Publication Date: 10/1/73
    Pages: 12
    Date Entered: 1/5/93
    Title: Nondestructive Assay of Special Nuclear Material Contained in Scrap and Waste
    U.S. ATOMIC ENERGY COMMISSION
    REGULATORY GUIDE
    DIRECTORATE OF REGULATORY STANDARDS
    REGULATORY GUIDE 5.11
    NONDESTRUCTIVE ASSAY OF SPECIAL NUCLEAR MATERIAL
    CONTAINED IN SCRAP AND WASTE
    October 1973
    NONDESTRUCTIVE ASSAY OF SPECIAL NUCLEAR MATERIAL CONTAINED IN SCRAP AND
    WASTE
A. INTRODUCTION
    Section 70.51, "Material Balance, Inventory, and Records
    Requirements," of 10 CFR Part 70, "Special Nuclear Material," requires
    licensees authorized to possess at any one time more than one effective
    kilogram of special nuclear material to establish and maintain a system
    of control and accountability such that the limit of error of any
    material unaccounted for (MUF), ascertained as a result of a measured
    material balance, meets established minimum standards. The selection
    and proper application of an adequate measurement method for each of the
    material forms in the fuel cycle is essential for the maintenance of
    these standards.
    With proper controls, licensees may select nondestructive assay
    (NDA) as an alternative to traditional measurement methods. This guide
    details procedures acceptable to the Regulatory staff to provide a
    framework for the utilization of NDA in the measurement of scrap and
    waste inventory components generated in conjunction with the processing
    of special nuclear materials (SNM). Subsequent guides will detail
    procedures specific to the application of a selected technique to a
    particular problem.
B. DISCUSSION
1. Applicable Nondestructive Assay Principles
    The nondestructive assay of the SNM content of heterogeneous
    material forms is achieved through observing either stimulated or
    spontaneously occurring radiations emitted from the isotopes of either
    plutonium or uranium, from their radioactive decay products, or from
    some combination of these materials. The isotopic composition must be
    known to permit a conversion of the amount of isotope measured to the
    amount of element present in the container. Assays are performed by
    isolating the container of interest to permit a measurement of its
    contents through a comparison with the response observed from known
    calibration standards. This technology permits quantitative assays of
    the SNM content of heterogeneous materials in short measurement times
    without sample preparation and without affecting the form of the
    material to be assayed. The proper application of this technology
    requires the understanding and control of factors influencing NDA
    measurements.
    1.1 Passive NDA Techniques
    Passive NDA is based on observing spontaneously emitted radiations
    created through the radioactive decay of plutonium or uranium isotopes
    or of their radioactive daughters. Radiations attributable to alpha
    (alpha) particle decay, to gamma ray transitions following alpha and
    beta (beta) particle decay, and to spontaneous fission have served as
    the bases for practical passive NDA measurements.
    1.1.1NDA Techniques Based on Alpha Particle Decay
    Alpha particle decay is indirectly detected in calorimetry
    measurements. (Note: a small contribution is attributable to the beta
    decay of (241)Pu in plutonium calorimetry applications.) The kinetic
    energy of the emitted alpha particle and the recoiling daughter nucleus
    is transformed into heat, together with some fraction of the gamma ray
    energies which may be emitted by the excited daughter nucleus in
    lowering its energy to a more stable nuclear configuration. The
    calorimetric measurement of the heat produced by a sample can be
    converted to the amount of alpha-particle-emitting nuclides present
    through the use of the isotopic abundance and the specific power [watts
    gm(-1) sec(-1)] of each nuclide.(1) Plutonium, because of its relatively
    high specific power, is amenable to calorimetry.
    The interaction of high-energy alpha particles with some light
    nuclides (e.g., (7)Li, (9)Be, (10)Be, (11)Be, (18)O, and (19)F) may
    produce a neutron. When the isotopic composition of the
    alpha-particle-emitting nuclides is known and the content of high-yield
    (alpha,n) targets is fixed, the observation of the neutron yield from a
    sample can be converted to the amount of SNM present.
    1.1.2NDA Techniques Based on Gamma Ray Analysis
    The gamma ray transitions which reduce the excitation of a
    daughter nucleus following either alpha or beta particle emission from
    an isotope of SNM occur in discrete energies.(2) (3) The known alpha
    particle decay activity of the SNM parent isotope and the probability
    that a specific gamma ray will be emitted following the alpha particle
    decay can be used to convert the measurement of that gamma ray to a
    measurement of the amount of the SNM parent isotope present in the
    container being measured. High-resolution gamma ray spectroscopy is
    required when the gamma ray(s) being measured is observed in the
    presence of other gamma rays or X-rays which, without being resolved,
    would interfere with the measurement of the desired gamma ray.
