Publication Date: 12/1/83
    Pages: 10
    Date Entered: 2/23/84
    Title: NONDESTRUCTIVE URANIUM-235 ENRICHMENT ASSAY BY GAMMA-RAY SPECTROMETRY (4/74)
    Revision 1
    December 1983
    U.S. NUCLEAR REGULATORY COMMISSION
    REGULATORY GUIDE
    OFFICE OF NUCLEAR REGULATORY RESEARCH
    REGULATORY GUIDE 5.21
    (Task SG 044-4) NONDESTRUCTIVE URANIUM-235 ENRICHMENT
    ASSAY BY GAMMA RAY SPECTROMETRY
A. INTRODUCTION
    Section 70.51, "Material Balance, Inventory, and Records
    Requirements," of 10 CFR Part 70, "Domestic Licensing of Special Nuclear
    Material," requires, in part, that licensees authorized to possess and
    use at any one time more than one effective kilogram of special nuclear
    material (SNM) determine the inventory difference (ID) and its
    associated standard error (estimator) of inventory difference (SEID) for
    each element and the fissile isotope for uranium contained in material
    in process. Such a determination is to be based on measurements of the
    quantity of the element and of the fissile isotope for uranium.
    The majority of measurement techniques used in SNM accountability
    are specific to either the element or the isotope but not to both. A
    combination of techniques is therefore required to determine the ID and
    SEID by element and by fissile isotope for uranium. Passive gamma ray
    spectrometry is a nondestructive method for measuring the enrichment or
    relative concentration of the fissile isotope (235)U in uranium, but
    this technique is used in conjunction with an assay for the element
    uranium in order to determine the amount of (235)U.
    This guide describes conditions for (235)U enrichment measurements
    using gamma ray spectrometry that are acceptable to the NRC staff and
    provides procedures for operation, calibration, error analysis, and
    measurement control.(1) Examples of (235)U enrichment assays using
    portable and in-line instruments based on the techniques outlined in
    this guide may be found in References 1 through 4.
    Any guidance in this document related to information collection
    activities has been cleared under OMB Clearance No. 3150-0009.
    ----------
    (1) Calibration, error analysis, and measurement control are
    discussed in Regulatory Guide 5.53, "Qualification, Calibration, and
    Error Estimation Methods for Nondestructive Assay." A proposed revision
    to this guide has been issued for comment as Task SG 049-4.
    ----------
B. DISCUSSION
1. BASIS FOR GAMMA RAY MEASUREMENT OF URANIUM ENRICHMENT
    The alpha decay of (235)U to (231)Th is accompanied by the
    emission of a prominent gamma ray at 185.7 keV (4.3 x 10(4) of these
    185.7-keV gamma rays are emitted per second per gram of (235)U). The
    relatively low energy and consequent low penetrating power of these
    gamma rays implies that most of the rays that are emitted in the
    interior of the sample are absorbed within the material itself.
    Thick(2) materials therefore exhibit a 185.7-keV gamma ray emission
    characteristic of an infinite medium; i.e., the 185.7-keV gamma flux
    emitted from the sample surface does not depend upon the size or
    dimensions of the material. Under these conditions, the 185.7-keV
    intensity is directly proportional to the (235)U enrichment. A measure
    of this 185.7-keV intensity with a suitable detector forms the basis for
    an enrichment measurement technique.
    The thickness of the material with respect to the mean free path
    of the 185.7-keV gamma ray is the primary characteristic that determines
    the applicability of passive gamma ray spectrometry for the measurement
    of isotope enrichment. The measurement technique is applicable only if
    the material is thick. However, in addition to the thickness of the
    material, other conditions must be satisfied before the gamma ray
    measurement technique can be accurately applied. An approximate
    analytical expression for the detected 185.7-keV activity is given
    below. This expression has been separated into several individual terms
    to aid in identifying those parameters that may interfere with the
    measurement. Although approximate, this relationship can be used to
    estimate the magnitude of interfering effects in order to establish
    limits on the range of applicability and to determine the associated
    uncertainties introduced into the measurement. This relationship is:
    ----------
    (2) The terms "thick" and "thin" are used throughout this guide to
    refer to distances in relation to the mean free path of the 185.7-keV
    gamma ray in the material under consideration. The mean free path is
    the 1/e-folding distance of the gamma ray flux or, in other terms, the
    average distance a gamma ray traverses before interacting.
