ASTM C759 - 10

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

    Active Standard ASTM C759 | Developed by Subcommittee: C26.05

    Book of Standards Volume: 12.01


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    ASTM C759

    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 Solution8 to 15
    Free Acid by Iodate Precipitation-Potentiometric Titration
    Test Method
    16 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 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


    ICS Code

    ICS Number Code 27.120.30 (Fissile materials and nuclear fuel technology)

    UNSPSC Code

    UNSPSC Code 15131500(Nuclear fuel)


    DOI: 10.1520/C0759-10

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