ASTM C696-19

Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets

SIGNIFICANCE AND USE
4.1 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.  
4.1.1 An assay is performed to determine whether the material has the minimum uranium content specified on a dry weight basis.  
4.1.2 The stoichiometry of the oxide powder is useful for predicting its sintering behavior in the pellet production process.  
4.1.3 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.  
4.1.4 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).  
4.1.5 Determination of the oxygen-to-uranium ratio is performed on the completed pellets to determine whether they have the appropriate stoichiometry for optimal performance during irradiation.
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 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.3 The analytical procedures appear in the following order:
Sections  
Uranium by Ferrous Sulfate Reduction in Phosphoric Acid and Dichromate Titration Method  
2  
Uranium and Oxygen Uranium Atomic Ratio by the Ignition (Gravimetric) Impurity Correction Method  
3  
Carbon (Total) by Direct Combustion-Thermal Conductivity Method  
2  
Total Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method  
3    
Moisture by the Coulometric, Electrolytic Moisture Analyzer Method  
8 – 15    
Nitrogen by the Kjeldahl Method  
16 – 23    
Isotopic Uranium Composition by Multiple-Filament Surface Ionization Mass Spectrometric Method  
4  
Spectrochemical Determination of Trace Elements in High-Purity Uranium Dioxide  
5  
Silver, Spectrochemical Determination of, by Gallium Oxide Carrier D-C Arc Technique  
5    
Rare Earths by Copper Spark-Spectrochemical Method  
2  
Impurity Elements by a Spark-Source Mass Spectrographic Method  
2  
Surface Area by Nitrogen Absorption Method  
24 – 30    
Total Gas in Reactor-Grade Uranium Dioxide Pellets  
2  
Thorium and Rare Earth Elements by Spectroscopy  
2  
Hydrogen by Inert Gas Fusion  
3    
Uranium Isotopic Analysis by Mass Spectrometry  
2  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Oct-2019
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C753-16 - Standard Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
• Effective Date: 01-Feb-2016
• Refers: ASTM C1502-16 - Standard Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide
• Effective Date: 15-Jan-2016
• Refers: ASTM C1408-16 - Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
• Effective Date: 01-Mar-2016
• Refers: ASTM C1517-16 - Standard Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission Spectroscopy
• Effective Date: 01-Apr-2016
• Refers: ASTM C1287-18 - Standard Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma Mass Spectrometry
• Effective Date: 01-Jan-2018
• Refers: ASTM C761-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
• Effective Date: 01-Feb-2018
• Refers: ASTM C1457-18 - Standard Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction
• Effective Date: 01-Feb-2018
• Refers: ASTM C1413-18 - Standard Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by Thermal Ionization Mass Spectrometry
• Effective Date: 01-Nov-2018
• Refers: ASTM C1453-19 - Standard Test Method for the Determination of Uranium by Ignition and the Oxygen to Uranium (O/U) Atomic Ratio of Nuclear Grade Uranium Dioxide Powders and Pellets
• Effective Date: 01-Jul-2019
• Referred By: ASTM C1430-18 - Standard Test Method for Determination of Uranium, Oxygen to Uranium (O/U), and Oxygen to Metal (O/M) in Sintered Uranium Dioxide and Gadolinia-Uranium Dioxide Pellets by Atmospheric Equilibration
• Effective Date: 01-Nov-2019
• Referred By: ASTM C1334-05(2022) - Standard Specification for Uranium Oxides with a ²³⁵U Content of Less Than 5 % for Dissolution Prior to Conversion to Nuclear-Grade Uranium Dioxide
• Effective Date: 01-Nov-2019
• Referred By: ASTM C799-19 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions
• Effective Date: 01-Nov-2019
• Referred By: ASTM C1682-21 - Standard Guide for Characterization of Spent Nuclear Fuel in Support of Interim Storage, Transportation and Geologic Repository Disposal
• Effective Date: 01-Nov-2019
• Referred By: ASTM C753-16a(2021) - Standard Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
• Effective Date: 01-Nov-2019
• Referred By: ASTM C1267-17(2022) - Standard Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium
• Effective Date: 01-Nov-2019
• Referred By: ASTM C1233-15(2021) - Standard Practice for Determining Equivalent Boron Contents of Nuclear Materials
• Effective Date: 01-Nov-2019
• Referred By: ASTM C776-17(2022) - Standard Specification for Sintered Uranium Dioxide Pellets for Light Water Reactors
• Effective Date: 01-Nov-2019
• Referred By: ASTM C1462-21 - Standard Specification for Uranium Metal Enriched to Less Than 20 % <sup> 235</sup >U
• Effective Date: 01-Nov-2019

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C696 − 19
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 1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 These test methods cover procedures for the chemical,
ization established in the Decision on Principles for the
mass spectrometric, and spectrochemical analysis of nuclear-
Development of International Standards, Guides and Recom-
grade uranium dioxide powders and pellets to determine
mendations issued by the World Trade Organization Technical
compliance with specifications.