    ----------
    (Due to database constraints, this equation is not included. Please
    contact LIS to obtain a copy.) A derivation of this expression, as well as other necessary
    background information on the theory of enrichment measurements, may be
    found in Reference 5. As evident in Equation 1, the activity (C) is
    proportional to the enrichment (E) but is affected by several other
    characteristics as well.
2. MATERIAL AND CONTAINER WALL EFFECTS ON MEASUREMENT
    2.1 Material Thickness
    In order for Equation 1 to be applicable, the material must be
    sufficiently thick to produce strong attenuation of 185.7-keV gamma
    rays. To determine whether this criterion is met, it is useful to
    compare the actual thickness of the material with a characteristic
    length called the critical distance x(o), where x(o) is defined as the
    thickness of material that produces 99.5 percent of the measured
    185.7-keV activity:
    (Due to database constraints, this equation is not included. Please
    contact LIS to obtain a copy.)Calculated values of x(o) for several common materials are given in in
    Table 1.
    (Due to database constraints, Tables 1 and 2 are not included. Please
    contact LIS to obtain a copy.)Other nondestructive assay (NDA) techniques are capable of detecting SNM
    distributed within a container. The enrichment measurement technique,
    however, is inherently a surface measurement. Therefore, the "sample"
    observed, i.e., the surface, must be representative of all the material
    in the container. In this respect the enrichment measurement is more
    analogous to chemical analysis than are other NDA techniques.
    2.2 Material Composition
    If the gamma ray measurement is to be dependent only on the
    enrichment, the term related to the composition of the matrix should be
    approximately equal to one, i.e.,
    (Due to database constraints, this equation is not included. Please
    contact LIS to obtain a copy.)This condition ensures that the enrichment measurement will be
    insensitive to variations in the matrix composition. However, if this
    matrix term differs significantly from unity, the enrichment measurement
    can still be performed provided the matrix composition of the standard
    and samples remains reasonably constant.
    Calculated values of this quantity for common materials are given
    in Table 1. The deviations of the numbers in Table 1 from unity
    indicate that a bias can be introduced by ignoring the difference in
    material composition.
    Inhomogeneities in matrix material composition, uranium density,
    and uranium enrichment within the measured volume of the material (as
    characterized by the depth x(o) and the collimated area A) can produce
    changes in the measured 185.7-keV activity and affect the accuracy of an
    enrichment calculated on the basis of that activity. Variations in the
    content of low-atomic-number (Z < 30) matrix materials and
    inhomogeneities in uranium density in such matrix material produce a
    small to negligible effect on measurement accuracy. Care is necessary,
    however, in applying this technique to materials having
    high-atomic-number matrices (Z > 50) or materials having uranium
    concentrations less than approximately 75 percent. Significant
    inaccuracies can arise when the uranium enrichment itself varies
    throughout the sample.
    The above conclusions about the effects of inhomogeneities are
    based on the assumption that the thickness of the material exceeds the
    critical distance, x(o), and that the inhomogeneities exist within this
    depth. In the case of extremely inhomogeneous materials such as scrap,
    the condition of sufficient depth may not always be fulfilled or
    inhomogeneities may exist beyond the depth x(o); i.e., the sample is not
    representative. Therefore, this technique is not applicable to such
    inhomogeneous materials.
    2.3 Container Wall Thickness
    Variations in the thickness of the container walls can
    significantly affect the activity measured by the detector. The
    fractional change in the activity deltaC/C due to a small change deltad
    in the container wall thickness can be expressed:
    (Due to database constraints, this equation is not included. Please
    contact LIS to obtain a copy.)Calculated values of DeltaC/C corresponding to a change in container
    thickness deltad of 0.0025 cm for common container materials are given
    in Table 2.