    1.1.3NDA Techniques Based on Spontaneous Fission
    A fission event is accompanied by the emission of from 2 to 3.5
    neutrons (depending on the parent nucleus) and an average of about 7.5
    gamma rays. A total of about 200 MeV of energy is released, distributed
    among the fission fragments, neutrons, gamma rays, beta particles, and
    neutrinos. Spontaneous fission occurs with sufficient frequency in
    (238)Pu, (240)Pu, (242)Pu, and (238)U to facilitate assay measurements
    through the observation of this reaction. Systems requiring the
    coincident observation of two or three of the prompt radiations
    associated with the spontaneous fission event provide the basis for
    available measurement systems.(4) 1.2 Active NDA Techniques
    Active NDA is based on the observation of radiations (gamma rays
    or neutrons) which are emitted from the isotope under investigation when
    that isotope undergoes a transformation resulting from an interaction
    with stimulating radiation provided by an appropriate external source.
    Isotopic(5) and accelerator(4) sources of stimulating radiation have
    been investigated.
    Stimulation with accelerator-generated high-energy neutrons or
    gamma rays should be considered only after all other NDA methods have
    been evaluated and found to be inadequate. Such systems have been
    tested to assay variable mixtures of fissile and fertile materials in
    large containers having a wide range of matrix variability. Operational
    requirements, including operator qualifications, maintenance, radiation
    shielding, and calibration considerations, normally require an
    inordinate level of support in comparison to the benefits of in-plant
    application.
    Fission is readily induced by neutrons in the (233)U and (235)U
    isotopes of uranium and in the (239)Pu and (241)Pu isotopes of
    plutonium. Active NDA systems have been developed using spontaneous
    fission ((252)Cf) neutron sources, as well as (gamma,n) [Sb-Be] sources
    and a variety of (alpha,n) [Am-Li, Pu-Li, Pu-Be] sources.(5) In the
    assay of scrap and waste, the neutron-induced fission reactions are
    separated from background radiations through observing radiations above
    a predetermined energy level or through observing two or three of the
    radiations emitted in fission in coincidence.(4) The detection of delayed neutrons or gamma rays has been employed
    using isotopic neutron sources to induce fission, then removing either
    source or container to observe the delayed emissions.
2. Factors Affecting the Response of NDA Systems
    Regardless of the technique selected, the observed NDA response
    depends on (1) the operational characteristics of the system, (2) the
    isotopic composition of the SNM, (3) the amount and distribution of SNM,
    (4) the amount and distribution of other materials within the container,
    and (5) the composition and dimensions of the container itself. Each of
    these variables contributes to the overall uncertainty associated with
    an NDA measurement.
    The observed NDA response represents primary contributions from
    the different SNM isotopes present in the container. To determine the
    amount of SNM present, the isotopic composition of the SNM must be known
    and the variation in the observed response as a function of varying
    isotopic composition must be understood. The effects due to items (3),
    (4), and (5) above on the observed response can be reduced through
    appropriate selection of containers, compatible segregation of scrap and
    waste categories, and consistent use of packaging procedures designed to
    improve the uniformity of container loadings.
    2.1 Operational Characteristics
    The operational characteristics of the NDA system, together with
    the ability of the system to resolve the desired response from a
    composite signal, determine the ultimate usefulness of the system.
    These operational characteristics include (1) operational stability, (2)
    geometric detection sensitivity, (3) stimulating radiation uniformity,
    and (4) energy of the stimulating radiation.
    The impact of the operational characteristics noted above on the
    uncertainty of the measured response can be reduced through the design
    of the system and the use of radiation shielding (where required).
    2.1.1Operational Stability
    The ability of an NDA system to reproduce a given measurement may
    be sensitive to fluctuations in the operational environment.
    Temperature, humidity, and line voltage variations affect NDA systems to
    some extent. These effects may be manifested through the introduction
    of spurious electronic noise or changes in the high voltage applied to
    the detector(s) or amplifiers, thereby changing the detection
    efficiency. The environment can be controlled if such fluctuations
    result in severe NDA response variations which cannot be eliminated
    through calibration and operational procedures.
    The sensitivity to background radiations can be monitored and
    controlled through proper location of the system and the utilization of
    radiation shielding, if required.
    2.1.2Geometric Detection Sensitivity
    The NDA system should be designed to have a uniform response
    throughout the detection chamber. The residual geometric response
    dependence can be measured using an appropriate source which emits
    radiation of the type being measured. The source should be small with
    respect to the dimensions of the detection chamber. The system response
    can then be measured with the source positioned in different locations
    to determine the volume of the detection chamber which can be reliably
    used.
