Publication Date: 1/1/1901
    Pages:
    Date Entered: 6/24/85
    Title: WITHDRAWN SEE 50 FR 25364, 6/18/85
    May 30, 1985
    Regulatory Guides 5.6, 5.16, 5.19, 5.40, and 5.47
    REGULATORY GUIDE DISTRIBUTION LIST (DIVISION 5)SUBJECT: WITHDRAWAL OF FIVE DIVISION 5 REGULATORY GUIDES
    The regulatory guides identified below were issued as indicated to
    provide guidance to licensees and applicants for implementing specified
    portions of the Commission's regulations.
    Regulatory Guide 5.6, "Standard Methods for Chemical, Mass
    Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium
    Dioxide Powders and Pellets and Nuclear-Grade Mixed Oxides ([U,
    Pu]O(2))," was issued in 1973. It endorses two out-of-date ASTM
    standards, C697-72a, "Standard Methods for Chemical, Mass Spectrometric,
    and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ([U,
    Pu]O(2))," and C698-72a, "Standard Methods for Chemical, Mass
    Spectrometric and Spectrochemical Analysis of Nuclear-Grade Plutonium
    Dioxide Powders and Pellets."
    Regulatory Guide 5.16, "Standard Methods for Chemical, Mass
    Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of
    Nuclear-Grade Plutonium Nitrate Solutions and Plutonium Metal," was
    revised in 1975. It endorses two out-of-date ASTM standards, C758-73,
    "Standard Methods for Chemical, Mass Spectrometric, Spectrochemical,
    Chemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium
    Metal," and C759-73, "Standard Methods for Chemical, Mass Spectrometric,
    Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade
    Plutonium Nitrate Solutions."
    Regulatory Guide 5.19, "Methods for the Accountability of Plutonium
    Nitrate Solutions," was issued in 1974. It endorses WASH 1282, "Methods
    for the Accountability of Plutonium Nitrate Solutions." This report,
    also published in 1974, is based on 1973 plutonium technology and is no
    longer state of the art.
    Regulatory Guide 5.40, "Methods for the Accountability of Plutonium
    Dioxide Powder," was issued in 1974. It endorses WASH 1335, "Methods of
    Accountability of Plutonium Dioxide Powder," a report published in 1974
    that is no longer state of the art.
    May 1973
    U.S. ATOMIC ENERGY COMMISSION
    REGULATORY GUIDE
    DIRECTORATE OF REGULATORY STANDARDS
    REGULATORY GUIDE 5.6
    STANDARD METHODS FOR CHEMICAL, MASS SPECTROMETRIC, AND SPECTROCHEMICAL
    ANALYSIS OF NUCLEAR-GRADE PLUTOMIUM DIOXIDE POWDERS AND PELLETS
    AND NUCLEAR-GRADE MIXED OXIDES ([U, Pu]O(2))A. INTRODUCTION
    Section 70.22(b) of 10 CFR Part 70, "Special Nuclear Material,"
    requires an applicant for a license to possess certain quantities of
    special nuclear material in an unsealed form to describe, among other
    things, his procedures for control of and accounting for special nuclear
    material. This guide identifies acceptable methods for chemical,
    isotopic, and impurity analyses which an applicant may specify as part
    of his procedures for accounting for special nuclear material.
B. DISCUSSION
    Committee C-26 on Fuel, Control, and Moderator Materials for
    Nuclear Reactor Applications of the American Society for Testing and
    Materials (ASTM) has developed standards containing methods for the
    chemical analysis of (1) nuclear-grade plutonium dioxide powders and
    pellets, and (2) nuclear-grade mixed oxides. These standards are ASTM
    Standard C 697-72, "Standard Methods for Chemical, Mass Spectrometric,
    and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders
    and Pellets,"(1) and ASTM Standard C 698-72a, "Standard Methods for
    Chemical, Mass Spectrometric, and Spectrochemical Analysis of
    Nuclear-Grade Mixed Oxides ([U, Pu]O(2))."(1) As used in these
    standards, nuclear grade material means material that is to be used
    exclusively for the fabrication of nuclear fuel.
    Plutonium Dioxide
    The standard C 697-72 was approved by the ASTM on March 3, 1972,
    and published in May 1972. Included in this standard are three methods
    for the determination of plutonium:
    ----------
    (1) Copies may be obtained from the American Society for Testing
    and Materials, 1916 Race St., Philadelphia, Pa. 19103.
    ----------
    a. Controlled-Potential Coulometry. The optimum quantities of
    plutomium to be determined are 2 to 6 mg with a stated precision of 0.14
    percent relative standard deviation (RSD).
    b. Ceric Sulfate Titration, stated precision of 0.27 percent
    RSD.
    c. Amperometric Titration with Iron (II). The optimum
    quantities of plutonium to be determined are 10 to 20 mg with a stated
    precision of 0.03-0.06 percent RSD and a bias of 0.02 percent or less.
    This standard also includes a method for the determination of the
    absolute isotopic composition of plutonium dioxide allowing for the use
    of reference standards to determine bias. The stated precision of the
    method for Pu-239 at the 91% concentration level is 0.034% RSD; for
    Pu-240 at the 7.9% concentration level, 0.182% RSD; for Pu-241 at the
    0.63% concentration level, 0.978% RSD; and for Pu-242 at the 0.033%
    concentration level, 4.6% RSD. Various impurities such as nitrogen,
    carbon, chloride, fluoride, sulfur, rare earths, trace elements and
    impurities, and moisture can be determined using the methods that are
    included in the standard.