    Therefore, the container wall thickness must be known (e.g., by
    measuring an adequate number of the containers before loading). In some
    cases, an unknown container wall thickness can be measured using an
    ultrasonic technique after which a simple correction can be applied to
    the data to account for attenuation of the 185.7-keV gamma rays (see
    Equation 5). Commercial equipment is available to measure wall
    thicknesses ranging from about 0.025 to 5.0 cm with relative precisions
    of approximately 1.0 percent to 0.1 percent, respectively.
    Using standardized containers to hold the sample material in order
    to minimize uncertainties and possible errors associated with
    container-to-container wall thickness corrections is strongly
    recommended.
3. DETECTOR-RELATED FACTORS
    3.1 Area and Geometrical Efficiency
    The area of the material viewed by the detector and the
    geometrical efficiency are variables that may be adjusted, within
    limits, to optimize a system. Two important factors must be noted:
1. Once these variables are fixed, changes in these parameters
    will alter the calibration of the instrument and invalidate subsequent
    measurement results.
2. The placement of the material within the container will
    affect the detected activity. It is important that there are no void
    spaces between the material and the container wall.
    3.2 Net Detector Efficiency
    Thallium-activated sodium iodide, NaI(Tl), lithium-drifted
    germanium, Ge(Li), and high-purity germanium, HPGe (also referred to as
    intrinsic germanium, IG), detectors have been used to perform these
    measurements. The detection systems are generally conventional gamma
    ray spectrometry systems that are commercially available in modular or
    single-unit construction. Some useful guidelines for the procurement
    and setup of a solid-state-detector-based system are given in Regulatory
    Guide 5.9, "Specifications for Ge(Li) Spectroscopy Systems for Material
    Protection Measurements."(3) Factors that influence detector selection and the control required
    for accurate results are discussed below.
    3.2.1Background
    3.2.1.1 Compton Background. This background is predominantly
    produced by the 765-keV and 1001-keV gamma rays of (234m)Pa, a daughter
    of (238)U. Since in most cases the Compton background behaves smoothly
    in the vicinity of the 185.7-keV peak, it can be readily subtracted,
    leaving only the net counts in the 185.7-keV full-energy peak.
    3.2.1.2 Overlapping Peaks. The observable peak from certain
    gamma rays may overlap that of the 185.7-keV peak owing to the finite
    energy resolution of the detector; i.e., the difference in energies may
    be less than twice the full width of the spectrum peak at half its
    maximum height (FWHM). This problem is common in enrichment
    measurements of recently separated uranium from a reprocessing plant.
    The peak from a strong 208-keV gamma ray from (237)U (half-life of 6.75
    days) can overlap the 185.7-keV peak when a NaI detector is used.
    Analytical separation of the two unresolved peaks, i.e., peak stripping,
    may be applied. An alternative solution is to use a Ge(Li) or HPGe
    detector so that both peaks are clearly resolved. The (237)U activity
    present in reprocessed uranium will depend on the amount of (241)Pu
    present before reprocessing and also on the time elapsed since
    separation.
    ----------
    (3) A proposed revision to this guide has been issued for comment
    as Task SG 042-2 with the title "Guidelines for Germanium Spectroscopy
    Systems for Measurement of Special Nuclear Material."
    ----------
    3.2.1.3 Ambient Background. The third source of background
    originates from natural sources and from other uranium-bearing materials
    located in the vicinity of the measuring apparatus. This source can be
    particularly bothersome since it can vary over time within wide limits
    depending on plant operating conditions.
    3.2.2Count-Rate Losses
    Calculation of the detector count rates for purposes of making
    dead-time(4) estimates requires calculation of the total count rate, not
    only that due to (235)U. Total count-rate estimates for low-enrichment
    material must therefore take into account the relatively important
    backgrounds of gamma rays from (238)U daughters. If other radioactive
    materials are present within the sample, their contributions to the
    total count rate must also be considered.
