ASTM C698-10
(Test Method)Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O2)
Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O<sub>2</sub>)
SIGNIFICANCE AND USE
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.
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.
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.
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 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 Plutonium by Controlled-Potential Coulometry Plutonium by Amperometric Titration with Iron (II) Nitrogen by Distillation Spectrophotometry Using Nessler Reagent 7 to 14 Carbon (Total) by Direct Combustion-Thermal Conductivity 15 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 Rare Earths by Copper Spark Spectroscopy 52 to 59 Trace Impurities by Carrier Distillation Spectroscopy 60 to 69 Impurities by Spark-Source Mass Spectrography 70 to 76 Total Gas in Reactor-Grade Mixed Dioxide Pellets 77 to 84 Tungsten by Dithiol-Spectrophotometry 85 to 93 Rare Earth Elements by Spectroscopy 94 to 97 Plutonium-238 Isotopic Abundance by Alpha Spectrometry Americium-241 in Plutonium by Gamma-Ray Spectrometry Uranium and Plutonium Isotopic Analysis by Mass Spectrometry 98 to 106 Oxygen-to-Metal Atom Ratio by Gravimetry 107 to 115
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 11, 20, 64, and 112 and 102.6.1.)
7.1 This test method covers the determination of 5 to 100 μg/g of nitride nitrogen in mixtures of plutonium and uranium oxides in either pellet or powder form.
15.1 This test method covers the determination of 10 to 200 μg of residual carbon in nuclear grade mixed oxides, (U,Pu)O2.
27.1 This test method is applicable to the determination of 5 to 100μ g/g of chlorine and 1 to 100 μg/g of fluorine in 1-g samples of nuclear-grade mixed oxides, (U, Pu)O2.
35.1 This test method covers the determination of sulfur in the concentration range from 10 to 600 μg/g for samples of nuclear-grade uranium and plutonium mixed oxides, (U, Pu)O2.
44.1 This test method covers the determination of moisture in nuclear-grade mixed oxides of uranium and plutonium (U,Pu)O2. Detection limits are as low as 10 μg.
52.1 This test method covers the determination of rare earths in uranium-plutonium dioxide over the range from 10 to 200 μg/g.
60.1 This test method cover...
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Designation: C698 − 10
StandardTest 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
5
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 C1008 Specification for Sintered (Uranium-Plutonium)
2
6
Plutonium byAmperometric Titration with Iron (II)
DioxidePellets—Fast Reactor Fuel (Withdrawn 2014)
Nitrogen by Distillation Spectrophotometry Using Nessler 7 to 14
C1009Guide for Establishing and Maintaining a Quality
Reagent
Carbon (Total) by Direct Combustion-Thermal Conductivity 15 to 26 AssuranceProgramforAnalyticalLaboratoriesWithinthe
Total Chlorine and Fluorine by Pyrohydrolysis 27 to 34
Nuclear Industry
Sulfur by Distillation-Spectrophotometry 35 to 43
C1068Guide for Qualification of Measurement Methods by
Moisture by the Coulometric, Electrolytic MoistureAnalyzer 44 to 51
3
Isotopic Composition by Mass Spectrometry
a Laboratory Within the Nuclear Industry
Rare Earths by Copper Spark Spectroscopy 52 to 59
C1108Test Method for Plutonium by Controlled-Potential
Trace Impurities by Carrier Distillation Spectroscopy 60 to 69
Coulometry
Impurities by Spark-Source Mass Spectrography 70 to 76
Total Gas in Reactor-Grade Mixed Dioxide Pellets 77 to 84 C1128Guide for Preparation of Working Reference Materi-
Tungsten by Dithiol-Spectrophotometry 85 to 93
als for Use in Analysis of Nuclear Fuel Cycle Materials
Rare Earth Elements by Spectroscopy 94 to 97
4 C1156Guide for Establishing Calibration for a Measure-
Plutonium-238 IsotopicAbundance byAlpha Spectrometry
Americium-241 in Plutonium by Gamma-Ray Spectrometry ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
Uranium and Plutonium IsotopicAnalysis by Mass 98 to 106
rials
Spectrometry
C1165 Test Method for Determining Plutonium by
Oxygen-to-MetalAtom Ratio by Gravimetry 107 to 115
Controlled-Potential Coulometry in H SO at a Platinum
2 4
1.3 The values stated in SI units are to be regarded as
Working Electrode
standard. The values given in parentheses are for information
C1168PracticeforPreparationandDissolutionofPlutonium
only.
