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    ASTM C696 - 19

    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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    Significance and Use

    4.1 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.

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

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

    4.1.3 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.

    4.1.4 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).

    4.1.5 Determination of the oxygen-to-uranium ratio is performed on the completed pellets to determine whether they have the appropriate stoichiometry for optimal performance during irradiation.

    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 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.

    1.3 The analytical procedures appear in the following order:




    Uranium by Ferrous Sulfate Reduction in Phosphoric Acid and Dichromate Titration Method


    Uranium and Oxygen Uranium Atomic Ratio by the Ignition (Gravimetric) Impurity Correction Method


    Carbon (Total) by Direct Combustion-Thermal Conductivity Method


    Total Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method


    Moisture by the Coulometric, Electrolytic Moisture Analyzer Method

    8 – 15

    Nitrogen by the Kjeldahl Method

    16 – 23

    Isotopic Uranium Composition by Multiple-Filament Surface Ionization Mass Spectrometric Method


    Spectrochemical Determination of Trace Elements in High-Purity Uranium Dioxide


    Silver, Spectrochemical Determination of, by Gallium Oxide Carrier D-C Arc Technique


    Rare Earths by Copper Spark-Spectrochemical Method


    Impurity Elements by a Spark-Source Mass Spectrographic Method


    Surface Area by Nitrogen Absorption Method

    24 – 30

    Total Gas in Reactor-Grade Uranium Dioxide Pellets


    Thorium and Rare Earth Elements by Spectroscopy


    Hydrogen by Inert Gas Fusion


    Uranium Isotopic Analysis by Mass Spectrometry


    1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

    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 for Light Water Reactors

    C859 Terminology Relating to Nuclear Materials

    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

    C1517 Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission Spectroscopy

    D1193 Specification for Reagent Water

    ICS Code

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

    UNSPSC Code

    UNSPSC Code 12141748(Uranium U)

    Referencing This Standard
    Link Here
    Link to Active (This link will always route to the current Active version of the standard.)

    DOI: 10.1520/C0696-19

    Citation Format

    ASTM C696-19, Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets, ASTM International, West Conshohocken, PA, 2019, www.astm.org

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