    Count-rate corrections can be made by determining the dead time or
    by making measurements for known live-time(4) intervals. The pileup or
    overlap of electronic pulses is a problem that also results in a loss of
    counts in the full-energy peak for Ge(Li) systems. An electronic pulser
    may be used to monitor and correct for these losses. However, a more
    reliable method involves the use of a radioactive source fixed to the
    detector in an invariant geometry. A photopeak area from the spectrum of
    this source is counted along with a uranium peak area. The source peak
    area can then be compared with an earlier value taken without uranium
    present, and the dead time for the assay measurement can be inferred.
    (Part of the regular measurement control would then involve uranium-free
    measurement of the source peak area.) One possible source could be
    (241)Am, whose 60-keV gamma ray peak would be easily resolved from the
    uranium lines by either a Ge- or NaI-based system. If filtering of
    ambient low-energy gamma radiation is used, the (241)Am source can be
    placed between the detector and the absorber used for the filtering. If
    a high-resolution system is used, the recommended source for this
    purpose is (109)Cd, which emits only an 88-keV peak, well below the
    uranium (185.7-keV) region, and has a half-life of 453 days. Radiation
    that provides no useful information can be selectively attenuated by
    filters; e.g., a 1-mm-thick cadmium filter will reduce x-ray
    interference, eliminating this source of count-rate losses. Note that
    present-day counting electronics are capable of handling high negative
    count rates without significant losses from either pileup or system dead
    time. However, if a measurement situation arises in which count rates
    are excessive, tighter collimation of the opening on the front face of
    the detector is a simple method for reducing count rates to tolerable
    levels at which complicated loss corrections are not essential.
    ----------
    (4) "Dead time" refers to that portion of the measurement period
    during which the instrument is busy processing data already received and
    cannot accept new data. "Live time" means that portion of the
    measurement period during which the instrument can record detected
    events. To compare different data for which dead times are appreciable,
    compare counts measured for equal live-time periods, i.e., (actual
    measurement period) - (dead time) = live time.
    ----------
    3.2.3Instability in Detector Electronics
    The gain of a photomultiplier tube is sensitive to changes in
    temperature, count rate, and magnetic field. Provision can be made for
    gain checks or gain stabilization for enrichment measurement
    applications. Various gain stabilizers that automatically adjust the
    system gain to keep a reference peak centered between two preset energy
    limits are available.
C. REGULATORY POSITION
    Passive gamma ray spectrometry constitutes a means acceptable to
    the NRC staff for nondestructively determining (235)U enrichment, if the
    conditions identified below are satisfied.
1. RANGE OF APPLICATION
    All material to be assayed under a certain calibration should be
    of similar chemical form, physical form, homogeneity, and impurity
    level.
    The critical distance of the material should be determined. Only
    those items of the material having dimensions greater than this critical
    distance should be assayed by this technique.
    The material should be homogeneous in all respects on a
    macroscopic(5) scale. The material should be homogeneous with respect
    to uranium enrichment on a microscopic(5) scale.
    The containers should all be of similar size, geometry, and
    physical and chemical composition.
2. SYSTEM REQUIREMENTS
    NaI(Tl) scintillation detectors having a resolution of FWHM less
    than 16 percent at the 185.7-keV peak of (235)U are generally adequate
    for measuring the enrichment of uranium. Crystals with a thickness in
    the range of 1.3 to 1.8 cm are recommended for optimum efficiency. If
    other radionuclides that emit significant quantities of gamma radiation
    in an energy region E = 185.7 keV @@ 2 FWHM at 185.7 keV are present,
    one of the following should be used:
    a. A higher resolution detector, e.g., Ge(Li) or HPGe, or
    ----------
    (5) Macroscopic refers to distances greater than the critical
    distance; microscopic to distances less than the critical distance.
    ----------
    b. A peak-stripping procedure to subtract the interference. In
    this case, data should be provided to show the range of concentration of
    the interfering radionuclide and the accuracy and precision of the
    stripping technique over this range.
    The detection system gain should be stabilized by monitoring a
    known reference peak.