Materials for Analysis
1.4 This standard does not purport to address all of the
C1204Test Method for Uranium in Presence of Plutonium
safety concerns, if any, associated with its use. It is the
by Iron(II) Reduction in Phosphoric Acid Followed by
responsibility of the user of this standard to establish appro-
Chromium(VI) Titration
priate safety and health practices and determine the applica-
C1206Test Method for Plutonium by Iron (II)/Chromium
bility of regulatory limitations prior to use. (For specific 6
(VI) Amperometric Titration (Withdrawn 2015)
safeguard and safety precaution statements, see Sections 11,
C1210Guide for Establishing a Measurement System Qual-
20, 64, and 112 and 102.6.1.)
ity Control Program for Analytical Chemistry Laborato-
ries Within the Nuclear Industry
C1268 Test Method for Quantitative Determination of
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.
5
CurrenteditionapprovedJune1,2010.PublishedJuly2010.Originallyapproved For referenced ASTM standards, visit the ASTM website, www.astm.org, or
in 1972. Last previous edition approved in 2004 as C698–04. DOI: 10.1520/ contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
C0698-10. Standards volume information, refer to the standard’s Document Summary page on
2
Discontinued as of November 15, 1992. the ASTM website.
3 6
Discontinued as of May 30, 1980. The last approved version of this historical standard is referenced on
4
Discontinued as of January 1, 2004. www.astm.org.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
1
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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.
Designation:C698–04 Designation:C698–10
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
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 byAmperometric Titration with Iron (II)
Nitrogen by Distillation Spectrophotometry Using Nessler Re- 7to14
agent
Carbon (Total) by Direct Combustion-Thermal Conductivity 15 to 26
Total Chlorine and Fluorine by Pyrohydrolysis 27 to 34
Sulfur by Distillation-Spectrophotometry 35 to 43
Moisture by the Coulometric, Electrolytic MoistureAnalyzer 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
Impurities by Spark-Source Mass Spectrography 70 to 76
Total Gas in Reactor-Grade Mixed Dioxide Pellets 77 to 84
Tungsten by Dithiol-Spectrophotometry 85 to 93
Rare Earth Elements by Spectroscopy 94 to 97
4
Plutonium-238 IsotopicAbundance byAlpha Spectrometry
Americium-241 in Plutonium by Gamma-Ray Spectrometry
Uranium and Plutonium IsotopicAnalysis by Mass Spectrom- 98 to 106
etry
Oxygen-to-MetalAtom Ratio by Gravimetry 107 to 115
1.3
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 11, 20, 64, and 112 and 102.6.1.)
2. Referenced Documents
5
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
C1008 Specification for Sintered (Uranium-Plutonium) Dioxide PelletsFast Reactor Fuel
C1009 GuideforEstablishingaQualityAssuranceProgramforAnalyticalChemistryLaboratoriesWithintheNuclearIndustry
C1068 Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry
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 Jan.June 1, 2004.2010. Published February 2004.July 2010. Originally approved in 1972. Last previous edition approved in 19982004 as
C698–98.C698–04. DOI: 10.1520/C0698-104.
2
Discontinued as of November 15, 1992.
3
Discontinued as of May 30, 1980.
4
Discontinued as of January 1, 2004.
5
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book ofASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
1
---------------------- Page: 1 ----------------------
C698–10
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 Calibration for a Measurement Method Used to Analyze Nuclear Fuel Cycle Materials
C1165 TestMethodforDeterminingPlutoniumbyControlled-PotentialCoulometryinH SO ataPlatinumWorkingElectrode
2 4
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1204 Test Method for Uranium in Presence of Plutonium by Iron(II) Reduction in Phosphoric Acid Followed by
Chromium(VI) Titration
C1206 Test Method for Plutonium by Iron (II)/Chromium (
...
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