    An encapsulated Pu source can be used to test gamma ray
    spectroscopic systems, active or passive NDA systems detecting neutrons
    or gamma rays, or calorimetry systems. Active NDA systems can be
    operated in a passive mode (stimulating source removed) to evaluate the
    magnitude of this effect. Rotating and Scanning containers during assay
    is a recommended means of reducing the response uncertainties
    attributable to residual nonuniform geometric detection sensitivity.
    2.1.3Uniformity of Stimulating Radiation
    The stimulating radiation field (i.e., interrogating neutron or
    gamma ray flux) in active NDA systems should be designed to be uniform
    in intensity and energy spectrum throughout the volume of the
    irradiation chamber. The residual effect can be measured using an SNM
    sample which is small with respect to the dimensions of the irradiation
    chamber. The response can then be measured with the SNM sample
    positioned in different locations within the irradiation chamber. If
    the same chamber is employed for irradiation and detection, a single
    test for the combined geometric nonuniformity is recommended.
    Various methods have been investigated to reduce the response
    uncertainty attributable to a nonuniform stimulating radiation field,
    including rotating and scanning the container, source scanning,
    distributed sources, and combinations of these methods. Scanning a
    rotating container with the detector and source positions fixed appears
    to offer an advantage in response uniformity and is therefore
    recommended.
    2.1.4Energy of Stimulating Radiation
    If the energy of the stimulating radiation is as high as
    practicable but below the threshold of any interfering reactions such as
    the neutron-induced fission in (238)U, the penetration of the
    stimulating radiation will be enhanced throughout the volume of the
    irradiation chamber. A high-energy source providing neutrons above the
    energy of the fission threshold for a fertile constituent such as (238)U
    or (232)Th can be employed to assay the fertile content of a container.
    The presence of extraneous materials, particularly those of low
    atomic number, lowers the energy spectrum of the interrogating neutron
    flux in active neutron NDA systems. Incorporating a thermal neutron
    detector to monitor this effect and thereby provide a basis for a
    correction to reduce the response uncertainty caused by this variable
    effect is recommended.
    Active neutron NDA systems with the capability to moderate the
    interrogating neutron spectrum can provide increased assay sensitivity
    for samples containing small amounts of fissile material (<100 grams).
    This moderation capability should be removable to enhance the range of
    usefulness of the system.
    2.2 Response Dependence on SNM Isotopic Composition
    The observed NDA response may be a composite of contributions from
    more than a single isotope of uranium or plutonium. Observed effects
    are generally attributable to one of the three sources described below.
    2.2.1Multiple Gamma Ray Sources
    Plutonium contains the isotopes (238)Pu through (242)Pu in varying
    quantities. With the exception of (242)Pu, these isotopes emit many
    gamma rays.(2) (3) The observed Pu gamma ray spectrum represents the
    contribution of all gamma rays from each isotope, together with the
    gamma rays emitted in the decay of (241)Am, which may also be present.
    Uranium gamma rays are generally lower in energy than Pu gamma
    rays. Uranium-232, occurring in combination with (233)U, has a series
    of prolific gamma-ray-emitting daughter products which include (228)Th,
    with the result that daughter products of (232)U and (232)Th are
    identical beyond (228)Th.
    2.2.2Multiple Spontaneously Fissioning Pu Isotopes
    In addition to the spontaneous fission observed from (240)Pu, the
    minor isotopes (238)Pu and (242)Pu typically contribute a few percent to
    the total rate observed.(6) In mixtures of uranium and plutonium
    blended for reactor fuel applications, the spontaneous fission yield
    from (238)U may approach one percent of the (240)Pu yield.
    2.2.3Multiple Fissile Isotopes
    In active systems, the observed fission response may consist of
    contributions from more than one isotope. For enriched uranium, if the
    energy spectrum of the stimulating radiation extends above the threshold
    for (238)U fission, that response contribution will be in addition to be
    induced (235)U fission response.
    In plutonium, the observed response will be the sum of
    contributions from the variable content of (239)Pu and (241)Pu.
    When elements (e.g., plutonium and uranium) are mixed for reactor
    utilization, the uncertainty in the response is compounded by
    introducing additional fissile components in variable combinations.
    2.3 Response Dependence on Amount and Distribution of SNM in a
    Container
    If a system has a geometrically uniform detection sensitivity and
    a uniform field of stimulating radiation (where applicable), a variation
    in the response per gram of the isotope(s) being measured is generally
    attributable to one of the three causes described below.
    2.3.1Self-Absorption of the Emitted Radiation Within the
    SNM
    For a fixed amount of SNM in a container, the probability that
    radiation emitted by the SNM nuclei will interact with other SNM atoms
    increases as the localized density of the SNM increases within the
    container. This is a primary source of uncertainty in gamma ray
    spectroscopy applications. It becomes increasingly important as the SNM
    aggregates into lumps and is more pronounced for low-energy gamma rays.
