ASTM C1165-23

Standard Test Method for Determining Plutonium by Controlled-Potential Coulometry in H<inf>2</inf>SO<inf>4</inf> at a Platinum Working Electrode

SIGNIFICANCE AND USE
5.1 This test method is used to ascertain whether or not materials meet specifications for plutonium concentration or plutonium mass fraction.  
5.1.1 The materials (nuclear grade plutonium nitrate solutions, plutonium metal, plutonium oxide powder, and mixed oxide and carbide powders and pellets) to which this test method applies are subject to nuclear safeguards regulations governing their possession and use. However, adherence to this test method does not automatically guarantee regulatory acceptance of the resulting safeguards measurements. It remains the sole responsibility of the user of this test method to ensure that its application to safeguards has the approval of the proper regulatory authorities.  
5.1.2 When used in conjunction with appropriate certified reference materials (CRMs), this test method can demonstrate traceability to the international measurements system (SI).  
5.2 Fitness for Purpose of Safeguards and Nuclear Safety Application—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.  
5.3 A chemical calibration of the coulometer is necessary for accurate results.
FIG. 1 Example of a Cell Design Used at Los Alamos National Laboratory (LANL)
SCOPE
1.1 This test method covers the determination of milligram quantities of plutonium in unirradiated uranium-plutonium mixed oxide having a U/Pu ratio range of 0.1 to 10. This test method is also applicable to plutonium metal, plutonium oxide, uranium-plutonium mixed carbide, various plutonium compounds including fluoride and chloride salts, and plutonium solutions.  
1.2 The recommended amount of plutonium for each aliquant in the coulometric analysis is 5 mg to 10 mg. Precision worsens for lower amounts of plutonium, and elapsed time of electrolysis becomes impractical for higher amounts of plutonium.  
1.3 The quantity values stated in SI units are to be regarded as standard. The quantity values with non-SI units are given in parentheses 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.  
1.5 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-Dec-2022
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

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: C1165 − 23
Standard Test Method for
Determining Plutonium by Controlled-Potential Coulometry
1
in H SO at a Platinum Working Electrode
2 4
This standard is issued under the fixed designation C1165; 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 C1009Guide for Establishing and Maintaining a Quality
AssuranceProgramforAnalyticalLaboratoriesWithinthe
1.1 This test method covers the determination of milligram
Nuclear Industry
quantities of plutonium in unirradiated uranium-plutonium
C1068Guide for Qualification of Measurement Methods by
mixed oxide having a U/Pu ratio range of 0.1 to 10. This test
a Laboratory Within the Nuclear Industry
methodisalsoapplicabletoplutoniummetal,plutoniumoxide,
C1108Test Method for Plutonium by Controlled-Potential
uranium-plutonium mixed carbide, various plutonium com-
Coulometry
pounds including fluoride and chloride salts, and plutonium
C1128Guide for Preparation of Working Reference Materi-
solutions.
als for Use in Analysis of Nuclear Fuel Cycle Materials
1.2 The recommended amount of plutonium for each ali-
C1156Guide for Establishing Calibration for a Measure-
quant in the coulometric analysis is 5mg to 10 mg. Precision
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
worsens for lower amounts of plutonium, and elapsed time of
rials
electrolysis becomes impractical for higher amounts of pluto-
C1168PracticeforPreparationandDissolutionofPlutonium
nium.
Materials for Analysis
1.3 The quantity values stated in SI units are to be regarded C1210Guide for Establishing a Measurement System Qual-
ity Control Program for Analytical Chemistry Laborato-
as standard.The quantity values with non-SI units are given in
parentheses for information only. ries Within Nuclear Industry
C1297Guide for Qualification of Laboratory Analysts for
1.4 This standard does not purport to address all of the
the Analysis of Nuclear Fuel Cycle Materials
safety concerns, if any, associated with its use. It is the
E691Practice for Conducting an Interlaboratory Study to
responsibility of the user of this standard to establish appro-
Determine the Precision of a Test Method
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3. Terminology
Specific precautionary statements are given in Section 9.
3.1 Except as otherwise defined herein, definitions of terms
1.5 This international standard was developed in accor-
are as given in Terminology C859.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Summary of Test Method
Development of International Standards, Guides and Recom-
4.1 In controlled-potential coulometry, the analyte reacts at
mendations issued by the World Trade Organization Technical
an electrode having a controlled potential that precludes
Barriers to Trade (TBT) Committee.
reactionsofasmanyimpuritycomponentsasisfeasible.Inthe
2. Referenced Documents
electrolysis, current decreases exponentially as the reaction
2
proceeds until a selected background current is reached. The
2.1 ASTM Standards:
quantity of analyte reacted is calculable by Faraday’s law.
C859Terminology Relating to Nuclear Materials
Detailed discussions of the theory and applications of this
3
technique are presented in Refs (1) and (2).
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
4.2 Plutonium and many impurity element ions are initially
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
reducedina0.5mol/L(0.5 M)H SO electrolyteataplatinum
2 4
Current edition approved Jan. 1, 2023. Published January 2023. Originally
working electrode (3) maintained at+0.310V versus a satu-
approved in 1990. Last previous edition approved in 2022 as C1165–22. DOI:
rated calomel electrode (SCE). Plutonium is then oxidized to
10.1520/C1165-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to a list of references at the end of
the ASTM website. the text.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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C1165 − 23
Pu(IV) at a poten
...

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: C1165 − 22 C1165 − 23
Standard Test Method for
Determining Plutonium by Controlled-Potential Coulometry
1
in H SO at a Platinum Working Electrode
2 4
This standard is issued under the fixed designation C1165; 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 This test method covers the determination of milligram quantities of plutonium in unirradiated uranium-plutonium mixed
oxide having a U/Pu ratio range of 0.1 to 10. This test method is also applicable to plutonium metal, plutonium oxide,
uranium-plutonium mixed carbide, various plutonium compounds including fluoride and chloride salts, and plutonium solutions.
1.2 The recommended amount of plutonium for each aliquant in the coulometric analysis is 5 mg to 10 mg. Precision worsens for
lower amounts of plutonium, and elapsed time of electrolysis becomes impractical for higher amounts of plutonium.
1.3 The quantity values stated in SI units are to be regarded as standard. The quantity values with non-SI units are given in
parentheses 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. Specific precautionary statements are given in Section 9.
1.5 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.
2. Referenced Documents
2
2.1 ASTM Standards:
C859 Terminology Relating to Nuclear Materials
C1009 Guide for Establishing and Maintaining a Quality Assurance Program for Analytical Laboratories Within the Nuclear
Industry
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
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1210 Guide for Establishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Within
Nuclear Industry
C1297 Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle Materials
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved July 1, 2022Jan. 1, 2023. Published August 2022January 2023. Originally approved in 1990. Last previous edition approved in 20172022 as
C1165 – 17.C1165 – 22. DOI: 10.1520/C1165-22.10.1520/C1165-23.
2
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1165 − 23
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Except as otherwise defined herein, definitions of terms are as given in Terminology C859.
4. Summary of Test Method
4.1 In controlled-potential coulometry, the analyte reacts at an electrode having a controlled potential that precludes reactions of
as many impurity components as is feasible. In the electrolysis, current decreases exponentially as the reaction proceeds until a
selected background current is reached. The quantity of analyte reacted is calculable by Faraday’s law. Detailed discussions of the
3
theory and applications of this technique are presented in Refs (1) and (2).
4.2 Plutonium and many impurity element ions are initially reduced in a 0.5 mol/L (0.5 M) H SO electrolyte at a platinum
2
...