    The system clock should be in live time. The system should
    provide a means of determining the count-rate losses based on the total
    counting rate, or provide additional collimation to reduce the count
    rate.
    The design of the system should allow reproducible positioning of
    the detector or item being assayed.
    The system should be capable of determining the gamma ray activity
    in at least two energy regions to allow subtraction of the background.
    One region should encompass 185.7 keV, and the other should be above
    this region but should not overlap it. The threshold and width of the
    regions should be adjustable. If dead-time corrections are measured
    with a pulser or source peak, a third and fourth region will have to be
    defined to establish the additional peak area and its background.
    The system should have provision for filtering out low-energy
    radiation from external sources.
3. DATA ACQUISITION
    Initial preparation of the assay instrumentation for data
    acquisition should involve careful determination of the system energy
    gain, the position of key photopeak and background regions, and the
    instrument response to calibration. However, after the proper instrument
    settings are established, routine operation can involve a less detailed
    check of the peak positions. This verification can consist of either a
    visual check of the gamma ray spectrum on a multichannel analyzer or a
    brief scan of the 140- to 200-keV energy region with a single-channel
    analyzer. Verification that the 185.7-keV peak position corresponds to
    its value at calibration ensures that the instrument is still biased
    properly. Verification of the 185.7-keV count rate with a uranium check
    source can also demonstrate continued validity of the response
    calibration. In some cases it may be useful to check the position of
    two peaks in the gamma ray spectrum, in which case a E57Co gamma ray
    source (with a photopeak at 122 keV) would be convenient.
    If the total counting rate is determined primarily by the
    185.7-keV gamma ray, the counting rate should be restricted (e.g., by
    absorbers or decreased geometrical efficiency) below those rates
    requiring correction. The system sensitivity will be reduced by these
    measures, and, if the sensitivity is no longer adequate, separate
    calibrations should be made in two or more enrichment regions.
    To determine the location and width of the 185.7-keV peak region
    and the background regions, the energy spectrum from each calibration
    standard (see Regulatory Position 4, Calibration) should be determined
    and the position of the 185.7-keV peak and neighboring peaks noted. The
    threshold and width of each energy region should then be selected to
    avoid including any neighboring peaks and to optimize the system
    stability and the signal-to-background ratio.
    The net response attributed to 185.7-keV gamma rays should be the
    accumulated counts in the peak region minus a multiple of the counts
    accumulated in a nearby background region. A single upper background
    region may be monitored, or both a region above the peak region and one
    below may be monitored. If only an upper background region is
    monitored, the net response, R, is given by
    R = G - bB
    where G and B are the gross counts in the peak region and the background
    region, respectively, and b is the multiple of the background to be
    subtracted. This net response, R, should then be proportional to the
    enrichment, E:
    E = C(1)R = C(1)(G - bB)where C(1) is a calibration constant to be determined (see Regulatory
    Position 4, Calibration). The gross counts, G and B, should be measured
    for all the standards. The quantities G/E should then be plotted as a
    function of the quantities B/E and a straight line through the data
    determined:
    G/E = b(B/E) + 1/C(1)The slope of this line is b, the multiple of the upper background region
    to be subtracted. The data from all the standards should be used in
    determining this slope.
    If both an upper and a lower background are monitored, the counts
    in each of these regions should be used to determine a straight-line fit
    to the background. Using this straight-line approximation, the area or
    number of counts under this line in the peak region should be subtracted
    from the gross counts, G, to obtain the net response. An adequate
    technique based on this principle is described in Reference 8. On a
    number of recently developed portable gamma ray spectroscopy
    instruments, these calibration procedures can be performed automatically
    by means of a microprocessor-based computational capability built into
    the instrument or by a calculator. In such cases, the more reliable
    procedure of complete calibration of the instrument before each assay
    session may be practical.
4. CALIBRATION
    CalibrationE6 standards should be obtained by:
1. Selecting items from the production material. A group of
    the items selected should, after determination of the gamma ray
    response, be measured by an independent, more accurate technique, e.g.,
    mass spectrometry, that is traceable to or calibrated with National
    Bureau of Standards (NBS) standard reference material. The other items
    should be retained as working standards.