    2.3.2Multiplication of Spontaneous or Induced Fission
    The neutrons given off in either a spontaneous or an induced
    fission reaction can be absorbed in a fissile nucleus and subsequently
    induce that nucleus to fission, resulting in the emission of two or more
    neutrons. This multiplication results in an increased response from a
    given quantity of SNM. Multiplication affects the response of all
    active NDA systems and passive coincidence neutron or gamma ray
    detection systems used to observe spontaneous fission. This effect
    becomes increasingly pronounced as the energy of the neutrons traversing
    the container becomes lower or as the density of SNM increases within
    the container.
    2.3.3Self-Shielding of the Stimulating Radiation
    This effect is particularly pronounced in active systems
    incorporating a neutron source to stimulate the fissile isotopes of the
    SNM to fission. More of the incident low-energy neutrons will be
    absorbed near the surface of a high-density lump of SNM, and fewer will
    penetrate deeper into the lump. Thus, the fissile nuclei located deep
    in the lump will not be stimulated to fission at the same rate as the
    fissile nuclei located near the surface, and a low assay content will be
    indicated. This effect is dependent on the energy spectrum of the
    incident neutrons and the density of fissile nuclei. It becomes
    increasingly pronounced as the energy of the incident neutrons is
    decreased or as the density of the SNM fissile content is increased.
    The density of fissile nuclei is increased when the SNM is lumped in
    aggregates or when the fissile enrichment of the SNM is increased.
    2.4 Response Dependence on Amount and Distribution of Extraneous
    Materials within the Container
    The presence of materials other than SNM within a container can
    affect the emitted radiations in passive and active NDA systems and can
    also affect the stimulating radiation in active assay systems. The
    presence of extraneous materials can result in either an increase or a
    decrease in the observed response.
    Effects on the observed NDA response are generally attributable to
    one of the four causes described below.
    2.4.1Interfering Radiations
    This problem arises when the material emits a radiation which
    cannot be separated from the desired signal. This problem is generally
    encountered in gamma ray spectroscopy and calorimetry applications as
    the daughters of (241)Pu, (238)U, and (232)U grow in. In gamma ray
    applications, the problem is manifested in the form of additional gamma
    rays which must be separated from the desired radiations. In
    calorimetry, the daughters contribute additional heat.
    2.4.2Interference to Stimulating Radiation
    Material lowers the energy of neutrons traversing a container
    giving rise to an increase in the probability of inducing fissions.
    This problem becomes increasingly pronounced with low-atomic-number
    materials. Hydrogenous materials (e.g., water, plastics) have the
    strongest capability to produce this effect.
    2.4.3Attenuation of the Emitted Radiation
    This effect may include the partial or complete loss of the energy
    of the emitted radiation. The detection of a reduced-energy radiation
    may mean that the radiation cannot be correctly assigned to its source.
    This effect can be severe for gamma ray systems. The effect increases
    with atomic number and the material density within the container. Also,
    systems which detect neutrons above a given energy will observe fewer
    neutrons above the given energy when low-atomic-number material is added
    to the container and thus produce a low assay indication.
    The attenuation of the emitted radiation may be complete, as in
    the case of the absorption of neutrons in the nuclei of extraneous
    material. The probability for this absorption generally increases as
    the energy of the incident neutrons decreases. Hence, this effect is
    further aggravated when low-atomic-number materials are present to
    reduce the energy of the emitted neutrons.
    2.4.4Attenuation of the Stimulating Radiation
    This phenomenon is similar to that of the preceding section. In
    this instance, the stimulating radiation does not penetrate to the SNM
    within the container and thus does not have the opportunity to induce
    fission. The presence of neutron poisons (e.g., Li, B, Cd, Gd) may
    attenuate the stimulating radiation to the extent that the response is
    independent of the SNM fissile content. Most materials absorb neutrons.
    The severity of this absorption effect is dependent on the type of
    material, its distribution, and the energy of the stimulating neutrons.
    The presence of extraneous material can thus alter the observed
    response, providing either a high or a low SNM content indication. This
    effect is further aggravated by nonuniformity within the container of
    either the SNM or the matrix in which it is contained. This dependence
    is severe. Failure to attend to its ramifications through the
    segregation of scrap and waste categories and the utilization of
    representative calibration standards may produce gross inaccuracies in
    NDA measurements.
    2.5 Response Dependence on Container Dimensions and Composition
    The items identified as potential sources of uncertainty in the
    observed response of an NDA system in Section 2.1, 2.3, and 2.4 above
    can be minimized or aggravated through the selection of containers to be
    employed when assaying SNM contained in scrap or waste.
