ASTM C697 - 10

    Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets

    Active Standard ASTM C697 | Developed by Subcommittee: C26.05

    Book of Standards Volume: 12.01

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    Significance and Use

    Plutonium dioxide is used in mixtures with uranium dioxide as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for plutonium content, isotopic composition, and impurity content. These test methods are designed to show whether or not a given material meets the specifications for these items as described in Specification C757.

    An assay is performed to determine whether the material has the minimum plutonium content specified on a dry weight basis.

    Determination of the isotopic content of the plutonium in the plutonium dioxide powder is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.

    Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements 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, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets to determine compliance with specifications.

    1.2 The analytical procedures appear in the following order:

    Plutonium Sample Handling 8 to 10
    Plutonium by Controlled-Potential Coulometry
    Plutonium by Ceric Sulfate Titration
    Plutonium by Amperometric Titration with Iron(II)
    Plutonium by Diode Array   Spectrophotometry
    Nitrogen by Distillation Spectrophotometry Using Nessler
    11 to 18
    Carbon (Total) by Direct CombustionThermal Conductivity 19 to 30
    Total Chlorine and Fluorine by Pyrohydrolysis 31 to 38
    Sulfur by Distillation Spectrophotometry 39 to 47
    Plutonium Isotopic Analysis by Mass Spectrometry
    Rare Earth Elements by Spectroscopy 48 to 55
    Trace Elements by CarrierDistillation Spectroscopy 56 to 63
    Impurities by ICP-AES
    Impurity Elements by Spark-Source Mass Spectrography64 to 70
    Moisture by the Coulometric Electrolytic Moisture Analyzer71 to 78
    Total Gas in Reactor-Grade Plutonium Dioxide Pellets79 to 86
    Plutonium-238 Isotopic Abundance by Alpha Spectrometry
    Americium-241 in Plutonium by Gamma-Ray Spectrometry
    Rare Earths By Copper Spark-Spectroscopy87 to 96
    Plutonium Isotopic Analysis by Mass Spectrometry97 to 105
    Oxygen-To-Metal Atom Ratio by Gravimetry106 to 114

    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 precautionary statements, see Sections 6, 15, 24, 111, and 52.9 and 101.5.1 .

    8.1 This test method covers the conditions necessary to preserve the integrity of plutonium dioxide samples. Conditions listed here are directed toward the analytical chemist. However, they are just as applicable to any group handling the material.

    11.1 This test method covers the determination of 5 to 100 μg/g of nitride nitrogen in 1-g samples of nuclear-grade plutonium dioxide.

    19.1 This test method covers the determination of 10 to 200 μg of residual carbon in nuclear-grade plutonium dioxide.

    31.1 This test method covers the determination of 5 to 100 μg/g of chlorine and 1 to 100 μg/g of fluorine in 1-g samples of nuclear-grade plutonium dioxide.

    39.1 This test method coves the determination of sulfur in the concentration range from 10 to 600 μg/g for samples of nuclear-grade plutonium dioxide powders or pellets.

    48.1 This test method covers the determination of dysprosium, europium, gadolinium, and samarium in plutonium dioxide (PuO2) in concentrations of 0.1 to 10 μg/g of PuO2.

    FIG. 5 Schematic Diagram of Atmosphere Chamber

    56.1 This test method covers the determination of 36 impurity elements in nuclear-grade plutonium dioxide (PuO2). The concentration ranges covered by the method and the analytical lines used for each element are listed in Table 1.

    TABLE 1 Impurity Elements, Lines, and Concentration Limits

    ElementWavelength, Concentration
    Range, ppm
    (first order)
    (first order)
    (first order)

    A These elements are determined with the aid of a microphotometer.

    B These elements are analyzed by using a AgCl carrier and PdCl2 as an internal standard. Mix 20 mg of PdCl2 with 10.0 g of AgCl. Add 80 mg of this mixture to 120 mg of PuO2 sample-blend before loading 50-mg charges in a graphite electrode ASTM-Type-S-4 (follow 96.2.2).

    71.1 This test method covers the determination of moisture in plutonium dioxide samples. Detection limits are as low as 10 μg.

    79.1 This test method covers the measurement of volatiles other than water in reactor-grade plutonium dioxide pellets (16). The lower limit of the test method using the described equipment and a sample of approximately 1 g is 0.01 cm3 per gram of sample at STP conditions.

    87.1 This test method covers the determination of rare earths in plutonium dioxide over the range from 10 to 200 μg/g.

    97.1 This test method covers the determination of the isotopic composition of plutonium in nuclear-grade plutonium dioxide powders and pellets.

    106.1 This test method is applicable to the determination of the oxygen-to-metal atom ratio (O/M) in plutonium dioxide pellets and powders.

    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

    C757 Specification for Nuclear-Grade Plutonium Dioxide Powder, Sinterable

    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

    C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis

    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

    E60 Practice for Analysis of Metals, Ores, and Related Materials by Spectrophotometry

    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/C0697-10

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