ASTM C696-11
(Test Method)Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets
Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets
SIGNIFICANCE AND USE
Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, and impurity content. These test methods are designed to show whether or not a given material meets the specifications for these items as described in Specifications C753 and C776.
An assay is performed to determine whether the material has the minimum uranium content specified on a dry weight basis.
The stoichiometry of the oxide is useful for predicting its sintering behavior in the pellet production process.
Determination of the isotopic content of the uranium in the uranium dioxide powder is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.
Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC).
SCOPE
1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
Sections Uranium by Ferrous Sulfate Reduction in Phosphoric Acid and Dichromate Titration Method C1267 Test Method for Uranium By Iron (II) Reduction In Phosphoric Acid Followed By Chromium (VI) Titration In The Presence of Vanadium Uranium and Oxygen Uranium Atomic Ratio by the Ignition (Gravimetric) Impurity Correction Method C1453 Standard Test Method for the Determination of Uranium by Ignition and Oxygen to Uranium Ratio (O/U) Atomic Ratio of Nuclear Grade Uranium Dioxide Powders and Pellets Carbon (Total) by Direct Combustion-Thermal Conductivity Method C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Total Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method C1502 Standard Test Method for the Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Moisture by the Coulometric, Electrolytic Moisture Analyzer Method7-14 Nitrogen by the Kjeldahl Method15-22 Isotopic Uranium Composition by Multiple-Filament Surface Ionization Mass Spectrometric Method Spectrochemical Determination of Trace Elements in High-Purity Uranium Dioxide23-30 Silver, Spectrochemical Determination of, by Gallium OxideCarrier D-C Arc Technique31 and 32 Rare Earths by Copper Spark-Spectrochemical Method Impurity Elements by a Spark-Source Mass Spectrographic Method C761 Test Method for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry Surface Area by Nitrogen Absorption Method33-39 Total Gas in Reactor-Grade Uranium Dioxide Pellets Thorium and Rare Earth Elements by Spectroscopy Hydrogen by Inert Gas Fusion C1457 Standard Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction Uranium Isotopic Analysis by Mass Spectrometry C1413 Test Method for Isotopic Analysis of Hydrolysed Uranium Hexafluoride and Uranyl Nitrate Solutions By Thermal Ionization Mass Spectrometry
7.1 This test method covers the determination of moisture in uranium dioxide samples. Detection limits are as low as 10 μg.
15.1 This test method covers the determination of nitride nitrogen in uranium dioxide in the range from 10 to 250 μg.
23.1 This test method covers the spectrographic analysis of nuclear-grade UO2 for the 26 elements in the ranges indicated in Table 1.
23.2 For simultaneous determination of trace elements by plasma emission spectroscopy refer to Test Method C76...
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Designation: C696 − 11
Standard Test Methods for
Chemical, Mass Spectrometric, and Spectrochemical
Analysis of Nuclear-Grade Uranium Dioxide Powders and
1
Pellets
This standard is issued under the fixed designation C696; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope
Silver, Spectrochemical Determination of, by Gallium 31 and 32
OxideCarrier D-C Arc Technique
1.1 These test methods cover procedures for the chemical, 2
Rare Earths by Copper Spark-Spectrochemical
mass spectrometric, and spectrochemical analysis of nuclear- Method
2
Impurity Elements by a Spark-Source Mass Spectro-
grade uranium dioxide powders and pellets to determine
graphic Method
3
compliance with specifications.