    2.5.1Container Dimensions
    The practical limitation on container size for scrap and waste to
    be nondestructively assayed represents a compromise of throughput
    requirements and the increasing uncertainties in the observed NDA
    response incurred as a penalty for assaying large containers. Radiations
    emitted deep within the container must travel a greater distance to
    escape the confines of the container. Therefore, with increasing
    container size, the probability that radiations emitted near the center
    of the container will escape the container to the detectors decreases
    with respect to the radiations emitted near the surface of the
    container.
    In active NDA systems, a relatively uniform field of stimulating
    radiation must be provided throughout that volume of the container which
    is observed by the detection system. This criterion is required to
    obtain a uniform response from a lump of SNM positioned anywhere within
    a container. It becomes increasingly difficult to satisfy this
    criterion and maintain a compact, geometrically efficient system with
    increasing container size. For this reason, the assay of small-size
    containers is recommended.
    To facilitate loading into larger containers for storage or
    offsite shipment following assay, the size and shape of the inner and
    outer containers should be chosen to be compatible.
    Packaging in small containers will produce more containers to be
    assayed for the same scrap and waste generation rates. An offsetting
    benefit, however, is that the assay accuracy of an individual container
    should be significantly improved over that of large containers. In
    addition, the total scrap and waste assay uncertainty should be reduced
    through statistically propagating a larger number of random component
    uncertainties to determine the total uncertainty.
    2.5.2Container Structural Composition
    The structural composition of containers will affect the
    penetration of the incident or the emerging radiation. Provided all
    containers are uniform, their effect on the observed response can be
    factored into the calibration of the system. The attainable assay
    accuracy will be reduced when containers with poor penetrability or
    varying composition or dimensions are selected.
3. Nondestructive Assay for the Accountability for SNM Contained in
    Scrap and Waste
    3.1 NDA Performance Objectives
    The measurement accuracy objectives for any inventory component
    can be estimated by considering the amount of material typically
    contained in that inventory category. The measurement performance
    required is such that, when the uncertainty corresponding to the scrap
    and waste inventory component is combined with the uncertainties
    corresponding to the other inventory components, the quality constraints
    on the total limit of error of the material unaccounted for (LEMUF) will
    be satisfied.
    3.2 NDA Technique Selection
    NDA technique selection should reflect a consideration of the
    accuracy requirements for the assay and the type and range of scrap and
    waste categories to be encountered. No single technique appears capable
    of meeting all requirements. When more than one type of information is
    required to separate a composite response, more than one NDA technique
    may be required to provide that information.
    3.2.1Plutonium Applications
    Calorimetry determinations are the least sensitive to matrix
    effects, but rely on a detailed knowledge of the (241)Am content and the
    plutonium isotopic composition to transform the measured heat flux to
    grams of plutonium.(1) Gamma ray spectroscopy systems complement the potential of other
    assay methods by providing the capability to nondestructively determine,
    or verify, the (241)Am content and the plutonium isotopic composition
    (except (242)Pu). High-resolution gamma ray systems are capable of
    extracting the maximum amount of information (isotopic composition,
    isotopic content, presence of extraneous gamma ray sources) from an
    assay, but content density severely affects the accuracy of quantitative
    predictions based upon that assay method.
    Passive coincidence detection of the spontaneous fission yield of
    Pu-bearing systems provides an indication of the combined (238)Pu,
    (240)Pu, and (242)Pu sample content. With known isotopic composition,
    the Pu content can be computed.(6) Neutron multiplication effects
    become severe at high Pu sample loadings.(7) Plastic scintillation
    coincidence detection systems are often designed in conjunction with
    active neutron interrogation source systems. Operated in passive and
    active modes, such systems are able to provide an assay of both the
    spontaneously fissioning and the fissile content of the sample. The
    spontaneous background can be subtracted from an active NDA response to
    provide a yield attributable to the fissile SNM content of the
    container.
    Active NDA can be considered for plutonium scrap and waste
    applications after the potential implementation of the passive
    techniques has been evaluated. With the wide range of isotopic
    compositions encountered, together with the mixture with various
    enrichments of uranium, the requirements to convert an observed
    composite response into an accurate assay of the plutonium and uranium
    fissile content become increasingly severe.
    The application of these methods to the assay of plutonium-bearing
    solids and solutions are the subjects of other Regulatory Guides.
    3.2.2Uranium Applications
    Active neutron systems can provide for both high-energy and
    moderated interrogation spectrum capabilities. Operation with the
    high-energy neutron source will decrease the density dependence and
    neutron self-shielding effects, significantly enhancing the uniqueness
    of the observed response. To extend the applicability of such a system
    to small fissile loadings, a well-moderated interrogating spectrum can
    be used to take advantage of the increased (235)U fission probability
    for neutrons of low energy. In highly enriched uranium scrap and waste
    (>20% (235)U), active NDA featuring a high-energy stimulating neutron
    flux is recommended.
