ASTM C1108-23

Standard Test Method for Plutonium by Controlled-Potential Coulometry

SIGNIFICANCE AND USE
5.1 Factors governing selection of a method for the determination of plutonium include available quantity of sample, sample purity, desired level of reliability, and equipment.  
5.1.1 This test method determines 5 mg to 20 mg of plutonium with prior dissolution using Practice C1168.  
5.1.2 This test method calculates plutonium mass fraction in solutions and solids using an electrical calibration based upon Ohm’s Law and the Faraday Constant.  
5.1.3 Chemical standards are used for quality control. When prior chemical separation of plutonium is necessary to remove interferences, the quality control standards should be included with each chemical separation batch (9).  
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.
SCOPE
1.1 This test method describes the determination of dissolved plutonium from unirradiated nuclear-grade (that is, high-purity) materials by controlled-potential coulometry. Controlled-potential coulometry may be performed in a choice of supporting electrolytes, such as 0.9 mol/L (0.9 M) HNO3, 1 mol/L (1 M) HClO4, 1 mol/L (1 M) HCl, 5 mol/L (5 M) HCl, and 0.5 mol/L (0.5 M) H2SO4. Limitations on the use of selected supporting electrolytes are discussed in Section 6. Optimum quantities of plutonium for this procedure are 5 mg to 20 mg.  
1.2 Plutonium-bearing materials are radioactive and toxic. Adequate laboratory facilities, such as gloved boxes, fume hoods, controlled ventilation, etc., along with safe techniques must be used in handling specimens containing these materials.  
1.3 The values stated in SI units are to be regarded as the 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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: C1108 − 23
Standard Test Method for
1
Plutonium by Controlled-Potential Coulometry
This standard is issued under the fixed designation C1108; 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 describes the determination of dis-
Nuclear Industry
solved plutonium from unirradiated nuclear-grade (that is,
C1068Guide for Qualification of Measurement Methods by
high-purity) materials by controlled-potential coulometry.
a Laboratory Within the Nuclear Industry
Controlled-potential coulometry may be performed in a choice
C1128Guide for Preparation of Working Reference Materi-
of supporting electrolytes, such as 0.9 mol/L (0.9 M) HNO ,
3
als for Use in Analysis of Nuclear Fuel Cycle Materials
1mol⁄L(1 M)HClO ,1mol⁄L(1 M)HCl,5mol/L(5 M)HCl,
4
C1156Guide for Establishing Calibration for a Measure-
and 0.5mol⁄L (0.5 M)H SO . Limitations on the use of
2 4
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
selected supporting electrolytes are discussed in Section 6.
rials
Optimum quantities of plutonium for this procedure are 5mg
C1168PracticeforPreparationandDissolutionofPlutonium
to 20 mg.
Materials for Analysis
1.2 Plutonium-bearing materials are radioactive and toxic.
C1210Guide for Establishing a Measurement System Qual-
Adequate laboratory facilities, such as gloved boxes, fume
ity Control Program for Analytical Chemistry Laborato-
hoods, controlled ventilation, etc., along with safe techniques
ries Within Nuclear Industry
mustbeusedinhandlingspecimenscontainingthesematerials.
C1297Guide for Qualification of Laboratory Analysts for
1.3 The values stated in SI units are to be regarded as the the Analysis of Nuclear Fuel Cycle Materials
E691Practice for Conducting an Interlaboratory Study to
standard. The values given in parentheses are for information
only. Determine the Precision of a Test Method
1.4 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Except as otherwise defined herein, definitions of terms
responsibility of the user of this standard to establish appro-
are as given in Terminology C859.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4. Summary of Test Method
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
4.1 In a controlled-potential coulometric measurement, the
ization established in the Decision on Principles for the
substancebeingdeterminedreactsatastationaryelectrode,the
Development of International Standards, Guides and Recom-
potential of which is maintained at such a value that unwanted
mendations issued by the World Trade Organization Technical
electrode reactions are precluded under the prevailing experi-
Barriers to Trade (TBT) Committee.
mental conditions. Those substances which have reduction-
oxidation (redox) potentials near that of the ion being deter-
2. Referenced Documents
mined constitute interferences. Electrolysis current decreases
2
2.1 ASTM Standards: exponentially as the reaction proceeds, until constant back-
C859Terminology Relating to Nuclear Materials
ground current is obtained. Detailed discussions of the theory
andapplicationsofthistechniquehavebeenpublished (1, 2, 3,
3
4, 5, 6). Thecontrol-potentialadjustmenttechnique (7)canbe
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
used to terminate the electrolysis of the specimen at constant
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
background current without exhaustive electrolysis with con-
Test.
siderable reduction in operating time. Use of the control-
Current edition approved Jan. 1, 2023. Published January 2023. Originally
approved in 1988. Last previous edition approved in 2022 as C1108–22. DOI:
potential adjustment technique requires that the coulometer
10.1520/C1108-23.
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 Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
the ASTM website. this test method.
Copyright © ASTM International, 100
...

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: C1108 − 22 C1108 − 23
Standard Test Method for
1
Plutonium by Controlled-Potential Coulometry
This standard is issued under the fixed designation C1108; 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 describes the determination of dissolved plutonium from unirradiated nuclear-grade (that is, high-purity)
materials by controlled-potential coulometry. Controlled-potential coulometry may be performed in a choice of supporting
electrolytes, such as 0.9 mol/L (0.9 M) HNO , 1 mol ⁄L (1 M) HClO , 1 mol ⁄L (1 M) HCl, 5 mol/L (5 M) HCl, and 0.5 mol ⁄L (0.5
3 4
M) H SO . Limitations on the use of selected supporting electrolytes are discussed in Section 6. Optimum quantities of plutonium
2 4
for this procedure are 5 mg to 20 mg.
1.2 Plutonium-bearing materials are radioactive and toxic. Adequate laboratory facilities, such as gloved boxes, fume hoods,
controlled ventilation, etc., along with safe techniques must be used in handling specimens containing these materials.
1.3 The values stated in SI units are to be regarded as the 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
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
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 Test Method for Determining Plutonium by Controlled-Potential Coulometry in H SO at a Platinum Working Electrode
2 4
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 1988. Last previous edition approved in 20172022 as
C1108 – 17.C1108 – 22. DOI: 10.1520/C1108-22.10.1520/C1108-23.
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

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C1108 − 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 a controlled-potential coulometric measurement, the substance being determined reacts at a stationary electrode, the
potential of which is maintained at such a value that unwanted electrode reactions are precluded under the prevailing experimental
conditions. Those substances which have reduction-oxidation (redox) potentials near that of the ion being determined constitute
interferences. Electrolysis current decreases exponentially as the reaction proceeds, until constant background c
...