Publication Date: 2/1/84
    Pages: 10
    Date Entered: 3/11/84
    Title: QUALIFICATION, CALIBRATION, AND ERROR ESTIMATION METHODS FOR NONDESTRUCTIVE ASSAY (8/75)
    Revision 1(*)
    February 1984
    U.S. NUCLEAR REGULATORY COMMISSION
    REGULATORY GUIDE
    OFFICE OF NUCLEAR REGULATORY RESEARCH
    REGULATORY GUIDE 5.53
    (Task SG 049-4) QUALIFICATION, CALIBRATION, AND ERROR ESTIMATION
    METHODS FOR NONDESTRUCTIVE ASSAY
A. INTRODUCTION
    Section 70.58, "Fundamental Nuclear Material Controls," of 10 CFR
    Part 70, "Domestic Licensing of Special Nuclear Material," requires
    certain licensees to establish a measurement quality assurance program
    for material control and accounting. Specifically, paragraph 70.58(f)
    requires that a program be established, maintained, and followed for the
    maintenance of acceptable measurement quality in terms of measurement
    bias and for the evaluation and control of the quality of the
    measurement system.
    Nondestructive assay (NDA) constitutes a unique measurement
    technology. When applied under appropriate rigorous controls, can
    enhance the ability of the material control and accounting system to
    detect unaccounted-for loss or diversion of special nuclear material
    (SNM) to unauthorized uses. This guide describes methods and procedures
    acceptable to the NRC staff for meeting the provisions of paragraph
    70.58(f) of 10 CFR Part 70 as it relates to the use of nondestructive
    assay.
    Any guidance in this document related to information collection
    activities has been cleared under OMB Clearance No. 3150-0009.
B. DISCUSSION
    Nondestructive assay has been applied to virtually every chemical
    or physical form of special nuclear material encountered in contemporary
    reactor fuel processing. Special considerations are required to achieve
    high-accuracy assay results and to properly estimate the errors
    associated with NDA applications. Recognizing these considerations, the
    American National Standards Institute has developed a standard, ANSI
    N15.20-1975, "Guide to Calibrating Nondestructive Assay Systems."(1)
    This standard was reviewed and reaffirmed without modification in 1980.
    This guide endorses the entire standard as supplemented in the
    regulatory position.
    ----------
    (1) Copies may be obtained from the American National Standards
    Institute, 1430 Broadway, New York, New York 10018.
    ----------
C. REGULATORY POSITION
    The methods, procedures, and guidance relating to the application
    of NDA in ANSI N15.20-1975, "Guide to Calibrating Nondestructive Assay
    Systems," are acceptable to the NRC staff for use in material protection
    programs as supplemented by the following.
1. METHOD SELECTION
    Prior to selecting an assay method, a study should be made to
    determine the required performance for that application. The specific
    NDA method should be selected to provide results that are compatible
    with plant material balance requirements. Methods to enhance attainable
    performance should be considered (e.g., container selection and
    packaging procedures for bulk materials discussed in Regulatory Guide
    5.11, "Nondestructive Assay of Special Nuclear Material Contained in
    Scrap and Waste"(2)).
2. INSTRUMENT SPECIFICATIONS
    An evaluation of each new NDA application, including the proposed
    placement of the instrument, should be conducted prior to procurement.
    Studies of existing NDA applications should be conducted periodically to
    evaluate their performance and substantiate the basis for their
    continued use. The impact of each of the measurement-to-measurement
    sources of error encountered in practice or anticipated should be
    established as a part of each of these efforts.
    ----------
    (*) The substantial number of changes in this revision has made it
    impractical to indicate the changes with lines in the margin.
    (2) A proposed revision to this guide has been issued for comment
    as Task SG 043-4.
    ----------
    A decision should be made to reduce each potentially significant
    source of error through (1) appropriate instrument design
    considerations, (2) operational controls, or (3) supplementary
    measurements made to establish bias corrections (see also Reference 1).
    Instrument procurement specifications and operational instructions
    should be developed and followed to reflect each error-reduction
    decision.
    To minimize operator-related errors and to promote uniform
    measurement practices, NDA instruments used for fixed-station operations
    should be automated to control (1) data acquisition and analysis, (2)
    diagnostic testing of instrument performance stability and calibration
    validity, and (3) calculation of associated error estimates. It is
    recognized that, for some less complicated NDA measurements, consistency
    of operation may be achieved through the implementation of carefully
    written and tested standard operating procedures.
