.1 Take proper safety precautions to prevent inhalation, or
infrared detector for measuring carbon dioxide, and auxiliary
purification systems. ingestion of uranium dioxide powders or dust during grinding
or handling operations.
6.2 Crucibles, expendable alumina or similar refractory
material. Both the crucible and cover, if used, must be
9.2 Operation of equipment presents electrical and thermal
pre-ignited at a temperature of 1000°C or higher for a time
hazards. Follow manufacturer recommendations for safe op-
sufficient to produce constant blank values.
eration.
6.3 Muffle Furnace, capable of attaining temperature of
9.3 This procedure uses hazardous chemicals. Use appro-
1000°C, for pre-igniting crucibles.
priate precautions for handling corrosives, oxidizers, and
6.4 Tongs and Forceps, for handling crucibles and lids.
gases.
6.5 Stainless Steel Scoops and Spatulas
10. Preparation of Apparatus
7. Reagents and Materials
10.1 Change instrument column packing and reagents as
7.1 Purity of Reagents—Reagent grade chemicals shall be
recommended by manufacturer.
used in all tests. Unless otherwise indicated, it is intended that
10.2 Set the operating controls of the instrument system
all reagents shall conform to the specifications of the Commit-
according to the operating instructions for the specific equip-
tee onAnalytical Reagents of theAmerican Chemical Society,
ment used.
where such specifications are available. Other grades may be
10.3 Condition the apparatus by combustion of several
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the blanks prepared with sample crucible and accelerator in the
amount to be used with the samples. Successi
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