C761 Test Method for Chemical, Mass
Spectrometric, Spectrochemical, Nuclear, and Ra-
1.2 Theanalyticalproceduresappearinthefollowingorder:
diochemical Analysis of Uranium Hexafluoride
3
C1287 Test Method for Determination of Impurities
Sections
In Uranium Dioxide By Inductively Coupled Plasma
2
Mass Spectrometry
Uranium by Ferrous Sulfate Reduction in Phosphoric
Surface Area by Nitrogen Absorption Method 33–39
Acid and Dichromate Titration Method
2
3
Total Gas in Reactor-Grade Uranium Dioxide Pellets
C1267 Test Method for Uranium By Iron (II) Reduc-
2
Thorium and Rare Earth Elements by Spectroscopy
tion In Phosphoric Acid Followed By Chromium (VI)
4
Hydrogen by Inert Gas Fusion
Titration In The Presence of Vanadium
3
4
C1457 Standard Test Method for Determination of
Uranium and Oxygen Uranium Atomic Ratio by the
Total Hydrogen Content of Uranium Oxide Powders
Ignition (Gravimetric) Impurity Correction Method
3
and Pellets by Carrier Gas Extraction
C1453 Standard Test Method for the Determination
2
Uranium Isotopic Analysis by Mass Spectrometry
of Uranium by Ignition and Oxygen to Uranium Ratio
3
C1413 Test Method for Isotopic Analysis of Hydro-
(O/U) Atomic Ratio of Nuclear Grade Uranium Diox-
lysed Uranium Hexafluoride and Uranyl Nitrate Solu-
ide Powders and Pellets
2
tions By Thermal Ionization Mass Spectrometry
Carbon (Total) by Direct Combustion-Thermal Con-
ductivity Method
3
C1408 Test Method for Carbon (Total) in Uranium
2. Referenced Documents
Oxide Powders and Pellets By Direct Combustion-
3
Infrared Detection Method 2.1 ASTM Standards:
4
Total Chlorine and Fluorine by Pyrohydrolysis Ion-
C753Specification for Nuclear-Grade, Sinterable Uranium
Selective Electrode Method
3
Dioxide Powder
C1502 Standard Test Method for the Determina-
tion of Total Chlorine and Fluorine in Uranium Diox-
C761Test Methods for Chemical, Mass Spectrometric,
ide and Gadolinium Oxide
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
Moisture by the Coulometric, Electrolytic Moisture 7–14
Uranium Hexafluoride
Analyzer Method
Nitrogen by the Kjeldahl Method 15–22
C776Specification for Sintered Uranium Dioxide Pellets
5
Isotopic Uranium Composition by Multiple-Filament
C1267Test Method for Uranium by Iron (II) Reduction in
Surface Ionization Mass Spectrometric Method
PhosphoricAcid Followed by Chromium (VI)Titration in
Spectrochemical Determination of Trace Elements in 23–30
High-Purity Uranium Dioxide
the Presence of Vanadium
C1287Test Method for Determination of Impurities in
Nuclear Grade Uranium Compounds by Inductively
1
These test methods are under the jurisdiction of ASTM Committee C26 on
Coupled Plasma Mass Spectrometry
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
C1347Practice for Preparation and Dissolution of Uranium
Methods of Test.
Current edition approved Sept. 1, 2011. Published October 2011. Originally
Materials for Analysis
approvedin1972.Lastpreviouseditionapprovedin2005asC696–99(2005).DOI:
C1408Test Method for Carbon (Total) in Uranium Oxide
10.1520/C0696-11.
Powders and Pellets By Direct Combustion-Infrared De-
2
Discontinued January 1999. See C696–80.
3
tection Method
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
C1413Test Method for Isotopic Analysis of Hydrolyzed
Standards volume information, refer to the standard’s Document Summary page on
Uranium Hexafluoride and Uranyl Nitrate Solutions by
the ASTM website.
4
Thermal Ionization Mass Spectrometry
Discontinued September 2011.
5
Discontinued as of May 30, 1980. C1453Test Method for the Determination of Uranium by
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C696 − 11
Ignition and the Oxygen to Uranium (O/U
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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.
ϵ1
Designation:C 696–93 Designation:C696–11
Standard Test Methods for
Chemical, Mass Spectrometric, and Spectrochemical
Analysis of Nuclear-Grade Uranium Dioxide Powders and
1
Pellets
This standard is issued under the fixed designation C696; 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
1
superscript epsilon (ϵ) indicates an editorial change since the last revision or reapproval. ϵ NOTE—Paragraph 91.2 was corrected
editorially in March 1994.
