Publication Date: 6/1/73
    Pages: 7
    Date Entered: 1/5/93
    Title: Guidelines for Germanium Spectroscopy Systems for Measurement for Special Nuclear Material
    June 1973
    U.S. NUCLEAR REGULATORY COMMISSION
    REGULATORY GUIDE
    OFFICE OF NUCLEAR REGULATORY RESEARCH
    REGULATORY GUIDE 5.9
    (Task SG 042-2) GUIDELINES FOR GERMANIUM SPECTROSCOPY SYSTEMS
    FOR MEASUREMENT OF SPECIAL NUCLEAR MATERIAL
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 at
    any one time more than one effective kilogram of special nuclear
    material establish and maintain a system of control and accountability
    so that the standard error (estimator) of any inventory difference,
    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.
    Many types of nondestructive assay (NDA) measurements on special
    nuclear material (SNM) can involve, or even require, a high-resolution
    gamma ray spectroscopy system. This guide is intended both to provide
    some general guidelines acceptable to the NRC staff for the selection of
    such systems and to point out useful resources for more detailed
    information on their assembly, optimization, and use in material
    protection measurements.
    Any guidance in this document related to information collection
    activities has been cleared under OMB Clearance No. 3150-0009.
B. DISCUSSION
1. BACKGROUND
    Gamma ray spectroscopy systems are used for NDA of various special
    nuclear material forms encountered in the nuclear fuel cycle, both for
    quantitative determination of the SNM content and for the determination
    of radionuclide abundances.
    Applications of high-resolution gamma ray spectroscopy have
    multiplied greatly in recent years. The samples encountered range from
    fresh fuel rods and reprocessing solutions to boxes and cans of
    uncharacterized waste material. Measurement conditions also vary widely
    from controlled laboratory environments to the unpredictable plant
    environment that can be hostile to the measurement equipment and can
    often contribute serious background interferences to the spectral data.
    As a result, there is no single gamma ray assay system that can be
    effective in all cases. The system chosen for a particular NDA task
    must therefore be determined from careful consideration of all factors
    that may affect the measurement and of the requirements for the
    precision and accuracy of the assay.
    The scope of this guide is limited to the consideration of
    high-resolution gamma ray spectroscopy with lithium-drifted germanium,
    Ge(Li), or high-purity germanium, HPGe (also referred to as intrinsic
    germanium, IG), detectors. No discussion of thallium-activated sodium
    iodide, NaI(T1), or lithium-drifted silicon, Si(Li), gamma ray systems
    is presented. In addition, no discussion of specific NDA applications
    of gamma ray spectroscopy is provided. The measurement procedures
    (including calibration), analysis methods, inherent limitations, and
    overall precision and accuracy attainable are specific to each
    application and are therefore the subject of separate application
    guides. Guidelines for measurement control, calibration, and error
    analysis of NDA measurements are dealt with in detail in Regulatory
    Guide 5.53, "Qualification, Calibration, and Error Estimation Methods
    for Nondestructive Assay," which endorses ANSI N15.20-1975, "Guide to
    Calibrating Nondestructive Assay Systems."(1) ANSI N15.20-1975 was
    reaffirmed in 1980.
    All of the major commercial vendors of Ge(Li) and HPGe detectors
    and the associated electronics maintain up-to-date documentation on the
    specifications of currently available equipment, as well as a variety of
    useful and informative notes on applications. This literature is
    available from the manufacturers upon request, and the potential
    customer may use this literature as a source of the most current
    information on the highest quality systems available.
    ----------
    (*) The substantial number of changes in this revision has made it
    impractical to indicate the changes with lines in the margin.
    (1) Copies of this standard may be obtained from the American
    National Standards Institute, Inc., 1430 Broadway, New York, New York
    10018.
    ----------
    Finally, the potential user ought to consult with those
    individuals currently active in the field of nondestructive assay of
    special nuclear material and seek their advice in the particular assay
    problem being considered.
2. BIBLIOGRAPHIC INFORMATION
    An annotated bibliography is included in this regulatory guide to
    provide more detailed information on spectroscopy systems and their use.
