ASTM C696 - 11

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

    Active Standard ASTM C696 | Developed by Subcommittee: C26.05

    Book of Standards Volume: 12.01


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    ASTM C696

    Significance and Use

    Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, 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 Specifications C753 and C776.

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

    The stoichiometry of the oxide is useful for predicting its sintering behavior in the pellet production process.

    Determination of the isotopic content of the uranium in the uranium 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 uranium dioxide powders and pellets to determine compliance with specifications.

    1.2 The analytical procedures appear in the following order:

    Sections
    Uranium by Ferrous Sulfate Reduction in Phosphoric Acid and Dichromate Titration Method
    C1267 Test Method for Uranium By Iron (II) Reduction In Phosphoric Acid Followed By Chromium (VI) Titration In The Presence of Vanadium
    Uranium and Oxygen Uranium Atomic Ratio by the Ignition (Gravimetric) Impurity Correction Method
    C1453 Standard Test Method for the Determination of Uranium by Ignition and Oxygen to Uranium Ratio (O/U) Atomic Ratio of Nuclear Grade Uranium Dioxide Powders and Pellets
    Carbon (Total) by Direct Combustion-Thermal Conductivity Method
    C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
    Total Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method
    C1502 Standard Test Method for the Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide    
    Moisture by the Coulometric, Electrolytic Moisture Analyzer Method7-14
    Nitrogen by the Kjeldahl Method15-22
    Isotopic Uranium Composition by Multiple-Filament Surface Ionization Mass Spectrometric Method
    Spectrochemical Determination of Trace Elements in High-Purity Uranium Dioxide23-30
    Silver, Spectrochemical Determination of, by Gallium OxideCarrier D-C Arc Technique31 and 32
    Rare Earths by Copper Spark-Spectrochemical Method
    Impurity Elements by a Spark-Source Mass Spectrographic Method
    C761 Test Method for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
    C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry
    Surface Area by Nitrogen Absorption Method33-39
    Total Gas in Reactor-Grade Uranium Dioxide Pellets
    Thorium and Rare Earth Elements by Spectroscopy
    Hydrogen by Inert Gas Fusion
    C1457 Standard Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by     Carrier Gas Extraction    
    Uranium Isotopic Analysis by Mass Spectrometry
    C1413 Test Method for Isotopic Analysis of Hydrolysed Uranium Hexafluoride and Uranyl Nitrate Solutions By Thermal Ionization Mass Spectrometry

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

    15.1 This test method covers the determination of nitride nitrogen in uranium dioxide in the range from 10 to 250 μg.

    23.1 This test method covers the spectrographic analysis of nuclear-grade UO2 for the 26 elements in the ranges indicated in Table 1.

    23.2 For simultaneous determination of trace elements by plasma emission spectroscopy refer to Test Method C761.

    TABLE 1 Recommended Analytical Spectral Lines and Concentration Range of Trace Elements

    ElementAnalytical Line,
    °AA
    Concentration range, μg/g of U
    AgB 3280.68 0.1 to 50
    Al 2367.06 10 to 200
    As 2349.84 5 to 50
    B 2497.73 0.10 to 5
    Ba 4554.04 10 to 300
    Be 2348.61 0.1 to 3
    Bi 3067.72 5 to 50
    Ca 4226.73 1 to 50
    Cd 2288.02 0.15 to 5
    Co 3453.51 5 to 50
    Cr 2843.25 10 to 100
    Cu 3247.54 1 to 10
    Fe 2462.64 10 to 300
    In 3256.09 5 to 50
    Mg 2779.83 10 to 100
    Mn 2605.69 5 to 50
    Mo 3132.59 0.5 to 10
    Na 3302.32 80 to 400
    Ni 3050.82 5 to 100
    P 2553.28 50 to 500
    Pb 2833.07 5 to 50
    Sb 2598.05 1 to 50
    Si 2435.16 10 to 200
    Sn 3175.02 5 to 50
    Ti 3361.26 1 to 100
    V 3183.41 1 to 100
    Zn 3345.02 20 to 300
    Zr 3438.23 25 to 300

    A All of the above lines are photographed in the second order, except barium and calcium which are first order lines.

    B A gallium oxide carrier must be used for silver. See Test Method E402.

    31.1 This test method covers the spectrochemical determination of silver in nuclear-grade uranium dioxide. The relative standard deviation is 15 % for the concentration range of 0.1 to 50 μg/g.

    33.1 This procedure is designed for a rapid determination of surface area of nuclear-grade uranium dioxide (UO2) powders. The determination of surface area by this procedure is automatic, simple, and fast enough to be used in quality control work. The range of analysis is from 1 to 1500 m2/g.


    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

    C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder

    C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride

    C776 Specification for Sintered Uranium Dioxide Pellets

    C1267 Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium

    C1287 Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma Mass Spectrometry

    C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis

    C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method

    C1413 Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by Thermal Ionization Mass Spectrometry

    C1453 Test Method for the Determination of Uranium by Ignition and the Oxygen to Uranium (O/U) Atomic Ratio of Nuclear Grade Uranium Dioxide Powders and Pellets

    C1457 Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction

    C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide

    D1193 Specification for Reagent Water

    E115 Practice for Photographic Processing in Optical Emission Spectrographic Analysis

    E130 Practice for Designation of Shapes and Sizes of Graphite Electrodes

    E402 Test Method for Spectrographic Analysis of Uranium Oxide (U3O8) by Gallium Oxide-Carrier Technique


    UNSPSC Code

    UNSPSC Code 12141748(Uranium U)


    DOI: 10.1520/C0696-11

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