    Section 6.1 of ASTM Standard C 697-72 states that plutonium
    dioxide is very hygroscopic. It must be noted that some forms of PuO(2)
    are not very hygroscopic. Therefore, if the form of PuO(2) being
    analyzed is of the non-hygroscopic variety, the dry atmosphere mentioned
    would not be needed.
    Mixed Oxides ([U, Pu]O(2)) The standard C 698-72a was approved by the ASTM on May 30, 1972,
    and published in July 1972. Included in this standard are two methods
    for the analysis of plutonium in the presence of uranium:
    a. Controlled-Potential Coulometry. The optimum quantities of
    plutonium to be determined are 2 to 6 mg. The method may be used for
    samples in which the U/Pu ratio varies within the limits of 0.1 to 10,
    with a stated precision for a single measurement of 0.14% relative
    standard deviation (RSD); and
    b. Amperometric Titration with Iron (II). The optimum
    quantities of plutonium to be determined are 10 to 20 mg in mixed oxides
    with a plutonium content varying between 4 and 27 mass %. The method
    has a stated precision of 0.03 to 0.06% RSD and a bias of 0.02% or less.
    One method for the analysis of uranium in the presence of
    plutonium is included in this standard: Controlled-Potential Coulometry.
    The optimum quantities of uranium to be determined are 3 to 10 mg. The
    method may be used for samples in which the U/Pu ratio varies within the
    limits of 0.1 to 10, with a stated precision for a single measurement of
    0.27% RSD.
    The standard also includes a method covering the determination of
    the absolute isotopic composition of plutonium or uranium or both by
    mass spectrometry utilizing solvent extraction techniques. The accuracy
    of the method depends primarily on the accuracy of the calibration
    standards of suitable isotopic composition. Precision of the
    measurements is dependent on the relative abundance of each isotope.
    Various impurities such as nitrogen, carbon, chloride, fluoride,
    sulfur, tungsten, moisture, rare earths, trace elements and impurities,
    and total gas can be determined using the methods that are included in
    the standard.
    Another method for the determination of uranium in the presence of
    various impurities that has been well characterized and found to be
    accurate, precise, and versatile which can be used as an alternate to
    the Controlled-Potential Coulometric procedure is the AEC New Brunswick
    Laboratory titrimetric method for uranium, NBL-252, "Titrimetric
    Determination of Uranium in Product, Fuel, and Scrap Materials after
    Ferrous Ion Reduction in Phosphoric Acid."(2)C. REGULATORY POSITION
    The analytical methods for the measurement of nuclear-grade
    plutonium dioxide powders and pellets contained in ASTM Standard C
    697-72 and the analytical methods for the measurement of nuclear-grade
    mixed oxides ([U, Pu]O(2)) contained in ASTM Standard C 698-72a are
    generally acceptable and provide an adequate basis for the assay,
    isotopic measurement, and impurity analysis of nuclear-grade plutonium
    dioxide powders and pellets and nuclear-grade mixed oxides subject to
    the following:
    ----------
    (2) Copies may be obtained from the National Technical Information
    Service, 5285 Port Royal Road, Springfield, Virginia 22151.
    ----------
1. Precision and Accuracy Statements. The listed statements provide
    guidance to the levels of performance which may be attained using the
    described methods. The actual precision and accuracy of a method
    applied within a selected laboratory can only be determined through a
    well-planned quality control program.
2. Sample Handling Conditions. Section 7.1 of C 697-72 recommends
    that all sampling and critical weighings be performed in an atmosphere
    with a dew point no greater than -23 degrees C. In some cases this may
    contribute to a sample sorption of water, especially in the case of
    low-fired oxide that has been held in an unsaturated condition.
    Therefore, an atmosphere containing less than 10 ppm of moisture should
    be established. It is especially important for the analyst to know the
    sample's history in order to assure a sample representative of the
    process batch before proceeding with various degrees of atmospheric
    moisture control since this information enables him to duplicate the
    conditions in which the oxide was handled. When sampling hygroscopic
    PuO(2), materials that are non-permeable to water should be used for
    sampling vials.
3. Sample Dissolution. Depending upon the process of manufacture
    including the temperature at which the material was fired (low-fired,
    high-fired), various degrees of difficulty in dissolution will be
    encountered. The dissolution techniques described in Section 30.1 of C
    697-72 and Section 28.1 of C 698-72a are acceptable for preparing
    samples to be analyzed using the analytical methods set forth in C
    697-72 and C 698-72a provided the proper matrix for the analytical
    methods can be obtained once the material is dissolved. The proper
    control of the dissolution techniques to assure complete dissolution and
    preclude the formation of method-incompatible plutonium species is
    extremely difficult and important; therefore, as a part of the
    laboratory quality control program, the complete and proper disdolution
    of the material should be verified.
4. Calibration and Standardization. The standards should be prepared
    in the same matrix as the samples, and the calibration points should
    bracket the estimated range of the samples.
5. Safety. Procedures involving the use of perchloric acid in
    radiochemical hoods and glove boxes should be performed with caution
    because of the potential explosion and fire hazard.
6. NBL-252. The AEC New Brunswick Laboratory titrimetric method for
    uranium, NBL-252, is an acceptable alternative to the
    Controlled-Potential Coulometric procedure in ASTM Standard C 698-72a
    for the determination of uranium.
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