    The number and energy of the gamma rays emitted from the uranium
    isotopes (with the exceptions of the minor isotopes (232)U and (237)U)
    are generally lower than for the plutonium case. The 185-keV transition
    observed in the decay of (235)U is frequently employed in uranium
    applications. The penetration of this (235)U primary gamma ray is so
    poor that the gamma ray NDA technique is not applicable with
    high-density, nonhomogeneous matrices.
    There arise occasions when a passive enrichment determination is
    practical through the measurement of the 185-keV gamma ray. One
    criterion required for this application is that the contents be
    relatively homogeneous. This information can then be combined with an
    assay of the (238)U content of the sample to compute the total uranium
    and (235)U sample content. The (238)U sample content can be obtained
    either through the detection of the (238)U spontaneous fission neutron
    yield or through the assay of the (234)Pa daughter gamma activity,
    provided either the (234)Pa is in equilibrium or its content is known.
    Enrichment meter applications for uranium will be the subject of another
    Regulatory Guide.
    Calorimetry is not applicable to the assay of uranium enriched in
    the (235)U isotope because of the low specific alpha activity. In
    (233)U applications, the intense activity of the daughter products of
    (232)U imposes a severe complication on the use of calorimetry.
    3.3 Categorization and Segregation of Scrap and Waste for NDA
    The range of variations in the observed response of an NDA system
    attributable to the effects noted in Sections 2.3 and 2.4 above can be
    reduced or controlled. Following an analysis of the types of scrap and
    waste generated in conjunction with SNM processing, a plan to segregate
    scrap and waste at the generation points can be formulated. Recovery or
    disposal compatibility is important in determining the limits of each
    category. Limiting the range in variability in those extraneous NDA
    interference parameters discussed in Sections 2.3 and 2.4 is a primary
    means of improving the accuracy of the scrap and waste assay. Once the
    categories are established, it is important that steps be taken to
    assure that segregation into separate, uniquely identified containers
    occurs at the generation point.
    Category limits can be established on the basis of measured
    variations observed in the NDA response of a container loaded with a
    known amount of SNM. The variation in extraneous parameters can then be
    mocked up and the resultant effect measured. In establishing
    categories, the following specific items are significant sources of
    error.
    3.3.1Calorimetry
    The presence of extraneous materials capable of absorbing
    (endothermic) heat or emitting (exothermic) heat will cause the observed
    response to be less or greater than the correct response for the Pu in
    the sample.
    3.3.2Neutron Measurements
    The presence of high-yield (alpha,n) target material will increase
    the number of neutrons present in the sample. A fraction of these
    neutrons will induce fission in the fissile SNM isotopes and add another
    error to the measurement.
    3.3.3Gamma Ray Measurements
    Gamma rays are severely attenuated in interactions with heavy
    materials. Mixing contaminated combustibles with heavy, dense materials
    complicates the attenuation problem. Mixing of isotopic batches or
    mixing with radioactive non-SNM can also add to the complexity of the
    response.
    3.3.4Fission Measurements
    Scrap or waste having low-atomic-number materials will reduce the
    energy of the neutrons present in the container, significantly affecting
    the probability of stimulating fission reactions.
    Neutron-absorbing materials present in SNM scrap or waste may
    significantly affect the operation of NDA systems. Table B-1 of this
    guide identifies neutron absorbers in the order of decreasing
    probability of absorption of thermal neutrons. An estimate of the
    significance of the presence of one of these materials may be obtained
    from the ratio of its absorption cross section to the absorption cross
    section of the SNM present in the container:
    (Due to database constraints, this equation is not included. Please
    contact LIS to obtain a copy.)(Due to database constraints, Tables B-1 through C-3 are not included.
    Please contact LIS to obtain a copy.) The magnitude of this effect is dependent on the distribution of
    the materials and the energy of the neutrons present within the
    container. The relationship above is a gross approximation, and for
    convenience in calculation, including only the primary fissile isotope
    is sufficient to determine which materials may constitute a problem
    requiring separate categorization for assay. In extreme cases, either
    methods should be sought to measure the content of the neutron absorber
    to provide a correction for the NDA response or a different method
    should be sought for the assay of that category.
    3.4 Packaging for Nondestructive Assay
    Nondestructive assay provides optimal accuracy potential when the
    packages to be assayed are essentially identical and when the
    calibration standards represent those packages in content and form.
    Containers for most scrap and waste can be loaded using procedures which
    will enhance the uniformity of the loading within each container and
    from container to container. Compaction and vibration are two means to
    accomplish this objective.