    Instruments should be tested to ensure that they meet procurement
    specifications prior to calibration.
3. OPERATORS
    Adequate operator qualification requirements are crucial to proper
    calibration and effective measurement control of an NDA instrument. The
    qualification requirements should include a general knowledge of the
    assay technique being used and an understanding of the typical behavior
    and the limitations of the instrument and the technique. A knowledge of
    the external factors to which the measurement technique is sensitive
    (factors such as matrix composition, background, material forms, and
    container type) is also necessary. Only then can proper standards be
    chosen for calibration and measurement control data be interpreted
    effectively.
    If the operators have only a general knowledge of external
    factors, the NDA measurement program must be overseen by a director with
    a detailed knowledge of all related factors. Only qualified operators
    should be permitted to make SNM assays.
4. STABILITY TESTING
    A preventive maintenance program should be devised and implemented
    to ensure the long-term stability and reliability of each instrument.
    As part of an ongoing program of measurement control, more working
    standards(3) should be fabricated to periodically test the performance
    stability of the instrument. Each working standard should contain a
    different amount of the species of SNM to be assayed. Current licensing
    review criteria require the use of four working standards. On a rotating
    basis, one or two of these standards are used to check the system each
    day.
    ----------
    (3) Working standards are used to check the performance of an NDA
    instrument. They should be nominally representative of the items to be
    assayed. They should be fabricated and handled to ensure their internal
    integrity so that deviations in the measured response of the assay
    system can be attributed to the instrument. As stated in ANSI
    N15.20-1975, working standards built to meet these requirements are not
    acceptable as calibration standards. Calibration standards are defined
    in ANSI N15.20-1975 as "physically and chemically similar to the items
    to be assayed, for which the mass of the nuclide(s) of interest and all
    properties to which the measurement technique is sensitive are known."
    Calibration standards can be used as working standards, but working
    standards cannot be used as calibration standards. When calibration
    standards meet the requirements for working standards, licensees may
    elect to maintain only calibration standards. However, calibration
    standards may deteriorate through extensive use or may be prohibitively
    expensive for stability monitoring purposes.
    ----------
    It should be noted that, in general, a working standard need not
    be fabricated from the same type of material being assayed. Even a
    material from a different radioactive species may be acceptable if
    carefully chosen and prepared. The essential requirements for a working
    standard are that (1) the radiation characteristics of the working
    standard are sufficiently stable to ensure that fluctuations in
    instrument response during measurement control can confidently be
    attributed to aberrations in instrument parameters rather than to
    variations in source characteristics and (2) the working standard
    induces a response in the NDA instrument that is characteristic of the
    expected response to real assay material. The most convenient means of
    achieving this "representative response" characteristic is to use
    material similar to the material that will be assayed.
    A study should be made to determine the frequency with which the
    working standards are to be measured. If there is some instability, a
    working standard should be measured before and after each assay of an
    unknown item, and the calibration should be normalized to reflect the
    average of the before-assay and after-assay tests. In general,
    excessive instabilities should not be tolerated; they should be remedied
    by frequent recalibration. If instabilities persist, an alternative
    technique, an alternative instrument, or another measurement environment
    should be sought. In any case, a working standard should be measured a
    minimum of twice per shift, once at the beginning of the shift and again
    at some random time during the shift.
    As a general principle, working standards should be run with a
    frequency directly proportional to the frequency of measurements (i.e.,
    increase as the measurement frequency increases and decrease as the
    measurement frequency decreases). Also, the quantity of SNM in the
    standards measurements should closely follow the quantities of SNM being
    measured (i.e., the frequency of high-SNM-content working standards
    measurements increases as the frequency of assays of like items
    increases). These procedures provide a useful estimate of the bias when
    determined at the end of the inventory period. In addition, working
    standards should be run frequently enough for each measurement system so
    that no one system could contribute excessively to the inventory
    difference (ID) by being out of control for an extended period. A
    minimum of 16 control measurements should be made per material balance
    period. Assuming two systems having equal material flows in SNM
    quantity and number of items, the system with the greater uncertainty
    per measurement should run more working standards to reduce its
    potential impact on the ID.
