ASTM C1165-12
(Test Method)Standard Test Method for Determining Plutonium by Controlled-Potential Coulometry in H2SO4 at a Platinum Working Electrode
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
This test method is to be used to ascertain whether or not materials meet specifications for plutonium content or plutonium assay, or both.
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 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 values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. Specific precautionary statements are given in Section 8.
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Designation: C1165 − 12
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 Nuclear-Grade Plutonium Nitrate Solutions
C833Specification for Sintered (Uranium-Plutonium) Diox-
1.1 This test method covers the determination of milligram
ide Pellets
quantities of plutonium in unirradiated uranium-plutonium
C859Terminology Relating to Nuclear Materials
mixed oxide having a U/Pu ratio range of 0.1 to 10. This test
C1009Guide for Establishing and Maintaining a Quality
methodisalsoapplicabletoplutoniummetal,plutoniumoxide,
AssuranceProgramforAnalyticalLaboratoriesWithinthe
uranium-plutonium mixed carbide, various plutonium com-
Nuclear Industry
pounds including fluoride and chloride salts, and plutonium
C1068Guide for Qualification of Measurement Methods by
solutions.
a Laboratory Within the Nuclear Industry
1.2 The recommended amount of plutonium for each ali-
C1108Test Method for Plutonium by Controlled-Potential
quant in the coulometric analysis is 5 to 10 mg. Precision
Coulometry
worsens for lower amounts of plutonium, and elapsed time of
C1128Guide for Preparation of Working Reference Materi-
electrolysis becomes impractical for higher amounts of pluto-
als for Use in Analysis of Nuclear Fuel Cycle Materials
nium.
C1156Guide for Establishing Calibration for a Measure-
1.3 The values stated in SI units are to be regarded as ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
rials
standard. No other units of measurement are included in this
standard. C1168PracticeforPreparationandDissolutionofPlutonium
Materials for Analysis
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-
C1297Guide for Qualification of Laboratory Analysts for
bility of regulatory limitations prior to use. Specific precau-
the Analysis of Nuclear Fuel Cycle Materials
tionary statements are given in Section 8.
2. Referenced Documents 3. Summary of Test Method
2
2.1 ASTM Standards: 3.1 In controlled-potential coulometry, the analyte reacts at
C757Specification for Nuclear-Grade Plutonium Dioxide an electrode having a maintained potential that precludes
Powder, Sinterable reactionsofasmanyimpuritycomponentsasisfeasible.Inthe
C758Test Methods for Chemical, Mass Spectrometric, electrolysis, current decreases exponentially as the reaction
Spectrochemical,Nuclear,andRadiochemicalAnalysisof proceeds until a selected background current is reached. The
Nuclear-Grade Plutonium Metal quantity of analyte reacted is calculable by Faraday’s law.
C759Test Methods for Chemical, Mass Spectrometric, Detailed discussions of the theory and applications of this
3
Spectrochemical,Nuclear,andRadiochemicalAnalysisof technique are presented in Refs (1) and (2).
3.2 Plutonium and many impurity element ions are initially
1
reduced in a 0.5 M H SO electrolyte at a platinum working
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
2 4
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
electrode (3) maintained at+0.310 V versus a saturated
Test.
calomelelectrode(SCE).PlutoniumisthenoxidizedtoPu(IV)
Current edition approved June 1, 2012. Published June 2012. Originally
at a potential of+0.670 V. The quantity of plutonium is
approved in 1990. Last previous edition approved in 2005 as C1165–90(2005).
DOI: 10.1520/C1165-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. 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
---------------------- Page: 1 ----------------------
C1165 − 12
calculatedfromthenumberofcoulombsrequiredforoxidation
according to Faraday’s law.
t
Q 5 * idt 5 nwF/M (1)
o
Rearrangement to solve for w gives:
w 5 MQ/nF (2)
where:
w = weight of Pu(III) oxidized to Pu(IV), g,
M = gram-molecular mass of plutonium (adjusted for isoto-
pic compositio
...
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:C1165–90(Reapproved2005) Designation:C1165–12
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
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 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 values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. Specific precautionary statements are given in Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder, Sinterable
C758 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Metal
C759 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Nitrate Solutions
C833 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets
C859 Terminology Relating to Nuclear Materials
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
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 forAnalytical Chemistry Laboratories Within
the Nuclear Industry
C1297 Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle Materials
3. Summary of Test Method
3.1 In controlled-potential coulometry, the analyte reacts at an electrode having a maintained 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’sFaraday’s law. Detailed
3
discussions of the theory and applications of this technique are presented in Refs (1) and (2).
3.2 Plutonium and many impurity element ions are initially reduced in a 0.5 M H SO electrolyte at a platinum working
2 4
electrode (3) maintained at+0.310 V versus a saturated calomel electrode (SCE). Plutonium is then oxidized to Pu(IV) at a
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.
´1
Current edition approved June 1, 2005. Published December 2005. Originally approved in 1990. Last previous edition approved in 2000 as C1165–90(2000) . DOI:
10.1520/C1165-90R05.
Current edition approved June 1, 2012. Published June 2012. Originally approved in 1990. Last previous edition approved in 2005 as C1165–90(2005). DOI:
10.1520/C1165-12.
2
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.
3
The boldface numbers in parentheses refer to a list of references at the end of the text.
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...
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