1. Scope
1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade
uranium dioxide powders and pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
Sections
2
Uranium by Ferrous Sulfate Reduction in Phosphoric
Acid and Dichromate Titration Method7-15
2
Uranium by Ferrous Sulfate Reduction in Phosphoric
Acid and Dichromate Titration Method
3
C1267 Test Method for Uranium By Iron (II) Reduc-
tion In Phosphoric Acid Followed By Chromium (VI)
Titration In The Presence of Vanadium
4
Uranium and Oxygen Uranium Atomic Ratio by the
Ignition (Gravimetric) Impurity Correction
Method16-22
4
Uranium and Oxygen Uranium Atomic Ratio by the
Ignition (Gravimetric) Impurity Correction Method
3
C1453 Standard Test Method for the Determination
of Uranium by Ignition and Oxygen to Uranium Ratio
(O/U) Atomic Ratio of Nuclear Grade Uranium Diox-
ide Powders and Pellets
2
Carbon (Total) by Direct Combustion-Thermal Con-
ductivity Method23-32
2
Carbon (Total) by Direct Combustion-Thermal Con-
ductivity Method
3
C1408 Test Method for Carbon (Total) in Uranium
Oxide Powders and Pellets By Direct Combustion-
Infrared Detection Method
4
Total Chlorine and Fluorine by Pyrohydrolysis Ion-
Selective Electrode Method33-39
4
Total Chlorine and Fluorine by Pyrohydrolysis Ion-
Selective Electrode Method
3
C1502 Standard Test Method for the Determination
of Total Chlorine and Fluorine in Uranium Dioxide
and Gadolinium Oxide
Moisture by the Coulometric, Electrolytic Moisture 40-47
Analyzer Method
Moisture by the Coulometric, Electrolytic Moisture 7-14
Analyzer Method
Nitrogen by the Kjeldahl Method 48-55
Nitrogen by the Kjeldahl Method 15-22
5
Isotopic Uranium Composition by Multiple-Filament
a
Surface Ionization Mass Spectrometric Method1
5
Isotopic Uranium Composition by Multiple-Filament
Surface Ionization Mass Spectrometric Method
1
These test methods are under the jurisdiction of ASTM Committee C-26 on Nuclear Fuel Cycle.
Current edition approved Nov. 15, 1993. Published February 1994. Originally published as C 696 – 72. Last previous edition C 696 – 80.
1a
Discontinued as of May 30, 1980.
1
These test methods are under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methods
of Test.
Current edition approved Sept. 1, 2011. Published October 2011. Originally approved in 1972. Last previous edition approved in 2005 as C696–99(2005). DOI:
10.1520/C0696-11.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
C696–11
Spectrochemical Determination of Trace Elements in 56-63
High-Purity Uranium Dioxide
Spectrochemical Determination of Trace Elements in 23-30
High-Purity Uranium Dioxide
Silver, Spectrochemical Determination of, by Gallium 64 to 65
OxideCarrier D-C Arc Technique
Silver, Spectrochemical Determination of, by Gallium 31 and 32
OxideCarrier D-C Arc Technique
2
Rare Earths by Copper Spark-Spectrochemical
Method66-75
2
Rare Earths by Copper Spark-Spectrochemical
Method
2
Impurity Elements by a Spark-Source Mass Spectro-
graphic Method76-82
2
Impurity Elements by a Spark-Source Mass Spectro-
graphic Method
3
C761 Test Method for Chemical, Mass Spectromet-
ric, Spectrochemical, Nuclear, and Radiochemical
Analysis of Uranium Hexafluoride
3
C1287 Test Method for Determination of Impurities
In Uranium Dioxide By Inductively Coupled Plasma
Mass Spectrometry
Surface Area by Nitrogen Absorption Method 83-89
Surface Area by Nitrogen Absorption Method 33-39
2
Total Gas in Reactor-Grade Uranium Dioxide
Pellets90-97
2
Total Gas in Reactor-Grade Uranium Dioxide Pellets
2
Thorium and Rare Earth Elements by
Spectroscopy98-105
2
Thorium and Rare Earth Elements by Spectroscopy
4
Hydrogen by Inert Gas Fusion106-
...
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