    Each response to a working standard should be compared to the
    previous calibration data as well as to the mean value of previous
    measurements of that working standard (under the same calibration) that
    were accumulated during the preceding material balance period. The
    difference should be plotted on a control chart. Control chart limits
    should be established at 0.05 and 0.001 levels of significance.
    Whenever control data exceed the 0.05 control limits, the test should be
    repeated. Whenever the control data exceed the 0.001 control limits,
    normal assay operations should cease. Normal operations should not
    resume until the out-of-control performance has been remedied and the
    instrument has been recalibrated.
    The control chart of the working standard responses should be
    examined at frequent intervals to detect indications of drift, which
    should be compensated. The frequency for such examinations should be
    determined by the operating characteristics of each instrument. The
    minimum frequency for examining the control chart of a regularly used
    instrument for indications of drift should be once per week.
5. CALIBRATION
    Calibration of NDA instruments should be accomplished by measuring
    the response to calibration standards as described in ANSI N15.20-1975.
    The nuclear material content of these standards should be characterized
    through established assay procedures (e.g., chemical assays) that are
    calibrated relative to national standards or nationally accepted
    measurement systems. The calibration standards should represent the
    unknown items in all physical and chemical characteristics that affect
    the response of the instrument. Calibration data should be obtained by
    averaging the responses from repeated measurements of the calibration
    standards and should be corrected to remove observed nonrandom
    variations.
    Recalibration of an instrument is required following repair or
    replacement of parts if measurement of one or more working standards
    shows the instrument response to have changed. In addition, the
    calibration should be checked following a power outage or any unusual
    mechanical or electrical shock to the system. Recalibration data are
    also required if the characteristics of the items to be assayed change
    to the extent that previous calibration standards no longer adequately
    represent the unknown items.
    Criteria for segregating and packaging different forms of SNM
    should be developed and implemented. Each material category should be
    established to enhance assay performance, consistent with safety
    requirements and subsequent processing needs. Guidance for material
    categorization is provided in Regulatory Guides 5.11, "Nondestructive
    Assay of Special Nuclear Material Contained in Scrap and Waste,"(2) and
    5.34, "Nondestructive Assay for Plutonium in Scrap Material by
    Spontaneous Fission Detection."(4) For all categories of materials to be assayed, with the exception
    of small-content miscellaneous categories (e.g., furnace liner bricks,
    contaminated tools, or machine parts), the calibration relationship
    should be determined by a suitable method such as a least-squares fit to
    an appropriate function as described in ANSI N15.20-1975. The graphical
    calibration method is acceptable only for miscellaneous categories of
    material that contain a total of no more than 0.1 effective kilogram(5)
    of SNM in each category during a material balance period. The combined
    contribution from all assays calibrated through the graphical method
    should be less than 10 percent of the total plant standard error
    (estimator) of inventory difference (SEID).
    ----------
    (4) A proposed revision to this guide has been issued for comment
    as Task SG 046-4.
    ----------
6. CALIBRATION STANDARDS
    Calibration standards should be obtained to serve as the basis for
    the initial calibration of each instrument for each separate measurement
    technique or category of material. The number of standards in each set
    should be greater than the number of free parameters in the calibration
    function for that set. It is recognized that, in some special cases,
    one set of calibration standards may suffice for more than one
    measurement technique or material category with proper analysis of the
    raw calibration data. Furthermore, if the NDA instrument is intended
    for use over a very narrow range of SNM loadings, a more restricted
    range of SNM content in the calibration standards (confined to bracket
    the expected assay range) would prove adequate. The calibration
    standards should be completely characterized, including the mass and
    isotopic composition of the species of SNM to be assayed and all
    physical or chemical variables to which the response of the instrument
    is sensitive.
    In general, the mass of SNM contained in the standards should
    extend over the range of loadings encountered in routine assays. This
    is especially true for NDA instruments whose responses are not linear
    functions of SNM content (e.g., some neutron-based NDA instruments).
    However, if the assay response (after application of appropriate
    corrections) is known to be highly linear and to have zero offset (i.e.,
    zero response for zero SNM content), it may be more advantageous to
    avoid using standards with low loading, where calibration precision
    would suffer because of low count rates. In such a case, calibration in
    the upper half of the range of expected SNM loadings, combined with the
    constraint of zero response for zero loading, can produce a higher
    precision calibration than a least-squares fitting of measured responses
    to the standard over the full range of expected loadings, including
    values at low concentrations of SNM. If such a calibration procedure is
    used, careful initial establishment of the zero offset and instrument
    linearity followed by occasional verification of both assumptions is
    strongly recommended. Such verification could be accomplished by an
    occasional extended measurement of a low-loading standard.