    3.5 Calibration of NDA Systems for Scrap and Waste
    To obtain an assay value on SNM in a container of scrap or waste
    with an associated limit of error, the observed NDA response or the
    predicted content must be corrected for background and for significant
    effects attributable to the factors described in the preceding parts of
    this discussion.
    The calibration of radiometric nondestructive assay systems is the
    subject of another Regulatory Guide.(*) One procedure for referencing NDA results to primary standards is
    the periodic selection of a container at random from a lot submitted for
    assay. That container should then be assayed a sufficient number of
    times to reduce the random uncertainty of the measurement to a
    negligible value. The SNM content of that container can then be
    determined through a different technique having an accuracy sufficient
    to verify the stated performance of the NDA system. This reference
    method should be traceable to primary standards. High-integrity
    recovery of the contents, followed by sampling and chemical analysis is
    one recommended technique.
C. REGULATORY POSITION
    In the development of an acceptable framework for the
    incorporation of nondestructive assay for the measurement of SNM-bearing
    scrap and waste, strong consideration should be given to technique
    selection, calibration, and operational procedures; to the segregation
    of scrap and waste categories; and to the selection and packaging of
    containers. The guidelines presented below are generally acceptable to
    the Regulatory staff for use in developing such a framework that can
    serve to improve materials accountability.
    ----------
    (*) To be based on ANSI N15.20, which is currently in development.
    ----------
1. Analysis of Scrap and Waste
    The origin of scrap and waste generated in conjunction with SNM
    processing activities should be determined as follows:
    a. Identify those operations which generate SNM-bearing scrap or
    waste as a normal adjunct of a process.
    b. Identify those operations which occasionally generate SNM-bearing
    scrap or waste as the result of an abnormal operation which renders the
    product unacceptable for further processing or utilization without
    treatment.
    c. Identify those scrap and waste items generated in conjunction with
    equipment cleanup, maintenance, or replacement.
    The quantities of scrap and waste generated during normal
    operations in each category in terms of the total volume and SNM content
    should be estimated. Bulk measurement throughput requirements should be
    determined to assure that such assay will not constitute an operational
    bottleneck.
2. NDA Selection
    2.1 Technique
    The performance objectives for the NDA system should be derived as
    discussed in Section B.3.1. Techniques should be considered for
    implementation in the order of precedence established in Table C-1 of
    this guide. Selection should be based on attainable accuracy, factoring
    into consideration the characteristics of the scrap and waste
    categories. The application of such techniques will be the subjects of
    other Regulatory Guides.
    2.2 System Specifications
    NDA systems for SNM accountability should be designed and
    shielding should be provided to meet the following objectives:
    a. Performance characteristics should be essentially independent of
    fluctuations in the ambient operational environment, including:
    (1) External background radiations,
    (2) Temperature,
    (3) Humidity, and
    (4) Electric power.
    b. Response should be essentially independent of positioning of SNM
    within the scrap or waste container, including effects attributable to:
    (1) Detector geometrical efficiency, and
    (2) Stimulating source intensity and energy.
    Techniques to achieve these objectives are discussed in Section B of
    this guide.
3. Categorization
    Scrap and waste categories should be developed on the basis of NDA
    interference control, recovery or disposal compatibility,(9) and
    relevant safety considerations. Categorization for NDA interference
    control should be directed to limiting the range of variability in an
    interference. Items to be considered depend upon the sensitivity of the
    specific NDA technique, as shown in Table C-2.
    The means through which these interferences are manifested are
    detailed in Section B. When such effects or contents are noted,
    separate categories should be established wherein the materials are
    isolated.
4. Containers
    4.1 Size Constraints
    Scrap and waste should be packaged for assay in containers as
    small as practicable, consistent with the capability and sensitivity of
    the NDA system.
    To enhance the penetration of stimulating or emitted radiations
    containers should be cylindrical. The diameter should be less than five
    inches to provide for significant loading capability, ease in loading,
    reasonable penetrability characteristics, and compatibility with
    criticality-safe geometry requirements for individual containers, where
    applicable.
    Containers having an outside diameter of 4-3/8 inches will permit
    nineteen such containers to be arranged in a cross section of a
    55-gallon drum, even when that drum contains a plastic liner.
    Containers having an overall length equal to some integral fraction of
    the length of a 55-gallon drum are further recommended when shipment or
    storage within such containers is to be considered. For normal
    operations, an overall length of either 16-1/2 inches (two layers or 38
    containers per drum) or 11 inches (three layers or 57 containers per
    drum) is therefore recommended.
    4.2 Structural Features
    Containers should be selected in accordance with normal safety
    considerations and should be:
    a. Structurally identical for all samples to be assayed within each
    category,
    b. Structurally identical for as many categories as practicable to
    facilitate loading into larger containers or storage facilities,
    c. Uniform in wall thickness and material composition,
    d. Fabricated of materials that do not significantly interfere with
    the radiations entering or leaving the sample,
    e. Capable of being sealed to verify post-assay integrity, and
    f. Compatible with subsequent recovery, storage, and disposal
    requirements, as applicable.