Barriers to Trade (TBT) Committee.
1.2 Units—The values stated in SI units are to be regarded
2. Referenced Documents
as standard. The values given in parentheses are for informa-
6
tion only.
2.1 ASTM Standards:
C753Specification for Nuclear-Grade, Sinterable Uranium
1.3 Theanalyticalproceduresappearinthefollowingorder:
Dioxide Powder
Sections
C761Test Methods for Chemical, Mass Spectrometric,
2
Uranium by Ferrous Sulfate Reduction in Phosphoric
Spectrochemical,Nuclear,andRadiochemicalAnalysisof
Acid and Dichromate Titration Method
3 Uranium Hexafluoride
Uranium and Oxygen Uranium Atomic Ratio by the
Ignition (Gravimetric) Impurity Correction Method C776SpecificationforSinteredUraniumDioxidePelletsfor
2
Carbon (Total) by Direct Combustion-Thermal
Light Water Reactors
Conductivity Method
3 C859Terminology Relating to Nuclear Materials
Total Chlorine and Fluorine by Pyrohydrolysis Ion-
Selective Electrode Method
C1267Test Method for Uranium by Iron (II) Reduction in
Moisture by the Coulometric, Electrolytic Moisture 8–15
PhosphoricAcid Followed by Chromium (VI)Titration in
Analyzer Method
the Presence of Vanadium
Nitrogen by the Kjeldahl Method 16–23
4
Isotopic Uranium Composition by Multiple-Filament
C1287Test Method for Determination of Impurities in
Surface Ionization Mass Spectrometric Method
Nuclear Grade Uranium Compounds by Inductively
5
Spectrochemical Determination of Trace Elements in
Coupled Plasma Mass Spectrometry
High-Purity Uranium Dioxide
5
Silver, Spectrochemical Determination of, by Gallium
C1347Practice for Preparation and Dissolution of Uranium
Oxide Carrier D-C Arc Technique
Materials for Analysis
2
Rare Earths by Copper Spark-Spectrochemical
C1408Test Method for Carbon (Total) in Uranium Oxide
Method
2
Impurity Elements by a Spark-Source Mass Spectro-
Powders and Pellets By Direct Combustion-Infrared De-
graphic Method
tection Method
Surface Area by Nitrogen Absorption Method 24–30
2
C1413Test Method for Isotopic Analysis of Hydrolyzed
Total Gas in Reactor-Grade Uranium Dioxide Pellets
2
Thorium and Rare Earth Elements by Spectroscopy
Uranium Hexafluoride and Uranyl Nitrate Solutions by
3
Hydrogen by Inert Gas Fusion
Thermal Ionization Mass Spectrometry
2
Uranium Isotopic Analysis by Mass Spectrometry
C1453Test Method for the Determination of Uranium by
Ignition and the Oxygen to Uranium (O/U)Atomic Ratio
of Nuclear Grade Uranium Dioxide Powders and Pellets
1
These test methods are under the jurisdiction of ASTM Committee C26 on
C1457Test Method for Determination of Total Hydrogen
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
ContentofUraniumOxidePowdersandPelletsbyCarrier
Methods of Test.