    Unless isotopic composition is being measured, the isotopic
    composition of the material used in all calibration standards should be
    similar to the isotopic composition of the material being assayed. This
    is especially important for assays employing passive neutron coincidence
    counting or calorimetry. When the isotopic composition changes so that
    the response per gram of SNM differs by 10 percent or more from the
    value of the calibration standards, the material should be identified as
    a new material category. The NDA system should be recalibrated for that
    category using new calibration standards made up using the new isotopic
    composition. When the change in response per gram is less than 10
    percent, a bias correction should be determined and applied to the assay
    data.
    ----------
    (5) The term "effective kilogram" is defined in paragraph 70.4(t)
    of 10 CFR Part 70.
    ----------
    The uncertainty in the bias correction should be determined and
    accounted for in estimating the total assay uncertainty. Appropriate
    error propagation procedures are described in Regulatory Guide 5.18,
    "Limit of Error Concepts and Principles of Calculation in Nuclear
    Materials Control."
    When the response is sensitive to ingrowth or decay of a daughter
    product, the procedures described in the preceding paragraphs are
    appropriate and should be applied.
    Once fabricated, the calibration standards should be handled with
    extreme care to attempt to ensure that the distribution of contents
    remains fixed. It should be noted that solution standards lose their
    integrity over time because of evaporation and diffusion (Ref. 2) and
    radiolysis (Ref. 3). Calibration standards prepared by the mixing of
    different powders or densities tend to stratify or segregate. The
    containers should be tumbled periodically to reblend the constituents.
    Calibration standards should be used only when developing the initial
    calibration or when recalibrating the instrument following a repair or
    power outage. Working standards should be used to test the continued
    stability of the instrument (see footnote 3).
    The degree of effort that should be expended in fabricating the
    calibration standards depends on the method used to estimate the assay
    uncertainty, as described in the next section.
7. METHODS FOR ESTIMATING UNCERTAINTY
    Instrument errors associated with NDA should be estimated
    periodically by means of replicate assays as described in ANSI
    N15.20-1975.
    Three methods are acceptable to estimate the uncertainties
    associated with calibrations and bias corrections for NDA. The first
    two procedures, graphical estimation and analytical estimation through
    the calibration relationship, are detailed in ANSI N15.20-1975. The
    third procedure, comparative evaluation, is not described in the
    standard.
    7.1 Graphical Estimation
    Use of the graphical error estimation technique should result in a
    conservative error estimate that is acceptable for miscellaneous unusual
    assay categories, as described in Regulatory Position 5 of this guide.
    7.2 Analytical Estimation Through the Calibration Relationship
    When the calibration standards can be shown to represent
    adequately the unknown items, the bias associated with the NDA of an
    inventory of items can be estimated through the calibration relationship
    as demonstrated in ANSI N15.20-1975. The calibration standards should be
    fabricated from different batches of material. The uncertainty
    associated with the content of SNM elements and response-related
    isotopes contained in each calibration standard should be based on an
    extensive characterization as described in ANSI N15.20-1975. The
    uncertainty associated with the contained mass of the response-related
    isotopes should be included in the calibration as described in the
    standard. Further, the element uncertainty should be factored into the
    estimated total assay uncertainty.
    Using this procedure, it is necessary to periodically ensure that
    the calibration standards adequately represent the unknown items. This
    can be accomplished by isolating and characterizing the extraneous
    interference factors that affect the response of the instrument.
    Typically, this separation and characterization is most easily
    accomplished when the items are either finished fuel items or uniform
    containers of feed or intermediate product material.
    To ensure that the calibration standards continue to adequately
    represent unknown items, key parameters(6) that affect the observed
    response (i.e., item-to-item variations) should be monitored through
    separate tests. Measurements of the key parameters should be compiled
    and analyzed at least twice a month to catch any large instrument drift.
    For more timely measurement control, a superior approach would be to
    perform such analyses on a continuing basis and repeat measurements of
    unknowns where standards exceed control limits. This latter approach
    minimizes the backfitting of measurement data and provides a timely
    basis for measurement control.