    ----------
    (6) None of the calibration techniques or data reduction
    procedures discussed precludes the use of automated direct-readout
    systems for operation. The procedures described in this guide should be
    used for adjustment and calibration of direct-readout instruments.
    ----------
2. Fabricating standards that represent the material to be
    assayed in chemical form, physical form, and impurity level. The E235U
    enrichment of the material used in the fabrication of the standards
    should be determined by a technique, e.g., mass spectrometry, that is
    traceable to or calibrated with NBS standard reference material.
    The containers for the standards should have a geometry,
    dimensions, and a composition that approximate the mean of these
    parameters in the containers to be assayed. However, it should be
    emphasized that the best procedure is to standardize the sample
    containers to minimize, if not eliminate, container-to-container
    differences.
3. The values of enrichment for the calibration standards
    should span the range of values encountered in normal operation. No
    less than three separate standards should be used. (Good calibration
    practice dictates the use of at least two standards to determine the
    linear calibration constants and a third standard to check the
    calibration computations.) However, if the assay response (after
    application of appropriate corrections) can be shown to be highly linear
    and to have zero offset (i.e., zero response for zero enrichment), it
    may be more advantageous to avoid using standards with low enrichment
    because the low count rates would reduce the calibration precision. In
    such a case, calibration in the upper half of the range of expected
    enrichments combined with the constraint of zero response for zero
    enrichment can produce a higher precision calibration than a fitting of
    standard responses over the full range of expected enrichments,
    including values at low enrichment. 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-enrichment standard. It should
    be noted that if the measurement system exhibits a nonzero offset (i.e.,
    a nonzero response for zero sample enrichment), this is an indication of
    a background problem that should be corrected before assays are
    performed.
    Each standard should be measured at a number of different
    locations, e.g., for a cylinder, at different heights and rotations
    about the axis. The mean of these values should be used as the response
    for that enrichment. The dispersion in these values should be used as
    an initial estimate of the variance due to material and container
    inhomogeneity.
    In general, the data from the standards, i.e., the net responses
    attributed to the 185.7-keV gamma rays from the known uranium
    enrichments, can be employed in a simple linear calculation of the two
    calibration constants as described in Appendix 3 of Reference 5. If
    desired, more involved least-squares techniques can also be used.
5. OPERATIONS
    The measurement of enrichment involves counting the 185.7-keV
    gamma ray intensity from an infinite thickness of uranium-bearing
    material in a constant counting geometry. A schematic of the counting
    geometry is given in Figure 1. The detector should be collimated and
    shielded from ambient radiation so that, as much as possible, only the
    radiation from the sample container is detected.
    The detection system and counting geometry (i.e., collimator
    opening area, A, and collimator depth, x), the data reduction technique,
    and the count-rate loss corrections, if included, should be identical to
    those used in the calibration.
    Data from all measurements should be recorded in an appropriate
    log book.
    At least two working standards should be measured during each
    eight-hour operating shift. The measured response should be compared to
    the expected response (value used in calibration) to determine if the
    difference exceeds three times the expected standard deviation.E7 If
    this threshold is exceeded, measurements should be repeated to verify
    that the response is significantly different and that the system should
    be recalibrated. In the event of a significant change in the instrument
    response, every effort should be made to understand the underlying cause
    of the change and, if possible, to remedy the cause rather than simply
    calibrate around the problem.
    Prior to counting, all containers should be agitated. If this is
    not possible, the material should be mixed by some method. One
    container from every ten should be measured at two different locations
    on the container. The others may be measured at only one location. (If
    containers are scanned to obtain an average enrichment, the degree of
    inhomogeneity should still be measured by this method.) The difference between the measurements at different locations on
    the container should be used to indicate a lack of the expected
    homogeneity. If the two responses differ by more than three times the
    expected standard deviation (which should include the effects of the
    usual or expected inhomogeneity), measurements should be repeated to
    verify the existence of an abnormal inhomogeneity. If the threshold is
    exceeded, the container should be rejected and investigated to determine
    the cause of the abnormal inhomogeneity. (8) The container should be viewed at such a position that an infinite
    thickness of material fills the field of view defined by the collimator
    and detector (see Figure 1). The procedure for determining the fill of
    the container should be recorded, e.g., by visually inspecting at the
    time of filling and recording on the container tag.