    Elementary introductions to the concepts associated with the
    application of high-resolution gamma ray spectroscopy to problems of
    nuclear material assay are available in Augustson and Reilly and in
    Kull. These works discuss the physical processes of gamma ray detection
    and important instrumentation characteristics. More advanced discussion
    of gamma ray detectors and associated electronics may be found in Knoll
    and in Adams and Dams. A thorough treatise on the associated
    electronics is available in Nicholson. In addition, extensive discussion
    of a variety of NDA techniques and the implementation of some of these
    techniques with high-resolution gamma ray spectroscopy may be found in
    Sher and Untermeyer, in Rogers, and in Reilly and Parker. Detailed
    descriptions of detector efficiency and energy calibration procedures
    are available in section D of Knoll and also in Hajnal and Klusek; in
    Hansen, McGeorge, and Fink; in Hansen et al.; and in Roney and Seale.
    Relevant technical information beyond the introductory level,
    including nomenclature and definitions, is contained in three useful
    standards of the Institute of Electrical and Electronics Engineers,
    ANSI/IEEE Std 301-1976, "Test Procedures for Amplifiers and
    Preamplifiers for Semiconductor Radiation Detectors for Ionizing
    Radiation,"(2) ANSI/IEEE Std 325-1971, "Test Procedures for Germanium
    Gamma-Ray Detectors"(2) (reaffirmed in 1977), and ANSI/IEEE Std
    645-1977, "Test Procedures for High-Purity Germanium Detectors for
    Ionizing Radiation,"(2) which supplements ANSI/IEEE Std 325-1971. These
    describe detailed techniques for defining and obtaining meaningful
    performance data for Ge(Li) and HPGe detectors and amplifiers.
3. FUNCTIONAL DESCRIPTION
    A block diagram of a typical high-resolution gamma ray
    spectroscopy system is shown in Figure 1. In such a system, the solid
    state Ge(Li) or HPGe detector converts some or all of the incident gamma
    ray energy into a proportional amount of electric charge, which can be
    analyzed by the subsequent electronics. The detector output is
    converted into an analog voltage signal by the preamplifier, which is an
    integral part of the detector package. The preamplifier signal is
    further amplified and shaped and is then converted into digital
    information that can be stored, displayed, and otherwise processed by
    the data reduction and analytical components of the system.
    ----------
    (2) Copies may be obtained from the Institute of Electrical and
    Electronics Engineers, Inc., 345 East 47th Street, New York, New York
    10017.
    ----------
4. TYPES OF SYSTEMS
    High-resolution gamma ray spectroscopy systems are distinguished
    primarily by the type (p-type or n-type) and the configuration (planar
    or coaxial) of detector used. For assay applications involving the
    measurement of low-energy gamma radiation (i.e., energies below
    approximately 200 keV), a thin planar HPGe or Ge(Li) crystal is most
    appropriate. A coaxial detector crystal with a larger volume is much
    better suited for higher energy gamma ray measurements (i.e., for
    energies above approximately 120 keV). The distinction between these two
    types of detectors is not sharp. For instance, there may be some
    applications above 120 keV in which a planar detector would be useful to
    render the system less sensitive to interferences from ambient
    high-energy gamma radiation.
    It should be noted that Ge(Li) detectors have no real advantage
    over HPGe detectors with comparable performance specifications. In
    addition, Ge(Li) detectors require constant liquid nitrogen (LN)
    cooling, even when not in operation. HPGe detectors are, of course,
    also operated at LN temperature, but they can be stored at room
    temperature. This is an advantage to potential users who may have
    extended plant shutdowns. It also prevents complete loss of a detector
    due to operator procedure error, which can happen with a Ge(Li) detector
    when LN cooling is not continuously maintained. This added convenience
    and the greater ruggedness of the HPGe detectors make them especially
    attractive for in-plant NDA applications.
5. EQUIPMENT ACCEPTANCE PRACTICES
    Equipment descriptions and instructional material covering
    operation, maintenance, and servicing of all electronic components are
    supplied by the manufacturer for all individual modules or complete
    systems. Such descriptions should include complete and accurate
    schematic diagrams for possible in-house equipment servicing. Complete
    operational tests of system performance are to be made at the vendor's
    facility, and the original data are supplied to the user upon delivery
    of the equipment. Extensive performance testing of all systems by the
    user is generally not necessary.(3) However, qualitative verification
    of selected equipment performance specifications and detector resolution
    is recommended.
    It is necessary to have calibration sources on hand to verify the
    operational capabilities of the system. The following radioactive
    sources (with appropriate activities) will provide sufficient counting
    rates to verify the energy resolution specifications of the manufacturer
    and to carry out any other performance tests desired by the user:
    (60)Co 10-30 @@Ci, Gamma ray energies: 1173, 1332 keV
    (57)Co 1-10 @@Ci, Gamma ray energies: 14, 122, 136 keV
    ----------
    (3) Although the quality control and preshipment testing
    procedures of the commercial vendors of detectors and associated
    electronics have improved and are quite dependable, some user
    verification of the specifications claimed by the manufacturer is
    strongly recommended.
