Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions

SIGNIFICANCE AND USE
4.1 These test methods are designed to show whether a given material meets the purchaser's specifications.  
4.1.1 An assay is performed to determine whether the material has the specified plutonium content.  
4.1.2 Determination of the isotopic content of the plutonium in the plutonium-nitrate solution is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.  
4.1.3 Impurity content is determined by a variety of methods to ensure that the maximum concentration limit of specified impurities is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC).  
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, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications.  
1.2 The analytical procedures appear in the following order:    
Sections  
Plutonium by Controlled-Potential Coulometry  
2  
Plutonium by Amperometric Titration with Iron(II)  
2  
Plutonium by Diode Array Spectrophotometry  
Free Acid by Titration in an Oxalate Solution  
8 to 15  
Free Acid by Iodate Precipitation-Potentiometric Titration
Test Method  
16 to 22  
Uranium by Arsenazo I Spectrophotometric Test Method  
23 to 33  
Thorium by Thorin Spectrophotometric Test Method  
34 to 42  
Iron by 1,10-Phenanthroline Spectrophotometric Test Method  
43 to 50  
Impurities by ICP-AES  
Chloride by Thiocyanate Spectrophotometric Test Method  
51 to 58  
Fluoride by Distillation-Spectrophotometric Test Method  
59 to 66  
Sulfate by Barium Sulfate Turbidimetric Test Method  
67 to 74  
Isotopic Composition by Mass Spectrometry  
75 to 76  
Plutonium-238 Isotopic Abundance by Alpha Spectrometry  
Americium-241 by Extraction and Gamma Counting  
77 to 85  
Americium-241 by Gamma Counting  
86 to 94  
Gamma-Emitting Fission Products, Uranium, and Thorium by Gamma-Ray Spectroscopy  
94 to 102  
Rare Earths by Copper Spark Spectrochemical Test Method  
103 to 105  
Tungsten, Niobium (Columbium), and Tantalum by Spectro-
chemical Test Method  
106 to 114  
Sample Preparation for Spectrographic Analysis for General
Impurities  
115 to 118  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific safeguard and safety hazard statements, see Section 6.  
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-Aug-2018
Technical Committee
Drafting Committee
Current Stage
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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: C759 − 18
Standard Test Methods for
Chemical, Mass Spectrometric, Spectrochemical, Nuclear,
and Radiochemical Analysis of Nuclear-Grade Plutonium
1
Nitrate Solutions
This standard is issued under the fixed designation C759; 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 mine the applicability of regulatory limitations prior to use.
For specific safeguard and safety hazard statements, see
1.1 These test methods cover procedures for the chemical,
Section 6.
mass spectrometric, spectrochemical, nuclear, and radiochemi-
1.5 This international standard was developed in accor-
cal analysis of nuclear-grade plutonium nitrate solutions to
dance with internationally recognized principles on standard-
determine compliance with specifications.
ization established in the Decision on Principles for the
1.2 Theanalyticalproceduresappearinthefollowingorder:
Development of International Standards, Guides and Recom-
Sections
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2
Plutonium by Controlled-Potential Coulometry
2
Plutonium by Amperometric Titration with Iron(II)
2. Referenced Documents
Plutonium by Diode Array Spectrophotometry
Free Acid by Titration in an Oxalate Solution 8 to 15
3
2.1 ASTM Standards:
Free Acid by Iodate Precipitation-Potentiometric Titration 16 to 22
Test Method C697Test Methods for Chemical, Mass Spectrometric, and
Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33
Spectrochemical Analysis of Nuclear-Grade Plutonium
Thorium by Thorin Spectrophotometric Test Method 34 to 42
Dioxide Powders and Pellets
Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50
Impurities by ICP-AES C852/C852M Guide for Design Criteria for Plutonium
Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58
Gloveboxes
Fluoride by Distillation-Spectrophotometric Test Method 59 to 66
C859Terminology Relating to Nuclear Materials
Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74
Isotopic Composition by Mass Spectrometry 75 to 76
C1009Guide for Establishing and Maintaining a Quality
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
AssuranceProgramforAnalyticalLaboratoriesWithinthe
Americium-241 by Extraction and Gamma Counting 77 to 85
Nuclear Industry
Americium-241 by Gamma Counting 86 to 94
Gamma-Emitting Fission Products, Uranium, and Thorium by 94 to 102
C1068Guide for Qualification of Measurement Methods by
Gamma-Ray Spectroscopy
a Laboratory Within the Nuclear Industry
Rare Earths by Copper Spark Spectrochemical Test Method 103 to 105
C1108Test Method for Plutonium by Controlled-Potential
Tungsten, Niobium (Columbium), and Tantalum by Spectro- 106 to 114
chemical Test Method
Coulometry
Sample Preparation for Spectrographic Analysis for General 115 to 118
C1128Guide for Preparation of Working Reference Materi-
Impurities
als for Use in Analysis of Nuclear Fuel Cycle Materials
1.3 The values stated in SI units are to be regarded as
C1156Guide for Establishing Calibration for a Measure-
standard. The values given in parentheses are for information
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
only.
rials
1.4 This standard does not purport to address all of the
C1165 Test Method for Determining Plutonium by
safety concerns, if any, associated with its use. It is the
Controlled-Potential Coulometry in H SO at a Platinum
2 4
responsibility of the user of this standard to establish appro-
Working Electrode
priate safety, health, and environmental practices and deter-
C1206Test Method for Plutonium by Iron (II)/Chromium
4
(VI) Amperometric Titration (Withdrawn 2015)
1
These test methods are under the jurisdiction of ASTM Committee C26 on
3
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Methods of Test. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Sept. 1, 2018. Published October 2018. Originally Standardsvolume information, refer to the standard’s Document Summary page on
approved in 1973. Last previous edition approved in 2010 as C759–10. DOI: the ASTM website
4
10.1520/C0759-18. The last approved version of this historical standard is referenced on
2
Discontinued as of November 15, 1992. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19
...

