ASTM C697-16
(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
4.1 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.
4.1.1 An assay is performed to determine whether the material has the minimum plutonium content specified on a dry weight basis.
4.1.2 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.
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 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
2
Plutonium by Ceric Sulfate Titration
3
Plutonium by Amperometric Titration with Iron(II)
2
Plutonium by Diode Array Spectrophotometry
3
Nitrogen by Distillation Spectrophotometry Using Nessler
Reagent
11 to 18
Carbon (Total) by Direct Combustion–Thermal Conductivity
19 to 29
Total Chlorine and Fluorine by Pyrohydrolysis
30 to 37
Sulfur by Distillation Spectrophotometry
38 to 46
Plutonium Isotopic Analysis by Mass Spectrometry
4
Rare Earth Elements by Spectroscopy
47 to 54
Trace Elements by Carrier–Distillation Spectroscopy
55 to 62
(Alternative: Impurities by ICP-AES or ICP-MS)
Impurity Elements by Spark-Source Mass Spectrography
63 to 69
Moisture by the Coulometric Electrolytic Moisture Analyzer
70 to 77
Total Gas in Reactor-Grade Plutonium Dioxide Pellets
5
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
3
Americium-241 in Plutonium by Gamma-Ray Spectrometry
2
Rare Earths By Copper Spark-Spectroscopy
78 to 87
Plutonium Isotopic Analysis by Mass Spectrometry
88 to 96
Oxygen-To-Metal Atom Ratio by Gravimetry
97 to 104
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, 16.2.5, 44.7, 51.9 and 92.5.1.
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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: C697 − 16
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 bility of regulatory limitations prior to use. For specific
precautionarystatements,seeSections6,16.2.5,44.7,51.9and
1.1 These test methods cover procedures for the chemical,
92.5.1.
mass spectrometric, and spectrochemical analysis of nuclear-
grade plutonium dioxide powders and pellets to determine
2. Referenced Documents
compliance with specifications.
6
2.1 ASTM Standards:
1.2 Theanalyticalproceduresappearinthefollowingorder:
C757Specification for Nuclear-Grade Plutonium Dioxide
Sections
Powder for Light Water Reactors
Plutonium Sample Handling 8 to 10
2 C852Guide for Design Criteria for Plutonium Gloveboxes
Plutonium by Controlled-Potential Coulometry
3
Plutonium by Ceric Sulfate Titration C859Terminology Relating to Nuclear Materials
2
Plutonium by Amperometric Titration with Iron(II)
C1068Guide for Qualification of Measurement Methods by
3
Plutonium by Diode Array Spectrophotometry
a Laboratory Within the Nuclear Industry
Nitrogen by Distillation Spectrophotometry Using Nessler 11 to 18
Reagent C1108Test Method for Plutonium by Controlled-Potential
Carbon (Total) by Direct Combustion–Thermal Conductivity 19 to 29
Coulometry
Total Chlorine and Fluorine by Pyrohydrolysis 30 to 37
C1165 Test Method for Determining Plutonium by
Sulfur by Distillation Spectrophotometry 38 to 46
4
Plutonium Isotopic Analysis by Mass Spectrometry Controlled-Potential Coulometry in H SO at a Platinum
2 4
Rare Earth Elements by Spectroscopy 47 to 54
Working Electrode
Trace Elements by Carrier–Distillation Spectroscopy 55 to 62
C1168PracticeforPreparationandDissolutionofPlutonium
(Alternative: Impurities by ICP-AES or ICP-MS)
Impurity Elements by Spark-Source Mass Spectrography 63 to 69
Materials for Analysis
Moisture by the Coulometric Electrolytic Moisture Analyzer 70 to 77
C1206Test Method for Plutonium by Iron (II)/Chromium
5
Total Gas in Reactor-Grade Plutonium Dioxide Pellets
7
3
(VI) Amperometric Titration (Withdrawn 2015)
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
2
Americium-241 in Plutonium by Gamma-Ray Spectrometry
C1233Practice for Determining Equivalent Boron Contents
Rare Earths By Copper Spark-Spectroscopy 78 to 87
of Nuclear Materials
Plutonium Isotopic Analysis by Mass Spectrometry 88 to 96
C1235 Test Method for Plutonium by Titanium(III)/
Oxygen-To-Metal Atom Ratio by Gravimetry 97 to 104
7
Cerium(IV) Titration (Withdrawn 2005)
1.3 The values stated in SI units are to be regarded as
C1268 Test Method for Quantitative Determination of
standard. The values given in parentheses are for information
241
Am in Plutonium by Gamma-Ray Spectrometry
only.