    When the mean value of a parameter shifts from its previously
    established value, the impact of the shift on the response of the assay
    instrument should be measured through an appropriate experiment or
    calculation (Ref. 4). An appropriate bias correction should be
    determined and applied to all items that were assayed after the best
    estimate of when the parameter changed. The uncertainty in that bias
    estimate should be combined with the uncertainty in the assay values as
    predicted through the calibration function to estimate the total assay
    uncertainty.
    The uncertainty due to a bias correction may significantly
    increase the standard error of the assay. In severe cases, the effect
    may increase the SEID above the level acceptable for the total plant.
    In such cases, new calibration standards should be obtained and the
    assay system should be recalibrated.
    ----------
    (6) See Section 5.4 of ANSI N15.20-1975. See Regulatory Position
    6 of this guide for provisions to include the effects of changing
    isotopic compositions.
    ----------
    As a further check on the continued validity of the calibration
    standards, a program to periodically introduce new calibration standards
    should be implemented. The rate of replacement of standards with fresh
    material depends on the intrinsic durability and stability of the
    standard in question. Some solution standards lose their calibrated
    concentration values in a matter of days or weeks. On the other hand,
    standard fuel rods are much more durable and may last indefinitely with
    careful handling. In any case, calibration standards should be replaced
    with new standards at a rate sufficiently above their failure rate to
    ensure continued high quality in the instrument calibration.
    7.3 Comparative Evaluation
    The procedure described in this section is not included in ANSI
    N15.20-1975 but is appropriate for determining the validity of the
    calibration of NDA instruments.
    When two measurement methods are used for each of a series of
    items and one of the methods is considerably more accurate than the
    other, corresponding measurements can be usefully compared. The
    comparison can be used to establish an estimate of bias between the
    measurement methods. The comparison can also be used to estimate the
    total uncertainty associated with the less accurate measurement method.
    To determine the uncertainty associated with the NDA of an
    inventory of items using this method, unknown items should be randomly
    selected for comparative measurements. The SNM content of the items
    selected should span the range of contents normally encountered, subject
    to the qualification pointed out in Regulatory Position 6. Random error
    should be estimated through replicate analyses. To estimate the
    remaining contributions to the total assay uncertainty, each item should
    be repeatedly assayed to reduce the random assay error to less than 10
    percent of the estimated or previously established total uncertainty.
    Then, to determine the SNM content of each item selected for comparative
    evaluation, one of the following procedures should be employed:
1. Each item should be completely dissolved, independently, and
    the resulting solution should be analyzed by high-accuracy elemental and
    isotopic assay procedures, which in turn are calibrated relative to
    national standards or nationally accepted measurement systems. It
    should be recognized that dissolution residues may be present in such a
    procedure. These residues should also be assayed for a complete
    analysis. Items composed of an aggregate of similar units, e.g., fuel
    rods containing discrete pellets, should be opened and the contained
    units should be weighed, pulverized, blended, and sampled for assay
    through appropriate high-accuracy elemental and isotopic assay
    procedures. The emptied container should be examined for indications of
    residual accumulations and cleaned, leached, or assayed nondestructively
    to determine the residual SNM content.
2. For plutonium-bearing items only, each item can be assayed
    through calorimetric procedures (see Reference 5). Large items should be
    subdivided into smaller containers. Each small container should be
    assayed calorimetrically. Samples should be taken from at least three of
    the smaller containers. The samples should be measured by
    microcalorimetry and then assayed through highly accurate elemental and
    isotopic procedures that, in turn, are calibrated relative to national
    standards or nationally accepted measurement systems (Ref. 6). The
    isotopic measurement data should be examined for evidence of
    nonhomogeneous isotopic content. Isotopically nonhomogeneous materials
    should be blended and reanalyzed. On the basis of the average grams of
    plutonium per watt of the samples measured by microcalorimetry, the
    total amount of plutonium in each of the smaller containers should be
    determined. The total plutonium content of the items selected for
    comparison is then estimated as the combined contents of the smaller
    containers.
    For the first full material balance period during the initial
    implementation of this guide, two items from each category of assay
    items should be randomly selected each week for a check of the validity
    of the instrument calibration. Following this initial implementation
    period, licensees may reduce the verification measurement frequency to
    two items per month per category. When fewer than 100 new items of a
    given category are created per week, at least two of the item-comparison
    verification measurements should be made per material balance period per
    category through the procedures described above. In such cases, to
    provide an adequate data base to update the uncertainty estimates for
    NDA, licensees may pool the verification data provided the measurements
    are in statistical control, i.e., when repeated samples from the portion
    of the measurement system under test behave as random samples from a
    stable probability distribution. Under such conditions, data sets may
    be combined provided the parameters based on the current set of data and
    the previous set of data are not significantly different on the basis of
    acceptable statistical tests.