    ----------
    (7) The user can always have a stricter criterion. This is a
    minimum.
    (8) The difference may also be due to a large variation in wall
    thickness.
    ----------
    (Due to database constraints, Figure 1 is not included. Please contact
    LIS to obtain a copy.) The container wall thickness should be measured. The wall
    thickness and location of the measurement should be indicated if the
    individual wall thickness measurements and the gamma ray measurement are
    made at this location. If the containers are nominally identical, an
    adequate sampling of these containers should be sufficient. The mean of
    the measurements on these samples constitutes an acceptable measured
    value of the wall thickness that may be applied to all containers of
    this type or category.
    The energy spectrum from a process item selected at random should
    be used to determine the existence of unexpected interfering radiations
    and the approximate magnitude of the interference. This test should be
    performed at a frequency that will ensure testing:
1. At least one item in any new batch of material.
2. At least one item if any changes in the material processing
    occur.
3. At least one item per two-month period.
    If an interference appears, either a higher resolution detector
    should be acquired or an adequate peak-stripping routine applied. In
    both cases, additional standards that include the interfering radiations
    should be selected and the system should be recalibrated.
    No item should be assayed if the measured response exceeds that of
    the highest enrichment standard by more than twice the standard
    deviation in the response from this standard.
6. ERROR ANALYSIS
    A regression or analysis-of-variance technique should be used to
    determine the uncertainty in the calibration constants.
    The measurement-to-measurement variance should be determined by
    periodically observing the net response from the standards and repeating
    measurements on selected process items. Each repeated measurement
    should be made at a different location on the container surface, at
    different times of the day, and under different ambient conditions. (9)
    The standard deviation should be determined and any trends (e.g., trends
    due to time or temperature) corrected for.
    The item-to-item variance due to the variation in wall thickness
    should be determined. The variance in the container wall thickness
    should be determined from measurements of the sample container wall
    thickness, either during the course of the assays or from separate
    measurements of randomly selected samples. The computed variance in the
    samples should be used as the variance of wall thickness. This variance
    should be multiplied by the effect of a unit variation in that thickness
    on the measured 185.7-keV (see, e.g., Table 2) response to determine its
    contribution to the total measurement variance.
    Item-to-item variations other than those measured, e.g., wall
    thickness, should be determined by periodically (see guidelines in
    Regulatory Position 5) selecting an item and determining the enrichment
    by an independent technique traceable to, or calibrated with, NBS
    standard reference material. A recommended approach is to adequately
    sample and determine the E235U enrichment by calibrated mass
    spectrometry. In addition to estimating the standard deviation of these
    comparative measurements, the data can also be used to verify the
    continued stability of the instrument calibration. If any significant
    deviation of the calibration is noted from these comparisons, the cause
    of the change should be identified before further assays are performed.
    ----------
    (9) The variance due to counting (including background) and the
    variance due to inhomogeneity, ambient conditions, etc., will be
    included in this measurement-to-measurement variance.
    ----------
    REFERENCES
1. R. B. Walton et al., "Measurements of UF(6) Cylinders with
    Portable Instruments," Nuclear Technology, Vol. 21, p. 133, 1974.
2. T. D. Reilly et al., "A Continuous In-Line Monitor for UF(6)
    Enrichment," Nuclear Technology, Vol. 23, p. 318, 1974.
3. P. Matussek and H. Ottmar, "Gamma-Ray Spectrometry for In-Line
    Measurements of E235U Enrichment in a Nuclear Fuel Fabrication
    Plant," in Safeguarding Nuclear Materials, IAEA-SM-201/46, pp.
