ASTM C698-16

Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O<inf>2</inf>)

SIGNIFICANCE AND USE
4.1 Mixed oxide, a mixture of uranium and plutonium oxides, is used as a nuclear-reactor fuel in the form of pellets. The plutonium content may be up to 10 weight %, and the diluent uranium may be of any 235U enrichment. In order to be suitable for use as a nuclear fuel, the material must meet certain criteria for combined uranium and plutonium content, effective fissile content, and impurity content as described in Specification C833.  
4.1.1 The material is assayed for uranium and plutonium to determine whether the plutonium content is as specified by the purchaser, and whether the material contains the minimum combined uranium and plutonium contents specified on a dry weight basis.  
4.1.2 Determination of the isotopic content of the plutonium and uranium in the mixed oxide is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.  
4.1.3 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) as described in Practice C1233.  
4.2 Fitness for Purpose of Safeguards and Nuclear Safety Applications—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.
SCOPE
1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade mixed oxides, (U, Pu)O2, powders and pellets to determine compliance with specifications.  
1.2 The analytical procedures appear in the following order:    
Sections  
Uranium in the Presence of Pu by Potentiometric Titration  
2  
Plutonium by Controlled-Potential Coulometry  
2  
Plutonium by Amperometric Titration with Iron (II)  
2  
Nitrogen by Distillation Spectrophotometry Using Nessler Reagent  
8 to 15  
Carbon (Total) by Direct Combustion-Thermal Conductivity  
16 to 26  
Total Chlorine and Fluorine by Pyrohydrolysis  
27 to 34  
Sulfur by Distillation-Spectrophotometry  
35 to 43  
Moisture by the Coulometric, Electrolytic Moisture Analyzer  
44 to 51  
Isotopic Composition by Mass Spectrometry  
3  
Rare Earths by Copper Spark Spectroscopy  
52 to 59  
Trace Impurities by Carrier Distillation Spectroscopy  
60 to 68  
Impurities by Spark-Source Mass Spectrography  
69 to 75  
Total Gas in Reactor-Grade Mixed Dioxide Pellets  
4  
Tungsten by Dithiol-Spectrophotometry  
76 to 84  
Rare Earth Elements by Spectroscopy  
85 to 88  
Plutonium-238 Isotopic Abundance by Alpha Spectrometry  
5  
Americium-241 in Plutonium by Gamma-Ray Spectrometry  
Uranium and Plutonium Isotopic Analysis by Mass Spectrometry  
89 to 97  
Oxygen-to-Metal Atom Ratio by Gravimetry  
98 to 105  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.4 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. (For specific safety precaution statements, see Sections 6, 13.2.5, 41.7, and 93.6.1.)

General Information

• Status: Published
• Publication Date: 31-May-2016
• 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 C1817-15 - Standard Test Method for The Determination of the Oxygen to Metal (O/M) Ratio in Sintered Mixed Oxide ((U, Pu)O<inf>2</inf>) Pellets by Gravimetry
• Effective Date: 01-Jun-2015
• Refers: ASTM C1432-15 - Standard Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
• Effective Date: 01-Jun-2015
• Refers: ASTM C1168-15 - Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
• Effective Date: 01-Sep-2015
• Refers: ASTM C1817-16 - Standard Test Method for The Determination of the Oxygen to Metal (O/M) Ratio in Sintered Mixed Oxide ((U, Pu)O<inf>2</inf>) Pellets by Gravimetry
• Effective Date: 15-Jan-2016
• Refers: ASTM C697-16 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets
• Effective Date: 01-Jun-2016
• Refers: ASTM C1672-17 - Standard Test Method for Determination of Uranium or Plutonium Isotopic Composition or Concentration by the Total Evaporation Method Using a Thermal Ionization Mass Spectrometer
• Effective Date: 01-Jan-2017
• Refers: ASTM C1268-15 - Standard Test Method for Quantitative Determination of ²⁴¹Am in Plutonium by Gamma-Ray Spectrometry
• Effective Date: 01-Jun-2015
• Refers: ASTM C1415-18 - Standard Test Method for ²³⁸Pu Isotopic Abundance By Alpha Spectrometry
• Effective Date: 01-Jun-2018
• Refers: ASTM C1625-19 - Standard Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass Spectrometry
• Effective Date: 15-Sep-2019
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Referred By: ASTM C758-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Metal
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1411-20 - Standard Practice for The Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1233-15(2021) - Standard Practice for Determining Equivalent Boron Contents of Nuclear Materials
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1854-17 - Standard Test Method for Determination of Hydrogen (total from all sources) in Mixed Oxide ((U, Pu)O<inf>2</inf>) Sintered Pellets by the Inert Gas Fusion Technique Followed by Thermal Conductivity Measurement
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1853-17 - Standard Test Method for The Determination of Carbon (Total) Content in Mixed Oxide ((U, Pu)O<inf>2</inf>) Sintered Pellets by Direct Combustion-Infrared Detection Method
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1307-21 - Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry
• Effective Date: 01-Jun-2016
• Referred By: ASTM D6884-03(2015)e1 - Standard Practice for Installation of Articulating Concrete Block (ACB) Revetment Systems
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1816-16 - Standard Practice for The Ion Exchange Separation of Small Volume Samples Containing Uranium, Americium, and Plutonium Prior to Isotopic Abundance and Content Analysis
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1907-21 - Standard Practice for Preparation of Plutonium Materials by Pyrohydrolysis for Determination of Fluoride, Chloride, or Both
• Effective Date: 01-Jun-2016
• Referred By: ASTM C1030-10(2018) - Standard Test Method for Determination of Plutonium Isotopic Composition by Gamma-Ray Spectrometry
• Effective Date: 01-Jun-2016
• 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-Jun-2016
• Referred By: ASTM C833-23 - Standard Specification for Sintered (Uranium-Plutonium) Dioxide Pellets for Light Water Reactors
• Effective Date: 01-Jun-2016