    As an alternative to this selection criterion, licensees may elect
    the latter frequency for a specific category when it can be demonstrated
    that the contribution to the SEID from that category is less than 100
    grams in any material balance period.
    At the close of the reporting period, differences between assay
    values and verification values should be recorded and tested for
    outliers. Methods for detecting outliers are described in ANSI/ASTM
    E178-80, "Practice for Dealing with Outlying Observations."(7) See also
    Regulatory Guide 5.36, "Recommended Practice for Dealing with Outlying
    Observations," for further details.
    ----------
    (7) Copies may be obtained from the American Society for Testing
    and Materials, 1916 Race Street, Philadelphia, Pennsylvania 19103.
    ----------
    A straight line with a nonzero intercept should be fitted to the
    nondestructive assay vs. verification measurement data as described in
    ANSI N15.20-1975. The slope and intercept should be jointly tested for
    one and zero, respectively, using the "F" ratio at the 5 percent
    significance level (Ref. 7). If this result is significant, separate
    tests on the slope equal to one and the intercept equal to zero should
    be made to determine the presence of either proportional or constant
    bias or both. When bias is indicated, the assay results during the
    preceeding operating period should be corrected. The variance
    associated with the bias corrections should be estimated by the standard
    error of estimate of the verification line. This variance must be
    included in the estimate of the variance of an assay result as described
    in ANSI N15.20-1975.
    Whenever a bias exceeding 50 percent of its estimated uncertainty
    is indicated, its cause should be investigated. This investigation
    should include a review of the assumptions factored into the NDA
    system's calibration. In particular, instrument stability and the
    stability of parameters that may influence the response of the assay
    system should be investigated. The investigation should also address
    the comparative measurement method, including sampling, sample handling,
    analytical procedures, interference compensation, and calibration
    validity. Results from the investigation, if they show the NDA system
    to have been incorrectly calibrated, should be employed to recalibrate
    the instrument for the forthcoming material balance period. Conversely,
    when the source of bias can be attributed to errors in the comparative
    measurements, bias corrections should not be made to the items assayed
    by NDA. Results from such investigations should be documented, and the
    documents should be maintained in accordance with Regulatory Position 8
    of this guide.
8. RECORDS RETENTION
    All records generated in connection with the activities discussed
    in this guide, including control charts, should be retained for a period
    of 5 years, as specified in paragraph 70.51(e)(4)(iii) of 10 CFR Part
    70.
    REFERENCES
1. T. E. Shea, "Reduction, Control, and Estimation of Nondestructive
    Assay Errors," Nuclear Materials Management, Vol. III, No. 3,
    1974.
2. G. J. Curtis, J. E. Rein, and S. S. Yamamura, "Comparative Study
    of Different Methods of Packaging Liquid Reagents," Analytical
    Chemistry, Vol. 45, No. 6, p. 996, 1973.
3. J. R. Weiss and E. E. Pietri, "Calculation of Hydrogen Generation
    from Pu-Induced Alpha Radiolysis of Nitric, Sulfuric, and
    Perchloric Acids," Radiation Effects, Vol. 19, p. 191, 1973.
4. R. A. Forster, D. B. Smith, and H. O. Menlove, "Error Analysis of
    a Cf-252 Fuel-Rod-Assay System," Los Alamos Scientific Laboratory,
    LA-5317, 1974.
5. U.S. Nuclear Regulatory Commission, "Calorimetric Assay for
    Plutonium," NUREG-0228, 1977.
6. F. S. Stephens et al., "Methods for the Accountability of
    Plutonium Dioxide," U.S. Nuclear Regulatory Commission, WASH-1335,
    1975.
7. F. A. Graybill, An Introduction to Linear Statistical Models,
    McGraw-Hill, New York, Vol. I, p. 128, 1961.
    BIBLIOGRAPHY
    Alvar, K., H. Lukens, and N. Lurie, "Standard Containers for SNM
    Storage, Transfer, and Measurement," U.S. Nuclear Regulatory Commission,
    NUREG/CR-1847, 1980.