    223-233, 1976. Available from the International Atomic Energy
    Agency, UNIPUB, Inc., P.O. Box 433, New York, New York 10016.
4. R. B. Walton, "The Feasibility of Nondestructive Assay
    Measurements in Uranium Enrichment Plants," Los Alamos Scientific
    Laboratory, LA-7212-MS, 1978.
5. L. A. Kull, "Guidelines for Gamma-Ray Spectroscopy Measurements of
    E235U Enrichment," Brookhaven National Laboratory, BNL-50414,
    March 1974.
6. J. H. Hubbell, "Photon Cross Sections, Attenuation Coefficients,
    and Energy Absorption Coefficients from 10 keV to 100 GeV,"
    National Bureau of Standards, NSRDS-NBS 29, 1969.
7. E. Storm and H. I. Israel, "Photon Cross Sections from .001 to 100
    MeV for Elements 1 through 100," Los Alamos Scientific Laboratory,
    LA-3753, 1967.
8. G. Gunderson and M. Zucker, "Enrichment Measurement in Low
    Enriched E235U Fuel Pellets," in "Proceedings: 13th Annual
    Meeting," Journal of the Institute of Nuclear Materials
    Management, Vol. 1, No. 3, p. 221, 1972.
    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. Available through the NRC/GPO Sales Program, U.S.
    Nuclear Regulatory Commission, Washington, D.C. 20555.
    This report describes 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.
    Augustson, R. H., and T. D. Reilly, "Fundamentals of Passive
    Nondestructive Assay of Fissionable Material," Los Alamos Scientific
    Laboratory, LA-5651-M, Albuquerque, New Mexico, 1974.
    This report contains a wealth of information on nondestructive
    assay techniques and their associated instrumentation and has an
    extensive treatise on gamma ray enrichment measurements.
    Sher, R., and S. Untermeyer, "The Detection of Fissionable Materials by
    Nondestructive Means," American Nuclear Society Monograph, La Grange
    Park, Illinois, 1980.
    This book contains a helpful overview of a wide variety of
    nondestructive assay techniques, including enrichment measurement
    by gamma ray spectrometry. In addition, it contains a rather
    extensive discussion of error estimation, measurement control
    techniques, and 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
    section 70.51 of 10 CFR Part 70 to determine the inventory difference
    (ID) and the associated standard error (SEID) for each element and the
    fissile isotope of uranium contained in material in process. The
    determination is made by measuring the quantity of the element and of
    the fissile isotope for uranium.
    It is not usually possible to determine both element and isotope with
    one measurement. Therefore, a combination of techniques is required to
    measure the SNM ID and the SEID by element and by fissile isotope.
    Passive gamma ray spectroscopy is a nondestructive method for measuring
    the relative concentration of the fissile isotope E235U in uranium.
    This technique is then used in conjunction with an assay for the element
    uranium to determine the amount of E235U.
    Regulatory Guide 5.21 describes conditions for E235U enrichment
    measurements using gamma ray spectroscopy that are acceptable to the NRC
    staff. The proposed action will revise the guide to conform to current
    usage and to add information on the state of the art of this technique.
    1.2 Need
    The proposed action is needed to bring Regulatory Guide 5.21 up to
    date.
    1.3 Value/Impact Assessment
    1.3.1NRC Operations
    The experience and improvements in technology that have occurred
    since the guide was issued will be made available for use in the
    regulatory process. Using these updated techniques should have no
    adverse impact.
    1.3.2Other Government Agencies
    Not applicable.
    1.3.3Industry
    Since industry is already applying the techniques discussed in the
    guide, updating these techniques should have no adverse impact.
    1.3.4Public
    No impact on the public can be foreseen.
    1.4 Decision on Proposed Action
    The guide should be revised to reflect improvements in technique
    and to bring the guide into conformity with current usage.
2. TECHNICAL APPROACH
    Not applicable.
3. PROCEDURAL APPROACH
    Of the alternative procedures 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.
    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
    Regulatory Guide 5.21 should be revised to bring it up to date.
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