ASTM C697 - 16

    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

    4.1 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.

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

    4.1.2 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.

    4.1.3 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) as described in Practice C1233.

    4.2 Fitness for Purpose of Safeguards and Nuclear Safety Applications—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.

    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 Combustion–Thermal Conductivity

    19 to 29

    Total Chlorine and Fluorine by Pyrohydrolysis

    30 to 37

    Sulfur by Distillation Spectrophotometry

    38 to 46

    Plutonium Isotopic Analysis by Mass Spectrometry


    Rare Earth Elements by Spectroscopy

    47 to 54

    Trace Elements by Carrier–Distillation Spectroscopy

    55 to 62

    (Alternative: Impurities by ICP-AES or ICP-MS)


    Impurity Elements by Spark-Source Mass Spectrography

    63 to 69

    Moisture by the Coulometric Electrolytic Moisture Analyzer

    70 to 77

    Total Gas in Reactor-Grade Plutonium Dioxide Pellets


    Plutonium-238 Isotopic Abundance by Alpha Spectrometry


    Americium-241 in Plutonium by Gamma-Ray Spectrometry


    Rare Earths By Copper Spark-Spectroscopy

    78 to 87

    Plutonium Isotopic Analysis by Mass Spectrometry

    88 to 96

    Oxygen-To-Metal Atom Ratio by Gravimetry

    97 to 104

    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, 16.2.5, 44.7, 51.9 and 92.5.1.

    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 for Light Water Reactors

    C852 Guide for Design Criteria for Plutonium Gloveboxes

    C859 Terminology Relating to Nuclear Materials

    C1068 Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry

    C1108 Test Method for Plutonium by Controlled-Potential Coulometry

    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

    C1233 Practice for Determining Equivalent Boron Contents of Nuclear Materials

    C1235 Test Method for Plutonium by Titanium(III)/Cerium(IV) Titration

    C1268 Test Method for Quantitative Determination of 241Am in Plutonium by Gamma-Ray Spectrometry

    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

    C1625 Test Method for Uranium and Plutonium Concentrations and Isotopic Abundances by Thermal Ionization Mass Spectrometry

    C1637 Test Method for the Determination of Impurities in Plutonium Metal: Acid Digestion and Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS) Analysis

    C1672 Test Method for Determination of Uranium or Plutonium Isotopic Composition or Concentration by the Total Evaporation Method Using a Thermal Ionization Mass Spectrometer

    D1193 Specification for Reagent Water

    D4327 Test Method for Anions in Water by Suppressed Ion Chromatography

    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

    E130 Practice for Designation of Shapes and Sizes of Graphite Electrodes

    ICS Code

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

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

    DOI: 10.1520/C0697-16

    Citation Format

    ASTM C697-16, Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets, ASTM International, West Conshohocken, PA, 2016,

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