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).
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 |
| |
| Plutonium by Controlled-Potential Coulometry | |
| 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
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 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 radioactive fission products or high specific-activity gamma emitters.
95.1 This test method covers the determination of gamma-emitting fission products (for example, 95Zr-95Nb, 103Ru, 106Rh, and 137Cs-137mBa) and actinide impurities (232Th, 235U, and 238U) in plutonium nitrate. Test portions of plutonium nitrate are prepared to contain from 0.1 to 1.0 g of plutonium. The age of the plutonium after the last separation from actinides must be considered in calculating the actinide contents.
103.1 This test method covers the determination of rare earths in plutonium nitrate solutions in the range from 10 to 200 μg/g of plutonium.
106.1 This test method covers the determination of tungsten, niobium, and tantalum in plutonium nitrate solutions.
115.1 This test method covers the sample preparation for spectrographic analysis of plutonium nitrate for general metallic impurities by the carrier distillation test method.
2. Referenced Documents (purchase separately) 
The documents listed below are referenced within the subject standard but are not provided as part of the standard.
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
C1009 Guide for Establishing a Quality Assurance Program for Analytical Chemistry 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 H2SO4 at a Platinum Working Electrode
C1206 Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration
C1210 Guide for Establishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Within the Nuclear Industry
C1235 Test Method for Plutonium by Titanium(III)/Cerium(IV) Titration
C1268 Test Method for Quantitative Determination of Americium 241 in Plutonium by Gamma-Ray Spectrometry
C1297 Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle Materials
C1307 Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry
C1415 Test Method for 238Pu Isotopic Abundance By Alpha Spectrometry
C1432 Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
D1193 Specification for Reagent Water
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E115 Practice for Photographic Processing in Optical Emission Spectrographic Analysis
E116 Practice for Photographic Photometry in Spectrochemical Analysis
Keywords
impurity content; isotopic composition; plutonium content; plutonium nitrate; Actinide impurities content; Americium-241 (241Am) content; Chloride analysis--nuclear applications; Columbium content; Fission by-products--gamma emitting; Fluoride content; Free acid content; Gamma radiation; Iron content; Isotopic analysis; Mass spectrometry--nuclear materials/applications; Plutonium--isotopic analysis; Plutonium solutions; Radiochemical analysis; Rare earth content; Spectrochemical analysis; Tantalum (Ta) content; Thorium-232 content; Thorium content; Trace elements--spectrochemical analysis; Tungsten content; Uranium-235; Uranium-238; Uranium content ;
ICS Code
ICS Number Code 27.120.30 (Fissile materials and nuclear fuel technology)
DOI: 10.1520/C0759-10
ASTM International is a member of CrossRef.
Citing ASTM Standards
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