ASTM C799 - 12

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

    Active Standard ASTM C799 | Developed by Subcommittee: C26.05

    Book of Standards Volume: 12.01

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    Significance and Use

    Uranyl nitrate solution is used as a feed material for conversion to the hexafluoride as well as for direct conversion to the oxide. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, isotopic composition, acidity, radioactivity, and impurity content. These methods are designed to show whether a given material meets the specifications for these items described in Specification C788.

    An assay is performed to determine whether the material has the specified uranium content.

    Determination of the isotopic content of the uranium is made to establish whether the effective fissile content is in accordance with the purchasers specifications.

    Acidity, organic content, and alpha, beta, and gamma activity are measured to establish that they do not exceed their maximum limits.

    Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded. Impurity concentrations are also required for calculation of the equivalent boron content (EBC), and the total equivalent boron content (TEBC).

    1. Scope

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solution to determine compliance with specifications.

    1.2 The analytical procedures appear in the following order:

    Determination of Uranium 7
    Specific Gravity by Pycnometry 15-20
    Free Acid by Oxalate Complexation 21-27
    Determination of Thorium28
    Determination of Chromium29
    Determination of Molybdenum30
    Halogens Separation by Steam Distillation 31-35
    Fluoride by Specific Ion Electrode 36-42
    Halogen Distillate Analysis: Chloride, Bromide, and Iodide by
    Amperometric Microtitrimetry
    Determination of Chloride and Bromide44
    Determination of Sulfur by X-Ray Fluorescence45
    Sulfate Sulfur by (Photometric) Turbidimetry46
    Phosphorus by the Molybdenum Blue (Photometric) Method 54-61
    Silicon by the Molybdenum Blue (Photometric) Method62-69
    Carbon by Persulfate Oxidation-Acid Titrimetry70
    Conversion to U3O871-74
    Boron by Emission Spectrography75-81
    Impurity Elements by Spark Source Mass Spectrography82
    Isotopic Composition by Thermal Ionization Mass Spectrometry83
    Uranium-232 by Alpha Spectrometry84-90
    Total Alpha Activity by Direct Alpha Counting91-97
    Fission Product Activity by Beta Counting98-104
    Entrained Organic Matter by Infrared Spectrophotometry105
    Fission Product Activity by Gamma Counting106
    Determination of Arsenic107
    Determination of Impurities for the EBC Calculation108
    Determination of Technetium 99109
    Determination of Plutonium and Neptunium110

    1.3 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. Specific precautionary statements are given in Section 5.

    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

    C696 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium Dioxide Powders and Pellets

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

    C788 Specification for Nuclear-Grade Uranyl Nitrate Solution or Crystals

    C1219 Test Methods for Arsenic in Uranium Hexafluoride

    C1233 Practice for Determining Equivalent Boron Contents of Nuclear Materials

    C1254 Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence

    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

    C1295 Test Method for Gamma Energy Emission from Fission Products in Uranium Hexafluoride and Uranyl Nitrate Solution

    C1296 Test Method for Determination of Sulfur in Uranium Oxides and Uranyl Nitrate Solutions by X-Ray Fluorescence (XRF)

    C1380 Test Method for the Determination of Uranium Content and Isotopic Composition by Isotope Dilution Mass Spectrometry

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

    C1561 Guide for Determination of Plutonium and Neptunium in Uranium Hexafluoride and U-Rich Matrix by Alpha Spectrometry

    D1193 Specification for Reagent Water

    E12 Terminology Relating to Density and Specific Gravity of Solids, Liquids, and Gases

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

    American Chemical Society Specification

    Reagent Chemicals Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.

    Other Documents

    ISO 7097 Determination of Uranium in Uranium Product Solutions and Solids with Cerium IV Oxidation Titrimetric Method Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036,

    ICS Code

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

    UNSPSC Code

    UNSPSC Code 15131500(Nuclear fuel)

    Referencing This Standard
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    DOI: 10.1520/C0799-12

    Citation Format

    ASTM C799-12, Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions , ASTM International, West Conshohocken, PA, 2012,

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