    In most NDA applications, uniformity of composition is more
    important than the specification of a particular material. Table C-3
    gives general recommendations for container structural materials.
    4.3 Container Identification
    To facilitate loading and assay within the segregation categories,
    containers should either be uniquely color-coded or carry unique
    color-coded identification labels. Identification of categories should
    be documented and operating personnel instructed to assure compliance
    with established segregation objectives.
5. Packaging
    Containers, where practical, should be packaged with a quantity of
    material containing sufficient SNM to assure that the measurement is not
    being made at the extremes of the performance bounds for that system.
    Packaging procedures should be consistent with relevant safety
    practices.
    Containers should be packaged in as reproducible a manner as
    possible. Low-density items should be compacted to reduce bulk volume
    and to increase the container SNM loading. Lowering the bulk volume
    reduces the number of containers to be assayed and generally improves
    the assay precision.
    If assay predictions are significantly affected by the variability
    in the distribution of the container contents, compacting or vibrating
    the container on a shake table to settle the contents should be used to
    enhance the assay accuracy in conjunction with rotating and scanning the
    container during assay.
6. Calibration
    The NDA system(s) should be independently calibrated for each
    category of scrap or waste to be assayed.
    Within each category, the variation of interference effects should
    be measured within the boundaries defining the limits of that category.
    Calibration standards should employ containers identical to those to be
    employed for the scrap or waste. Their contents should be mocked up to
    represent the range of variations in the interferences to be
    encountered. To minimize the number of standards required, the
    calibration standards should permit the range of interference variations
    to be simulated over a range of SNM loadings.
    Calibration relationships should be verified at intervals
    sufficiently frequent to detect deviations from the expected response in
    time to make corrections before the containers are processed or shipped.
    Assay values should be periodically verified through an
    independent measurement using a technique sufficiently accurate to
    resolve NDA uncertainty. Periodically, a container of scrap or waste
    should be randomly selected for verification. Once selected, the NDA
    analysis should be repeated a minimum number of five times to determine
    the precision characteristics of the system. The contents of that
    container should then be independently measured using one of the
    following techniques:
    a. Recovery of the contents, followed by sampling and chemical
    analysis.
    b. High-accuracy calorimetry (Pu only) with isotopic sample taken
    from contents and determined through standard techniques.
    c. Small-sample screening followed by selective chemical analyses.
    This technique is applicable to cases in which the contents consist of a
    collection of similar items. Each item should be assayed in a
    small-sample system capable of an accuracy greater than or equal to that
    of the system being calibrated. No less than five items should then be
    selected for chemical analysis. Those items should be chosen to span the
    range of observed responses in the screening assay.
    Verification measurements should be used to periodically update
    calibration data when the comparison with predicted quantities is
    satisfactory. Calibration of the system is not acceptable when the NDA
    predicted value does not agree with the measured value to within the
    value of the combined limits of error:
    (Due to database constraints, this equation is not included. Please
    contact LIS to obtain a copy.) Calibration data and hypotheses should be reinvestigated when this
    criterion is not satisfied.
    The calibration of NDA systems will be the subject of another
    Regulatory Guide.
    REFERENCES
1. F. A. O'Hara et al., Calorimetry for Safeguards Purposes, MLM-1798
    (January 1972).
2. R. Gunnink and R. J. Morrow, Gamma Ray Energies and Absolute
    Branching Intensities for (238,239,240,241)Pu and (241)Am,
    UCRL-51087 (July 1971).
3. J. E. Cline, R. J. Gehrke, and L. D. McIsaac, Gamma Rays Emitted
    by the Fissionable Nuclides and Associated Isotopes, ANCR-1069
    (July 1972).
4. L. A. Kull, Catalogue of Nuclear Material Safeguards Instruments,
    BNL-17165 (August 1972).
5. J. R. Beyster and L. A. Kull, Safeguards Applications for Isotopic
    Neutron Sources, BNL-50267 (T-596) (June 1970).
6. R. Sher, Operating Characteristics of Neutron Well Coincidence
    Counters, BNL-50332 (January 1972).
7. R. B. Perry, R. W. Brandenburg, N. S. Beyer, The Effect of Induced
    Fission on Plutonium Assay with a Neutron Coincidence Well
    Counter, Trans. Am. Nucl. Soc., 15 674 (1972).
8. Reactor Physics Constants, ANL-5800 (1963).
9. Regulatory Guide 5.2, Classification of Unirradiated Plutonium and
    Uranium Scrap.
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