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: C698 − 16
Standard Test Methods for
Chemical, Mass Spectrometric, and Spectrochemical
1
Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O )
2
This standard is issued under the fixed designation C698; 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 2. Referenced Documents
6
1.1 These test methods cover procedures for the chemical, 2.1 ASTM Standards:
mass spectrometric, and spectrochemical analysis of nuclear- C697Test Methods for Chemical, Mass Spectrometric, and
grade mixed oxides, (U, Pu)O , powders and pellets to deter- Spectrochemical Analysis of Nuclear-Grade Plutonium
2
mine compliance with specifications. Dioxide Powders and Pellets
C833Specification for Sintered (Uranium-Plutonium) Diox-
1.2 Theanalyticalproceduresappearinthefollowingorder:
ide Pellets
Sections
C852Guide for Design Criteria for Plutonium Gloveboxes
2
Uranium in the Presence of Pu by Potentiometric Titration
2
Plutonium by Controlled-Potential Coulometry C859Terminology Relating to Nuclear Materials
2
Plutonium by Amperometric Titration with Iron (II)
C1068Guide for Qualification of Measurement Methods by
Nitrogen by Distillation Spectrophotometry Using Nessler 8 to 15
a Laboratory Within the Nuclear Industry
Reagent
Carbon (Total) by Direct Combustion-Thermal Conductivity 16 to 26 C1108Test Method for Plutonium by Controlled-Potential
Total Chlorine and Fluorine by Pyrohydrolysis 27 to 34
Coulometry
Sulfur by Distillation-Spectrophotometry 35 to 43
C1165 Test Method for Determining Plutonium by
Moisture by the Coulometric, Electrolytic Moisture Analyzer 44 to 51
3
Isotopic Composition by Mass Spectrometry
Controlled-Potential Coulometry in H SO at a Platinum
2 4
Rare Earths by Copper Spark Spectroscopy 52 to 59
Working Electrode
Trace Impurities by Carrier Distillation Spectroscopy 60 to 68
C1168PracticeforPreparationandDissolutionofPlutonium
Impurities by Spark-Source Mass Spectrography 69 to 75
4
Total Gas in Reactor-Grade Mixed Dioxide Pellets Materials for Analysis
Tungsten by Dithiol-Spectrophotometry 76 to 84
C1204Test Method for Uranium in Presence of Plutonium
Rare Earth Elements by Spectroscopy 85 to 88
5 by Iron(II) Reduction in Phosphoric Acid Followed by
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
Americium-241 in Plutonium by Gamma-Ray Spectrometry Chromium(VI) Titration
Uranium and Plutonium Isotopic Analysis by Mass 89 to 97
C1206Test Method for Plutonium by Iron (II)/Chromium
Spectrometry
7
(VI) Amperometric Titration (Withdrawn 2015)
Oxygen-to-Metal Atom Ratio by Gravimetry 98 to 105
C1233Practice for Determining Equivalent Boron Contents
1.3 The values stated in SI units are to be regarded as
of Nuclear Materials
standard. The values given in parentheses are for information
C1268 Test Method for Quantitative Determination of
only.
241
Am in Plutonium by Gamma-Ray Spectrometry
1.4 This standard does not purport to address all of the 238
C1415Test Method for Pu Isotopic Abundance By Alpha
safety concerns, if any, associated with its use. It is the
Spectrometry
responsibility of the user of this standard to establish appro-
C1432Test Method for Determination of Impurities in
priate safety and health practices and determine the applica-
Plutonium: Acid Dissolution, Ion Exchange Matrix
bility of regulatory limitations prior to use. (For specific safety
Separation, and Inductively Coupled Plasma-Atomic
precautionstatements,seeSections6,13.2.5,41.7,and93.6.1.)
Emission Spectroscopic (ICP/AES) Analysis
C1625Test Method for Uranium and Plutonium Concentra-
tions and Isotopic Abundances by Thermal Ionization
1
These test methods are under the jurisdiction of ASTM Committee C26 on
Mass Spectrometry
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
Methods of Test.
CurrenteditionapprovedJune1,2016.PublishedJuly2016.Originallyapproved
6
in 1972. Last previous edition approved in 2010 as C698–10. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
C0698-16. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
2
Discontinued as of November 15, 1992. Standards volume information, refer to the standard’s Document Summary page on
3
Discontinued as of May 30, 1980. the ASTM website.
4 7
Discontinued as of June 2016. The last approved version of this historical standard is referenced on
5
Discontinued as of January 1, 2004. www.astm.org.
Copyright © ASTM Internati
...

