ASTM C1408-98
(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
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.
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Designation: C 1408 – 98
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 within an induction-heated furnace and burned at a nominal
temperature of 1600 to 1700°C in a stream of oxygen. A
1.1 This test method covers the determination of carbon in
catalyst converts the carbon monoxide (CO) to carbon dioxide
nuclear-grade uranium oxide powders and pellets to determine
(CO ) and the products of combustion are scavenged free of
compliance with specifications. 2
sulfur compounds, halogens, and water vapor. The CO is
1.2 Gadolinium oxide (Gd O ) and gadolinium oxide-
2 3
swept into an infrared cell detector. The amount of carbon is
uranium oxide powders and pellets may also be analyzed using
automatically determined from stored calibration data, and is
this test method.
displayed or printed out, or both, by the carbon analyzer.
1.3 This test method covers the determination of 5 to 500 μg
3.2 The actual configuration of the system may vary with
of residual carbon.
vendor and model. Typical systems include columns of mate-
1.4 This test method describes an induction furnace carrier
rials such as copper oxide, platinized silica gel, magnesium
gas combustion system equipped with an infrared detector. It
perchlorate, sodium hydroxide, and cellulose to purify the CO
may also be applied to a similar instrument equipped with a
stream.
thermal conductivity detector.
1.5 The preferred system of units is micrograms carbon per
4. Significance and Use
gram of sample (μg/g sample) or micrograms carbon per gram
4.1 Uranium dioxide is used as a nuclear-reactor fuel.
of uranium (μg/g U).
Gadolinium oxide is used as an additive to uranium dioxide. In
1.6 This standard does not purport to address all of the
order to be suitable for this purpose, these materials must meet
safety concerns, if any, associated with its use. It is the
certain criteria for impurity content. This test method is
responsibility of the user of this standard to establish appro-
designed to determine whether the carbon content meets
priate safety and health practices and determine the applica-
Specifications C 753, C 776, C 888, and C 922.
bility of regulatory limitations prior to use.
5. Interferences
2. Referenced Documents
5.1 Contamination of carrier gas, crucibles, or samples with
2.1 ASTM Standards:
extraneous sources of carbon may cause a positive bias. The
C 753 Specification for Nuclear-Grade, Sinterable Uranium
2 blank correction will help to minimize the bias from carrier gas
Dioxide Powder
2 and crucibles. Interference from absorbed carbon on samples
C 776 Specification for Sintered Uranium Dioxide Pellets
may be eliminated by keeping the sample in an inert atmo-
C 888 Specification for Nuclear-Grade Gadolinium Oxide
2 sphere or vacuum.
Powder
5.2 Powdered Gd O samples may adsorb CO/CO from the
2 3 2
C 922 Specification for Sintered Gadolinium Oxide-
2 atmosphere. Sample preheating to 120° for2his recom-
Uranium Dioxide Pellets
mended in this case.
3. Summary of Test Method 5.3 The purification system typically associated with the
recommended combustion and detection equipment is de-
3.1 The powered or crushed test specimen and an appropri-
signed to minimize other expected sources of interferences,
ate accelerator (metal flux) are added to a crucible, placed
such as sulfur, halogens and water.
This test method is under the jurisdiction of ASTM Committee C-26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
Current edition approved Sept. 10, 1998. Published December 1998.
Annual Book of ASTM Standards, Vol 12.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1408–98
6. Apparatus 9. Hazards and Precautions
6.1 Low-Carbon Analyzer, consisting of an induction- 9.1 Take proper safety precautions to prevent inhalation, or
heated furnace suitable for operation at 1600 to 1700 °C, an ingestion of uranium dioxide powders or dust during grinding
infrared detector for measuring carbon dioxide, and auxiliary or handling operations.
purification systems. 9.2 Operation of equipment presents electrical and thermal
6.2 Crucibles, expendable alumina or similar refractory hazards. Follow manufacturer recommendations for safe op-
material. Both the crucible and cover, if used, must be eration.
pre-ignited at a temperature of 1000°C or higher for a time 9.3 This procedure uses hazardous chemicals. Use appro-
sufficient to produce constant blank values. priate precautions for handling corrosives, oxidizers, and
6.3 Muffle Furnace, capable of attaining temperature of gases.
1000°C, for pre-igniting crucibles.
10. Preparation of Apparatus
6.4 Tongs and Forceps, for handling crucibles and lids.
10.1 Change instrument column packing and reagents as
6.5 Stainless Steel Scoops and Spatulas
recommended by manufacturer.
7. Reagents and Materials
10.2 Set the operating controls of the instrument system
7.1 Purity of Reagents—Reagent grade chemicals shall be
according to the operating instructions for the specific equip-
used in all tests. Unless otherwise indicated, it is intended that ment used.
all reagents shall conform to the specifications of the Commit-
10.3 Condition the apparatus by combustion of several
tee on Analytical Reagents of the American Chemical Society,
blanks prepared with sample crucible and accelerator in the
where such specifications are available. Other grades may be
amount to be used with the samples. Successive blanks should
used, provided it is first ascertained that the reagent is of
approach a constant value, allowing for normal statistical
sufficiently high purity to permit its use without lessening the
fluctuations.
accuracy of the determination.
4 11. Calibration
7.2 Accelerators—Copper metal, tin-tungsten mixture ,
copper oxide, granular tin, and high purity iron chip accelera- 11.1 The calibration range and number of standards will
depend upon the instrument used. Two to four standards
tor
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