    ----------
    (Due to database constraints, Figure 1 is not included. Please contact
    LIS to obtain a copy.)C. REGULATORY POSITION
    Ge(Li) or HPGe gamma ray spectroscopy data acquisition systems
    meeting the general guidelines outlined briefly below are considered
    more than adequate for use in SNM assay requiring resolution better than
    that obtainable with NaI detectors. The potential user should select
    the detector and associated electronics that meet the needs of the
    particular assay task required, with careful consideration of all
    factors that could affect the quality of the assay.
1. DETECTOR PERFORMANCE
    Excellent performance, routinely available in coaxial germanium
    detectors, may be represented by energy resolutions (FWHM)(4) of
    approximately 1.7 keV at 1332 keV ((60)Co) and approximately 0.7 keV at
    122 keV ((57)Co) for detectors with efficiencies up to 20 percent.(5)
    The full width at 0.1 maximum (FWTM) for such detectors is typically up
    to 1.9 times the FWHM. For these higher efficiency detectors,
    "peak-to-Compton ratios" are usually quoted in the range of 25 to 40.
    These ratios are strong functions of resolution, efficiency, and exact
    detector crystal geometry, and no typical values can be given without
    knowledge of all of these parameters. Coaxial detectors with this kind
    of resolution will usually have cooled field-effect transistor (FET)
    preamplifiers and an energy-rate capability of approximately 50,000
    MeV/sec.(6) Room temperature pre-amplifiers have somewhat worse
    resolution but have rate capabilities on the order of 150,000 MeV/sec.
    The resolution of planar detectors is a stronger function of the
    crystal size and shape than that of coaxial detectors, so representative
    resolutions cannot be given over a range of sizes. As an example from
    the middle of the range of sizes usually offered, an excellent 2 cm(3)
    planar detector (i.e., 2 cm(2) front face area x 1 cm thick) would have
    a resolution of approximately 0.5 keV at 122 keV ((57)Co) and 0.21 keV
    at 5.9 keV (Mn X-ray from (55)Fe decay). Planar detectors will always
    have LN-cooled FET preamplifiers in order to achieve the excellent
    resolution of these systems. The preamplifier feedback loop may be
    either pulsed optical or resistive,(7) and the system will have fairly
    modest rate capabilities in the range of 5000 MeV/sec.(6) It is
    important to decouple the detector from noisy mechanical environments to
    avoid microphonic pickup.
    ----------
    (4) The full width of the gamma ray photopeak at half of its
    maximum height (FWHM) is defined in ANSI/IEEE Std 301-1976.
    (5) The full-energy peak efficiency (in percent) is defined
    relative to the full-energy peak efficiency of a 3-in. x 3-in. NaI(T1)
    scintillation detector for 1332-keV gamma rays ((60) Co) at a
    source-to-detector distance of 25 cm. The detailed procedures for
    determining the efficiency in accordance with this definition are
    presented in Section 5.2 of ANSI/IEEE Std 301-1976.
    (6) Counting rate capabilities, expressed in MeV/sec, denote the
    maximum charge-to-voltage conversion rate of which the pre-amplifier is
    capable. For (50) Co, a 50,000-MeV/sec rate capability corresponds to a
    pulse counting rate limitation of approximately 80,000 counts/sec. For
    (57) Co, a 5000-MeV/sec rate capability also corresponds to a pulse rate
    limitation of approximately 80,000 counts/sec. Of course, nuclear
    material assays should be performed at count rates well below these
    limiting values in order to minimize rate-related losses from pulse
    pileup and dead time.
    ----------
2. ELECTRONICS PERFORMANCE
    For ease of use, maintenance, and replacement of the components in
    a high-resolution gamma ray spectroscopy system, the electronic
    components should be standard nuclear instrument modules (NIM) (Ref. 1),
    with the possible exception of the pulse-height analysis (i.e.,
    multi-channel analyzer) components. Pulse signals should be transmitted
    from module to module in shielded coaxial cable to minimize the effects
    of possible electronic noise from nearby machinery at the measurement
    site. The cables should have a characteristic impedance that matches
    the terminations used in the NIM modules (generally 93 ohms).
    The system power supplies (detector high voltage, preamplifier,
    and NIM bin) should be capable of operating the system within the
    operating specifications when supplied with 115 volts (plus minus10
    percent) at 50 to 65 hertz (at constant room temperature). The power
    supplied for the detection system should be stabilized against voltage
    shifts in order to maintain resolution. The output voltage of the
    detector bias supply is determined by the detector requirements; 5
    kilo-volts is sufficient for most applications.