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: C759 − 10 C759 − 18
Standard Test Methods for
Chemical, Mass Spectrometric, Spectrochemical, Nuclear,
and Radiochemical Analysis of Nuclear-Grade Plutonium
1
Nitrate Solutions
This standard is issued under the fixed designation C759; 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, spectrochemical, nuclear, and radiochemical
analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications.
1.2 The analytical procedures appear in the following order:
Sections
2
Plutonium by Controlled-Potential Coulometry
2
Plutonium by Amperometric Titration with Iron(II)
Plutonium by Diode Array Spectrophotometry
Free Acid by Titration in an Oxalate Solution 8 to 15
Free Acid by Iodate Precipitation-Potentiometric Titration 16 to 22
Test Method
Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33
Thorium by Thorin Spectrophotometric Test Method 34 to 42
Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50
Impurities by ICP-AES
Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58
Fluoride by Distillation-Spectrophotometric Test Method 59 to 66
Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74
Isotopic Composition by Mass Spectrometry 75 to 76
Plutonium —238 Isotopic Abundance by Alpha Spectrometry
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
Americium-241 by Extraction and Gamma Counting 77 to 85
Americium-241 by Gamma Counting 86 to 94
Gamma-Emitting Fission Products, Uranium, and Thorium by 94 to 102
Gamma-Ray Spectroscopy
Rare Earths by Copper Spark Spectrochemical Test Method 103 to 105
Tungsten, Niobium (Columbium), and Tantalum by Spectro 106 to 114
chemical Test Method
Tungsten, Niobium (Columbium), and Tantalum by Spectro- 106 to 114
chemical Test Method
Sample Preparation for Spectrographic Analysis for General 115 to 118
Impurities
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific safeguard and safety hazard statements, see Section 6.
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.
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, 2010Sept. 1, 2018. Published July 2010October 2018. Originally approved in 1973. Last previous edition approved in 20042010 as
C759 – 04.C759 – 10. DOI: 10.1520/C0759-10.10.1520/C0759-18.
2
Discontinued as of November 15, 1992.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C759 − 18
2. Referenced Documents
3
2.1 ASTM Standards:
C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide
Powders and Pellets
C852C852/C852M Guide for Design Criteria for Plutonium Gloveboxes
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
C1165 Test Method for Determining Plutonium by Controlled-Potential Coulometry in H SO at a Platinum Working
...

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