ASTM C697-10
(Test Method)Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets
Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets
SIGNIFICANCE AND USE
Plutonium dioxide is used in mixtures with uranium dioxide as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for plutonium content, 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 Specification C757.
An assay is performed to determine whether the material has the minimum plutonium content specified on a dry weight basis.
Determination of the isotopic content of the plutonium in the plutonium 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 plutonium dioxide powders and pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
Sections Plutonium Sample Handling 8 to 10 Plutonium by Controlled-Potential Coulometry Plutonium by Ceric Sulfate Titration Plutonium by Amperometric Titration with Iron(II) Plutonium by Diode Array Spectrophotometry Nitrogen by Distillation Spectrophotometry Using Nessler
Reagent 11 to 18 Carbon (Total) by Direct Combustion–Thermal Conductivity 19 to 30 Total Chlorine and Fluorine by Pyrohydrolysis 31 to 38 Sulfur by Distillation Spectrophotometry 39 to 47 Plutonium Isotopic Analysis by Mass Spectrometry Rare Earth Elements by Spectroscopy 48 to 55 Trace Elements by Carrier–Distillation Spectroscopy 56 to 63 Impurities by ICP-AES Impurity Elements by Spark-Source Mass Spectrography64 to 70 Moisture by the Coulometric Electrolytic Moisture Analyzer71 to 78 Total Gas in Reactor-Grade Plutonium Dioxide Pellets79 to 86 Plutonium-238 Isotopic Abundance by Alpha Spectrometry Americium-241 in Plutonium by Gamma-Ray Spectrometry Rare Earths By Copper Spark-Spectroscopy87 to 96 Plutonium Isotopic Analysis by Mass Spectrometry97 to 105 Oxygen-To-Metal Atom Ratio by Gravimetry106 to 114
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 precautionary statements, see Sections 6, 15, 24, 111, and 52.9 and 101.5.1 .
8.1 This test method covers the conditions necessary to preserve the integrity of plutonium dioxide samples. Conditions listed here are directed toward the analytical chemist. However, they are just as applicable to any group handling the material.
11.1 This test method covers the determination of 5 to 100 μg/g of nitride nitrogen in 1-g samples of nuclear-grade plutonium dioxide.
19.1 This test method covers the determination of 10 to 200 μg of residual carbon in nuclear-grade plutonium dioxide.
31.1 This test method covers the determination of 5 to 100 μg/g of chlorine and 1 to 100 μg/g of fluorine in 1-g samples of nuclear-grade plutonium dioxide.
39.1 This test method coves the determination of sulfur in the concentration range from 10 to 600 μg/g for samples of nuclear-grade plutonium dioxide powders or pellets.
48.1 This test method covers the determination of dysprosium, europium, gadolinium, and samarium in plutonium dioxide (PuO2) in concentrations of 0.1 to 10 μg/g of PuO2.
FIG. 5 Schematic Diagram of Atmosphere Chamber
56.1 This test method covers the determination of 36 impurity elemen...
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Designation: C697 − 10
StandardTest Methods for
Chemical, Mass Spectrometric, and Spectrochemical
Analysis of Nuclear-Grade Plutonium Dioxide Powders and
1
Pellets
This standard is issued under the fixed designation C697; 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 bility of regulatory limitations prior to use. For specific
precautionary statements, see Sections 6, 15, 24, 111, and 52.9
1.1 These test methods cover procedures for the chemical,
and 101.5.1 .
mass spectrometric, and spectrochemical analysis of nuclear-
grade plutonium dioxide powders and pellets to determine
2. Referenced Documents
compliance with specifications.
5
2.1 ASTM Standards:
1.2 Theanalyticalproceduresappearinthefollowingorder:
C757Specification for Nuclear-Grade Plutonium Dioxide
Sections
Powder, Sinterable
Plutonium Sample Handling 8 to 10
C852Guide for Design Criteria for Plutonium Gloveboxes
2
Plutonium by Controlled-Potential Coulometry
3
C1009Guide for Establishing and Maintaining a Quality
Plutonium by Ceric Sulfate Titration
2
Plutonium by Amperometric Titration with Iron(II)
AssuranceProgramforAnalyticalLaboratoriesWithinthe
3
Plutonium by Diode Array Spectrophotometry
Nuclear Industry
Nitrogen by Distillation Spectrophotometry Using Nessler 11 to 18
C1068Guide for Qualification of Measurement Methods by
Reagent
Carbon (Total) by Direct Combustion–Thermal Conductivity 19 to 30
a Laboratory Within the Nuclear Industry
Total Chlorine and Fluorine by Pyrohydrolysis 31 to 38
C1108Test Method for Plutonium by Controlled-Potential
Sulfur by Distillation Spectrophotometry 39 to 47
4
Coulometry
Plutonium Isotopic Analysis by Mass Spectrometry
Rare Earth Elements by Spectroscopy 48 to 55
C1128Guide for Preparation of Working Reference Materi-
Trace Elements by Carrier–Distillation Spectroscopy 56 to 63
als for Use in Analysis of Nuclear Fuel Cycle Materials
Impurities by ICP-AES
Impurity Elements by Spark-Source Mass Spectrography 64 to 70 C1156Guide for Establishing Calibration for a Measure-
Moisture by the Coulometric Electrolytic Moisture Analyzer 71 to 78
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
Total Gas in Reactor-Grade Plutonium Dioxide Pellets 79 to 86
3 rials
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
2
Americium-241 in Plutonium by Gamma-Ray Spectrometry C1165 Test Method for Determining Plutonium by
Rare Earths By Copper Spark-Spectroscopy 87 to 96
Controlled-Potential Coulometry in H SO at a Platinum
2 4
Plutonium Isotopic Analysis by Mass Spectrometry 97 to 105
Working Electrode
Oxygen-To-Metal Atom Ratio by Gravimetry 106 to 114
C1168PracticeforPreparationandDissolutionofPlutonium
1.3 The values stated in SI units are to be regarded as
Materials for Analysis
standard. The values given in parentheses are for information
C1206Test Method for Plutonium by Iron (II)/Chromium
only.