    The main amplifier, commonly referred to as the spectroscopy
    amplifier, should have variable gain and pulse-shaping controls for
    maximum setup flexibility. Most high-quality amplifiers are equipped
    with baseline restoration and pole-zero cancellation circuits (Ref. 2),
    which greatly improve the resolution that can be achieved on a routine
    basis. Baseline restoration is essential for assay situations in which
    count rates in excess of several kilohertz are anticipated. Pulse pileup
    suppression is also a useful feature, if available; it may be found in
    some spectroscopy amplifiers and even in separate NIM modules designed
    for that purpose.
    Electronic components should be obtained with state-of-the-art
    linearity and temperature sensitivity. Maintenance of long-term gain
    stability may require the use of a spectrum stabilizer. Centroid
    variations of a stabilization peak of less than one channel in a
    4096-channel spectrum are achievable with commercially available
    stabilizer modules. Stabilization peaks can be provided either by a
    pulser or by a radioactive source. Generally, a radioactive source is
    preferred because it contributes less distortion to the gamma ray
    spectrum and has a stable (although decaying) emission rate.
    Furthermore, stabilization peaks from natural sources may be obtained
    from existing peaks in the assay spectrum itself, which simplifies the
    assay setup.. Dead-time and pileup corrections may also be performed
    using a pulser or a separate radioactive source fixed to the detector.
    The latter method is preferred for the reasons stated above.
    ----------
    (7) Feedback methods for charge-sensitive preamplifiers are
    discussed thoroughly in Chapter 5 of Reference 2.
    ----------
3. SYSTEM SELECTION AND USE
    The detailed requirements and constraints of a particular
    measurement situation will cause wide variation in the optimum choice of
    systems, even within a fairly well-defined application. For example, a
    requirement for high throughput may dictate higher efficiency detectors
    and highly automated data acquisition electronics. Anticipated
    interferences from uranium, thorium, or fission products may make the
    best possible system resolution the most important consideration.
    Severe operating environments may make the use of digital stabilization
    highly desirable. Constraints of space and location could dictate an
    unusually small LN dewar with automatic filling capacity. The list of
    such considerations in a given situation can be long, and each situation
    should be considered carefully and individually in order to achieve a
    system that can acquire the required measurement data.
    Beyond the choice of data acquisition systems, many other factors
    influence the successful use of gamma ray spectroscopy in quantitative
    assay measurements. Some of these are:
    a. Gamma Ray Signatures: The energies and intensities of the
    relevant gamma rays place fundamental restrictions on the sensitivity,
    precision, and accuracy of any assay. The range of gamma ray energies
    of interest also determines the type of gamma ray detector appropriate
    for optimum efficiency.
    b. Full-Energy Peak Area Determination: The procedure for
    extracting this fundamental information from the spectral data will be
    determined by the complexity of the gamma ray spectra as well as the
    intensity and complexity of the gamma ray background at energies near
    the peaks of interest.
    c. Gamma Ray Attenuation by the Samples and Surrounding
    Materials: Corrections for this effect are essential for accurate
    assays. The importance of this correction will increase as the gamma
    ray energies of interest decrease and the absorptive power of the sample
    and surrounding materials increases.
    All of this emphasizes that by far the most important factor in
    choosing an appropriate data acquisition system, in implementing proper
    assay procedures, and in supervising the assay operations is a highly
    competent person, preferably experienced in gamma ray spectroscopy and
    its application to assay measurements of special nuclear materials. Such
    a person, with the assistance of the existing literature and of others
    in the gamma ray field, will be able to consider a particular
    application in detail and choose an appropriate detector and electronics
    to create a data acquisition system that is well suited to the required
    assay task.
    REFERENCES
1. L. Costrell, "Standard Nuclear Instrument Modules," U.S. Atomic
    Energy Commission, TID-20893, Revision 3, 1969.
2. P.W. Nicholson, Nuclear Electronics, John Wiley and Sons, New
    York, 1974.
    BIBLIOGRAPHY
    Adams, F., and R. Dams, Applied Gamma-Ray Spectros-copy, Pergamon Press,
    New York, 1970.
    This work provides a comprehensive coverage of background material
    pertinent to the gamma ray spectroscopist. Considerable
    information is provided on both NaI and Ge detectors.