C1307Test Method for PlutoniumAssay by Plutonium (III)
1.4 This standard does not purport to address all of the
Diode Array Spectrophotometry
safety concerns, if any, associated with its use. It is the 238
C1415Test Method for Pu Isotopic Abundance By Alpha
responsibility of the user of this standard to establish appro-
Spectrometry
priate safety and health practices and determine the applica-
C1432Test Method for Determination of Impurities in
Plutonium: Acid Dissolution, Ion Exchange Matrix
Separation, and Inductively Coupled Plasma-Atomic
1
These test methods are under the jurisdiction of ASTM Committee C26 on
Emission Spectroscopic (ICP/AES) Analysis
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 C697–10. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
C0697-16. contact ASTM Customer Service at service@astm.org. 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 January 1, 2004. the ASTM website.
4 7
Discontinued as of May 30, 1980. The last approved version of this historical standard is referenced on
5
Discontinued as of June 2016. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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...
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: C697 − 10 C697 − 16
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. 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
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
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
Carbon (Total) by Direct Combustion–Thermal Conductivity 19 to 29
Total Chlorine and Fluorine by Pyrohydrolysis 31 to 38
Total Chlorine and Fluorine by Pyrohydrolysis 30 to 37
Sulfur by Distillation Spectrophotometry 39 to 47
Sulfur by Distillation Spectrophotometry 38 to 46
4
Plutonium Isotopic Analysis by Mass Spectrometry
Rare Earth Elements by Spectroscopy 48 to 55
Rare Earth Elements by Spectroscopy 47 to 54
Trace Elements by Carrier–Distillation Spectroscopy 56 to 63
Trace Elements by Carrier–Distillation Spectroscopy 55 to 62
(Alternative: Impurities by ICP-AES or ICP-MS)
Impurity Elements by Spark-Source Mass Spectrography 64 to 70
Impurity Elements by Spark-Source Mass Spectrography 63 to 69
Moisture by the Coulometric Electrolytic Moisture Analyzer 71 to 78
Moisture by the Coulometric Electrolytic Moisture Analyzer 70 to 77
5
Total Gas in Reactor-Grade Plutonium Dioxide Pellets 79to 86
5
Total Gas in Reactor-Grade Plutonium Dioxide Pellets
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
Rare Earths By Copper Spark-Spectroscopy 78 to 87
Plutonium Isotopic Analysis by Mass Spectrometry 97 to 105
Plutonium Isotopic Analysis by Mass Spectrometry 88 to 96
Oxygen-To-Metal Atom Ratio by Gravimetry 106 to 114
Oxygen-To-Metal Atom Ratio by Gravimetry 97 to 104
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
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
C697 – 04.C697 – 10. DOI: 10.1520/C0697-10.10.1520/C0697-16.
2
Discontinued as of November 15, 1992.
3
Discontinued as of January 1, 2004.
4
Discontinued as of May 30, 1980.
5
Discontinued as of June 2016.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C697 − 16
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, 1516.2.5, 2444.7, 111, and 52.951.9 and
101.5.192.5.1.
2. Referenced Documents
6
2.1 ASTM Standards:
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder for Light Water Reactors
C852 Guide for Design Criteria for Plutonium Gloveboxes
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 Calibration for a Measurement Method Used to Analyze Nuclear Fuel Cycle Materials
C1
...
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