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: C698 − 10 C698 − 16
Standard Test Methods for
Chemical, Mass Spectrometric, and Spectrochemical
1
Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O )
2
This standard is issued under the fixed designation C698; 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
mixed oxides, (U, Pu)O , powders and pellets to determine compliance with specifications.
2
1.2 The analytical procedures appear in the following order:
Sections
2
Uranium in the Presence of Pu by Potentiometric Titration
2
Plutonium by Controlled-Potential Coulometry
2
Plutonium by Amperometric Titration with Iron (II)
Nitrogen by Distillation Spectrophotometry Using Nessler 7 to 14
Reagent
Nitrogen by Distillation Spectrophotometry Using Nessler 8 to 15
Reagent
Carbon (Total) by Direct Combustion-Thermal Conductivity 15 to 26
Carbon (Total) by Direct Combustion-Thermal Conductivity 16 to 26
Total Chlorine and Fluorine by Pyrohydrolysis 27 to 34
Sulfur by Distillation-Spectrophotometry 35 to 43
Moisture by the Coulometric, Electrolytic Moisture Analyzer 44 to 51
3
Isotopic Composition by Mass Spectrometry
Rare Earths by Copper Spark Spectroscopy 52 to 59
Trace Impurities by Carrier Distillation Spectroscopy 60 to 69
Trace Impurities by Carrier Distillation Spectroscopy 60 to 68
Impurities by Spark-Source Mass Spectrography 70 to 76
Impurities by Spark-Source Mass Spectrography 69 to 75
4
Total Gas in Reactor-Grade Mixed Dioxide Pellets 77to 84
4
Total Gas in Reactor-Grade Mixed Dioxide Pellets
Tungsten by Dithiol-Spectrophotometry 85 to 93
Tungsten by Dithiol-Spectrophotometry 76 to 84
Rare Earth Elements by Spectroscopy 94 to 97
Rare Earth Elements by Spectroscopy 85 to 88
5
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
Americium-241 in Plutonium by Gamma-Ray Spectrometry
Uranium and Plutonium Isotopic Analysis by Mass 98 to 106
Spectrometry
Uranium and Plutonium Isotopic Analysis by Mass 89 to 97
Spectrometry
Oxygen-to-Metal Atom Ratio by Gravimetry 107 to 115
Oxygen-to-Metal Atom Ratio by Gravimetry 98 to 105
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.4 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. (For specific safeguard and safety precaution statements, see Sections 116, 2013.2.5, 6441.7, and 112 and
102.6.193.6.1.)
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 June 1, 2010June 1, 2016. Published July 2010July 2016. Originally approved in 1972. Last previous edition approved in 20042010 as
C698 – 04.C698 – 10. DOI: 10.1520/C0698-10.10.1520/C0698-16.
2
Discontinued as of November 15, 1992.
3
Discontinued as of May 30, 1980.
4
Discontinued as of January 1, 2004.June 2016.
5
Discontinued as of January 1, 2004.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C698 − 16
2. Referenced Documents
6
2.1 ASTM Standards:
C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide
Powders and Pellets
C833 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets
C852 Guide for Design Criteria for Plutonium Gloveboxes
6
C1008 Specification for Sintered (Uranium-Plutonium) DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
C1009C859 Guide for Establishing and Maintaining a Quality Assurance Program for Analytical Laboratories Within the
Nuclear IndustryTerminology Relating to Nuclear Materials
C1068 Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry
C1108 Test Method for Plutonium by Controlled-Potential Coulometry
C1128 Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle Materials
C1156 Guide for Establishing
...