6
(VI) Amperometric Titration (Withdrawn 2015)
1.4 This standard does not purport to address all of the
C1210Guide for Establishing a Measurement System Qual-
safety concerns, if any, associated with its use. It is the
ity Control Program for Analytical Chemistry Laborato-
responsibility of the user of this standard to establish appro-
ries Within the Nuclear Industry
priate safety and health practices and determine the applica-
C1235 Test Method for Plutonium by Titanium(III)/
6
Cerium(IV) Titration (Withdrawn 2005)
C1268 Test Method for Quantitative Determination of
241
1 Am in Plutonium by Gamma-Ray Spectrometry
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 C697–04. DOI: 10.1520/ contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
C0697-10. 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 January 1, 2004. The last approved version of this historical standard is referenced on
4
Discontinued as of May 30, 1980. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C697 − 10
C1297Guide for Qualification of Laboratory Analysts for ments.Itremainsthesoleresponsibilityoftheuserofthesetest
the Analysis of Nuclear Fuel Cycle Materials meth
...
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:C697–04 Designation:C697–10
Standard Test Methods for
Chemical, Mass Spectrometric, and Spectrochemical
Analysis of Nuclear-Grade Plutonium Dioxide Powders and
1
Pellets
This standard is issued under the fixed designation C697; 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
plutonium dioxide powders and pellets to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
Sections
Plutonium Sample Handling 8to10
2
Plutonium by Controlled-Potential Coulometry
3
Plutonium by Ceric Sulfate Titration
2
Plutonium by Amperometric Titration with Iron(II)
3
Plutonium by Diode Array Spectrophotometry
Nitrogen by Distillation Spectrophotometry Using Nessler 11 to 18
Reagent
Carbon (Total) by Direct Combustion–Thermal Conductivity 19 to 30
Total Chlorine and Fluorine by Pyrohydrolysis 31 to 38
Sulfur by Distillation Spectrophotometry 39 to 47
4
Plutonium Isotopic Analysis by Mass Spectrometry
Rare Earth Elements by Spectroscopy 48 to 55
Trace Elements by Carrier–Distillation Spectroscopy 56 to 63
Impurities by ICP-AES
Impurity Elements by Spark-Source Mass Spectrography 64 to 70
Moisture by the Coulometric Electrolytic Moisture Analyzer 71 to 78
Total Gas in Reactor-Grade Plutonium Dioxide Pellets 79 to 86
3
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
2
Americium-241 in Plutonium by Gamma-Ray Spectrometry
Rare Earths By Copper Spark-Spectroscopy 87 to 96
Plutonium Isotopic Analysis by Mass Spectrometry 97 to 105
Oxygen-To-Metal Atom Ratio by Gravimetry 106 to 114
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 precautionary statements, see Sections 6, 15, 24, 111, and 52.9 and 101.5.1 .
2. Referenced Documents
5
2.1 ASTM Standards:
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder, Sinterable
C852 Guide for Design Criteria for Plutonium Gloveboxes
C1009 GuideforEstablishingaQualityAssuranceProgramforAnalyticalChemistryLaboratoriesWithintheNuclearIndustry
C1068 Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry
C1108 Test Method for Plutonium by Controlled-Potential Coulometry
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
C697–98.C697–04. DOI: 10.1520/C0697-104.
2
Discontinued as of November 15, 1992.
3
Discontinued as of January 1, 2004.
4
Discontinued as of May 30, 1980.
5
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM 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, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
C697–10
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
C1206 Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration
C1210 Guide for Establishing a Measurement System Quality Control Program forAnalytical Chemistry Laboratories Within
the Nuclear Industry
C1235 Test Method for Plutonium by Titanium(III)/Cerium(IV) Titration
C1268 Test Method for Quantitative Determination of Americium 241 in Plutonium
...
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