    Augustson, R.H., and T.D. Reilly, "Fundamentals of Passive
    Nondestructive Assay of Fissionable Material," Los Alamos Scientific
    Laboratory, LA-5651-M, 1974.
    This manual contains helpful introductory descriptions of NDA
    applications of gamma ray spectroscopy, as well as some discussion
    of gamma ray detection systems.
    Hajnal, F., and C. Klusek, "Semi-Empirical Efficiency Equations for
    Ge(Li) Detectors," Nuclear Instruments and Methods, Vol. 122, p. 559,
    1974.
    Hansen, J., J. McGeorge, and R. Fink, "Efficiency Calibration of
    Semiconductor Detectors in the X-Ray Region," Nuclear Instruments and
    Methods, Vol. 112, p. 239, 1973.
    Hansen, J., et al., "Accurate Efficiency Calibration and Properties of
    Semiconductor Detectors for Low-Energy Photons," Nuclear Instruments and
    Methods, Vol. 106, p. 365, 1973.
    Knoll, G. F., Radiation Detection and Measurement, John Wiley and Sons,
    New York, 1979.
    This book provides extensive discussion of all types of radiation
    detection systems, including high-resolution gamma ray
    spectroscopy systems. In particular, Section D deals exclusively
    with solid state detectors, and Section F is devoted to detector
    electronics and pulse processing.
    Kull, L. A., "An Introduction to Ge(Li) and NaI Gamma-Ray Detectors for
    Safeguards Applications," Argonne National Laboratory, ANL-AECA-103,
    1974.
P. W. Nicholson, Nuclear Electronics, John Wiley and Sons, New York,
    1974.
    This is an extensive treatise on electronics systems associated
    with high-resolution detectors. Detailed descriptions are given
    of detector preamplifiers, pulse shaping, rate-related losses,
    pulse-height analysis, and spectral resolution.
    Reilly, T. D., and J. L. Parker, "Guide to Gamma-Ray Assay for Nuclear
    Material Accountability," Los Alamos Scientific Laboratory, LA-5794-M,
    1975.
    This report briefly covers the principles involved in using gamma
    ray spectroscopy in the quantitative assay of SNM and attempts to
    describe both capabilities and limitations of gamma ray assay
    techniques. The report also includes a description of procedures
    for determining plutonium isotopic ratios.
    Rogers, D. R., "Handbook of Nuclear Safeguards Measurement Methods,"
    Nuclear Regulatory Commission, NUREG/CR-2078, 1983.
    Chapter 5, "Passive Nondestructive Assay Methods," contains
    descriptions of many applications of high-resolution gamma ray
    spectroscopy, as well as many references to original papers and
    reports.
    Roney, W., and W. Seale, "Gamma-Ray Intensity Standards for Calibrating
    Ge(Li) Detectors for the Energy Range 200-1700 keV," Nuclear Instruments
    and Methods, Vol. 171, p. 389, 1980.
    Sher, R., and S. Untermeyer, The Detection of Fissionable Materials by
    Nondestructive Means, American Nuclear Society Monograph, 1980.
    This relatively short book summarizes the principles of most
    nondestructive assay methods and briefly describes many typical
    applications, including those of high-resolution gamma ray
    spectroscopy. Chapters 3 and 5 are of particular interest since
    they deal, respectively, with nuclear detection methods and
    passive NDA techniques. The book also contains many references to
    original papers and reports.
    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 establish and maintain a system of
    control and accountability so that the standard error of any inventory
    difference 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 are essential for the maintenance of these standards.
    Many types of nondestructive assay (NDA) measurements on SNM can
    involve, or even require, a high-resolution gamma ray spectroscopy
    system. The proposed action is to provide some general guidelines in
    the selection of such systems and to point out useful resources for more
    detailed information on their assembly, optimization, and use in
    material protection measurements.
    1.2 Need for Proposed Action
    Regulatory Guide 5.9, which provides guidance in this area, has
    not been updated since 1974 and does not contain a list of pertinent
    information currently available in the literature.
    1.3 Value/Impact of Proposed Action
    1.3.1NRC Operations
    The experience and improvements in detector technology that have
    occurred since the guide was issued will be made available for 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 more recent detector
    technology discussed in the guide, updating these techniques should have
    no adverse impact.
    1.3.4Public
    No adverse impact on the public can be foreseen.
    1.4 Decision on Proposed Action
    The guide should be revised to reflect improvements in techniques,
    to bring the guide into conformity with current practice, and to provide
    a list of pertinent information currently available.
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 5.9 should be revised to bring it up to date.
    49