    This report details the variations of container properties
    (especially wall thicknesses) and their effects on NDA
    measurements. A candidate list of standard containers, each
    sufficiently uniform to cause less than 0.2 percent variation in
    assay results, is given, along with comments on the value and
    impact of container standardization.
    Brouns, R. J., F. P. Roberts, and U. L. Upson, "Considerations for
    Sampling Nuclear Materials for SNM Accounting Measurements," U.S.
    Nuclear Regulatory Commission, NUREG/CR-0087, 1978.
    This report presents principles and guidelines for sampling
    nuclear materials to measure chemical and isotopic content of the
    material. Development of sampling plans and procedures that
    maintain random and systematic errors of sampling within
    acceptable limits for SNM accounting purposes are emphasized.
    Cooper, B. E., Statistics for Experimentalists, Pergamon Press, New
    York, 1969.
    This book provides a complete discussion of statistical procedures
    and describes a variety of statistical tests of experimental data.
    Examples are provided.
    Reilly, T. D., and M. L. Evans, "Measurement Reliability for Nuclear
    Material Assay," Nuclear Materials Management, Vol. VI, No. 2, 1977.
    This paper provides an overview of experience in nuclear material
    assay by analytical chemistry, calorimetry, and nondestructive
    assay. Ranges of accuracy and precision obtained in the assay of
    nuclear material are given.
    Sher, R., and S. Untermeyer, The Detection of Fissionable Materials by
    Nondestructive Means, American Nuclear Society Monograph, 1980.
    This book contains a helpful overview of a wide variety of
    nondestructive assay techniques for special nuclear material. In
    addition, it contains a rather extensive discussion of error
    estimation and measurement control techniques, as well as a
    presentation on measurement statistics.
    VALUE/IMPACT STATEMENT
1. PROPOSED ACTION
    1.1 Description
    Licensees authorized to possess at any one time more than one
    effective kilogram of special nuclear material (SNM) are required in
    paragraph 70.58(f) of 10 CFR Part 70 to establish, maintain, and follow
    a program for the maintenance of acceptable measurement quality in terms
    of measurement bias and for the evaluation and control of the quality of
    the measurement system.
    This guide describes methods and procedures acceptable to the NRC
    staff for meeting the provisions of paragraph 70.58(f) of 10 CFR Part 70
    for nondestructive assay (NDA) systems.
    The proposed action would revise the guide, which is still
    basically sound.
    1.2 Need
    The regulatory guide endorses ANSI N15.20-1975, "Guide to
    Calibrating Nondestructive Assay Systems." This standard was reaffirmed
    without modification in 1980 and the regulatory guide should be revised
    to indicate this. Further, revisions are needed in some sections to make
    the guide clearer and more consistent with current thinking.
    This proposed action is needed to bring Regulatory Guide 5.53 up
    to date.
    1.3 Value/Impact
    1.3.1NRC
    The regulatory positions will be brought up to date.
    1.3.2Other Government Agencies
    Not applicable.
    1.3.3Industry
    Since industry is already applying the methods and procedures
    discussed in the guide, updating these should have no adverse impact.
    1.3.4Public
    No impact on the public can be foreseen.
    1.4 Decision
    The guide should be revised to reflect the affirmation of ANSI
    N15.20-1975 in 1980 and to make it more consistent with current usage.
2. TECHNICAL APPROACH
    Not applicable.
3. PROCEDURAL APPROACH
    Of the procedural alternatives considered, revision of the
    existing regulatory guide was selected as the most advantageous and cost
    effective.
4. STATUTORY CONSIDERATIONS
    4.1 NRC Authority
    Authority for the proposed action is derived from the Atomic
    Energy Act of 1954, as amended, and the Energy Reorganization Act of
    1974, as amended, and implemented through the Commission's regulations,
    in particular Section 70.51 of 10 CFR Part 70.
    4.2 Need for NEPA Assessment
    The proposed action is not a major action that may significantly
    affect the quality of the human environment and does not require an
    environmental impact statement.
5. RELATIONSHIP TO OTHER EXISTING OR PROPOSED REGULATIONS OR POLICIES
    The proposed action is one of a series of revisions of existing
    regulatory guides on nondestructive assay techniques.
6. SUMMARY AND CONCLUSIONS
    A revised guide should be prepared to bring Regulatory Guide 5.53
    up to date.
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