Current edition approved Nov. 1, 2019. Published November 2019. Originally
Gas Extraction
approved in 1972. Last previous edition approved in 2011 as C696–11. DOI:
10.1520/C0696-19.
2 6
Discontinued January 1999. See C696–80. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
Discontinued September 2011. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
4
Discontinued as of May 30, 1980. Standards volume information, refer to the standard’s Document Summary page on
5
Discontinued as of Nov. 1, 2019 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C696 − 19
C1502Test Method for Determination ofTotal Chlorine and 6. Safety Precautions
Fluorine in Uranium Dioxide and Gadolinium Oxide
6.1 Proper precautions should be taken to prevent
C1517TestMethodforDeterminationo
...

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: C696 − 11 C696 − 19
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. 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 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 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 The analytical procedures appear in the following order:
Sections
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
3
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 Method
3
C1408 Test Method for Carbon (Total) in Uranium
Oxide Powders and Pellets By Direct Combustion-
Infrared Detection Method
3
Total Chlorine and Fluorine by Pyrohydrolysis Ion-
Selective Electrode Method
3
C1502 Standard Test Method for the Determina-
tion of Total Chlorine and Fluorine in Uranium Diox-
ide and Gadolinium Oxide
Moisture by the Coulometric, Electrolytic Moisture 7 – 14
Analyzer Method
Moisture by the Coulometric, Electrolytic Moisture 8 – 15
Analyzer Method
Nitrogen by the Kjeldahl Method 15 – 22
Nitrogen by the Kjeldahl Method 16 – 23
4
Isotopic Uranium Composition by Multiple-Filament
Surface Ionization Mass Spectrometric Method
5
Spectrochemical Determination of Trace Elements in 23 – 30
High-Purity Uranium Dioxide
5
Spectrochemical Determination of Trace Elements in
High-Purity Uranium Dioxide
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, 2011Nov. 1, 2019. Published October 2011November 2019. Originally approved in 1972. Last previous edition approved in 20052011
as C696 – 99C696 – 11.(2005). DOI: 10.1520/C0696-11.10.1520/C0696-19.
2
Discontinued January 1999. See C696–80.
6
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Discontinued September 2011.
4
Discontinued as of May 30, 1980.
5
Discontinued as of Nov. 1, 2019
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C696 − 19
5
Silver, Spectrochemical Determination of, by Gallium 31 and 32
OxideCarrier D-C Arc Technique
5
Silver, Spectrochemical Determination of, by Gallium
Oxide Carrier D-C Arc Technique
2
Rare Earths by Copper Spark-Spectrochemical
Method
2
Impurity Elements by a Spark-Source Mass Spectro-
graphic Method
3
C761 Test Method for Chemical, Mass
Spectrometric, Spectrochemical, Nuclear, and Ra-
diochemical 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 33 – 39
Surface Area by Nitrogen Absorption Method 24 – 30
2
Total Gas in Reactor-Grade Uranium Dioxide Pellets
2
Thorium and Rare Earth Elements by Spectroscopy
3
Hydrogen by Inert Gas Fusion
3
C1457 Standard Test Method for Determination of
Total Hydrogen Content of Uranium Oxide Powders
and Pellets by Carrier Gas Extraction
2
Uranium Isotopic Analysis by Mass Spectrometry
3
C1413 Test Method for Isotopic Analysis of Hydro-
lysed Uranium Hexafluoride and Uranyl Nitrate Solu-
tions By Thermal Ionization Mass Spectrometry
1.4 This international standard was developed in accordance with internationally recognized principles on standardiza
...