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

SIGNIFICANCE AND USE
These test methods are designed to show whether a given material meets the purchaser's specifications.
An assay is performed to determine whether the material has the specified plutonium content.
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.
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).
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  Plutonium by Amperometric Titration with Iron(II)  Plutonium by Diode Array Spectrophotometry Free Acid by Titration in an Oxalate Solution8 to 15 Free Acid by Iodate Precipitation-Potentiometric Titration
Test Method16 to 22 Uranium by Arsenazo I Spectrophotometric Test Method23 to 33 Thorium by Thorin Spectrophotometric Test Method34 to 42 Iron by 1,10-Phenanthroline Spectrophotometric Test Method43 to 50 Impurities by ICP-AES Chloride by Thiocyanate Spectrophotometric Test Method51 to 58 Fluoride by Distillation-Spectrophotometric Test Method59 to 66 Sulfate by Barium Sulfate Turbidimetric Test Method67 to 74 Isotopic Composition by Mass Spectrometry75 to 76 Plutonium 238 Isotopic Abundance by Alpha Spectrometry Americium-241 by Extraction and Gamma Counting77 to 85 Americium-241 by Gamma Counting86 to 94 Gamma-Emitting Fission Products, Uranium, and Thorium by Gamma-Ray Spectroscopy94 to 102 Rare Earths by Copper Spark Spectrochemical Test Method103 to 105 Tungsten, Niobium (Columbium), and Tantalum by Spectro
chemical Test Method106 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific safeguard and safety hazard statements, see Section 6.  
8.1 This test method covers the determination of free acid in plutonium nitrate solutions (4, 5).  
16.1 This test method covers the determination of free acid in strong acid solutions of plutonium nitrate.  
23.1 This test method covers the determination of uranium in the range from 300 to 3000 μg/g of plutonium in plutonium nitrate solutions.  
34.1 This test method covers the determination of 10 to 150 μg of thorium per gram of plutonium in plutonium nitrate solutions.  
43.1 This test method covers the determination of microgram quantities of iron in plutonium nitrate solutions.  
51.1 This test method (9) is used to determine chloride in plutonium nitrate solution.  
59.1 This test method covers the determination of microquantities of fluoride in plutonium nitrate solutions.  
67.1 This test procedure covers the determination of the sulfate concentration in plutonium nitrate solutions in the range from 50 to 700 μg/g of plutonium.  
75.1 This test method covers the determination of the isotopic content of nuclear-grade plutonium nitrate solutions.  
77.1 This test method covers the determination of americium-241 in plutonium nitrate solutions.  
86.1 This test method covers the determination of americium-241 in plutonium nitrate solutions that do not contain significant amounts of other radioa...

General Information

Status
Historical
Publication Date
31-May-2010
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM C759-10 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: C759 − 10
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 bility of regulatory limitations prior to use. For specific
safeguard and safety hazard statements, see Section 6.
1.1 These test methods cover procedures for the chemical,
mass spectrometric, spectrochemical, nuclear, and radiochemi-
2. Referenced Documents
cal analysis of nuclear-grade plutonium nitrate solutions to
3
2.1 ASTM Standards:
determine compliance with specifications.
C697Test Methods for Chemical, Mass Spectrometric, and
1.2 Theanalyticalproceduresappearinthefollowingorder:
Spectrochemical Analysis of Nuclear-Grade Plutonium
Sections
Dioxide Powders and Pellets
2 C852Guide for Design Criteria for Plutonium Gloveboxes
Plutonium by Controlled-Potential Coulometry
2
Plutonium by Amperometric Titration with Iron(II) C1009Guide for Establishing and Maintaining a Quality
Plutonium by Diode Array Spectrophotometry
AssuranceProgramforAnalyticalLaboratoriesWithinthe
Free Acid by Titration in an Oxalate Solution 8 to 15
Nuclear Industry
Free Acid by Iodate Precipitation-Potentiometric Titration 16 to 22
Test Method C1068Guide for Qualification of Measurement Methods by
Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33
a Laboratory Within the Nuclear Industry
Thorium by Thorin Spectrophotometric Test Method 34 to 42
C1108Test Method for Plutonium by Controlled-Potential
Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50
Impurities by ICP-AES Coulometry
Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58
C1128Guide for Preparation of Working Reference Materi-
Fluoride by Distillation-Spectrophotometric Test Method 59 to 66
als for Use in Analysis of Nuclear Fuel Cycle Materials
Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74
Isotopic Composition by Mass Spectrometry 75 to 76
C1156Guide for Establishing Calibration for a Measure-
Plutonium —238 Isotopic Abundance by Alpha Spectrometry
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
Americium-241 by Extraction and Gamma Counting 77 to 85
rials
Americium-241 by Gamma Counting 86 to 94
Gamma-Emitting Fission Products, Uranium, and Thorium by 94 to 102
C1165 Test Method for Determining Plutonium by
Gamma-Ray Spectroscopy
Controlled-Potential Coulometry in H SO at a Platinum
2 4
Rare Earths by Copper Spark Spectrochemical Test Method 103 to 105
Working Electrode
Tungsten, Niobium (Columbium), and Tantalum by Spectro 106 to 114
chemical Test Method
C1206Test Method for Plutonium by Iron (II)/Chromium
Sample Preparation for Spectrographic Analysis for General 115 to 118 4
(VI) Amperometric Titration (Withdrawn 2015)
Impurities
C1210Guide for Establishing a Measurement System Qual-
1.3 The values stated in SI units are to be regarded as
ity Control Program for Analytical Chemistry Laborato-
standard. The values given in parentheses are for information
ries Within the Nuclear Industry
only.
C1235 Test Method for Plutonium by Titanium(III)/
4
1.4 This standard does not purport to address all of the
Cerium(IV) Titration (Withdrawn 2005)
safety concerns, if any, associated with its use. It is the
C1268 Test Method for Quantitative Determination of
241
responsibility of the user of this standard to establish appro-
Am in Plutonium by Gamma-Ray Spectrometry
priate safety and health practices and determine the applica-
C1297Guide for Qualification of Laboratory Analysts for
the Analysis of Nuclear Fuel Cycle Materials
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
CurrenteditionapprovedJune1,2010.PublishedJuly2010.Originallyapproved Standardsvolume information, refer to the standard’s Document Summary page on
in 1973. Last previous edition approved in 2004 as C759–04. DOI: 10.1520/ the ASTM website
4
C0759-10. 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 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C759 − 10
C1307Test Method for PlutoniumAssay by Plut
...

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:C759–04 Designation:C759–10
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
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
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
Sample Preparation for Spectrographic Analysis for General 115to118
Impurities123 to 126
Sample Preparation for Spectrographic Analysis for General 115to118
Impurities
1.3
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 safeguard and safety hazard statements, see Section 6.
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
C852 Guide for Design Criteria for Plutonium Gloveboxes
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 Jan.June 1, 2004.2010. Published February 2004.July 2010. Originally approved in 1973. Last previous edition approved in 19982004 as
C759–98.C759–04. DOI: 10.1520/C0759-104.
2
Discontinued as of November 15, 1992.
3
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
Standardsvolume 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 ----------------------
C759–10
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
C1165 TestMethodforDeterminingPlutoniumbyControlled-PotentialCoulometryinH SO ataPlatinumWorkingElectrode
2 4
C1206 Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration
C1210 Guide for Establishing a Measurement System Quality Control Program forAnalytical Chemistry Laboratories Within
the Nuclear Industry
C1235 Test Method for Plutonium by
...

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