Regulatory Guide 5.38: Difference between revisions

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{{#Wiki_filter:U.S. ATOMIC ENERGY COMMISSION
{{#Wiki_filter:September 1974 U.S. ATOMIC ENERGY COMMISSION
REGULATORY  
                                REGULATORY
GI DIRECTORATE  
                                DIRECTORATE OF REGULATORY STANDARDS
OF REGULATORY  
                                                                                                                                GI JIDE
STANDARDS REGULATORY  
                                                                  REGULATORY GUIDE 5.38 NONDESTRUCTIVE ASSAY OF HIGH-ENRICHMENT URANIUM
GUIDE 5.38 NONDESTRUCTIVE  
                                          FUEL PLATES BY GAMMA RAY SPECTROMETRY
ASSAY OF HIGH-ENRICHMENT  
URANIUM FUEL PLATES BY GAMMA RAY SPECTROMETRY
September
1974 JIDE


==A. INTRODUCTION==
==A. INTRODUCTION==
Part 70 of Title 10 of the Code of Federal Regula-tions requires each licensee authorized to possess more than 350 grams of contained U-235 to conduct a physical inventory of all special nuclear material in his possession at intervals not to exceed 12 months. Each licensee authorized to possess more than one effective kilogram of high-enrichment uranium is required to conduct measured physical inventories of his special nuclear materials at bimonthly intervals.
nondestructive assay of high-enrichment fuel plates by Part 70 of Title 10 of the Code of Federal Regula-                               gamma ray spectrometry (Ref. 1). The 185.7-keV
tions requires each licensee authorized to possess more                             gamma ray is the most useful U-235 gamma ray for this than 350 grams of contained U-235 to conduct a                                     application; it is emitted at the rate of 4.25 x 104 gamma rays per second per gram of U-235. Lower- physical inventory of all special nuclear material in his possession at intervals not to exceed 12 months. Each                               energy gamma rays emitted by U-235 are less pene- trating and more sensitive to errors due to fluctuations licensee authorized to possess more than one effective kilogram of high-enrichment uranium is required to                                   in clad and core thickness. In general, more accurate fuel conduct measured physical inventories of his special                                 plate assays may be made by measuring only the activity nuclear materials at bimonthly intervals. Further, these                            attributable to the 185.7-keV U-235 gamma ray.


Further, these licensees are required to conduct their nuclear material physical inventories in compliance with specific require-ments set forth in Part 70. Inventory procedures acceptable to the Regulatory  
licensees are required to conduct their nuclear material                                 Assay measurements are made by integrating the physical inventories in compliance with specific require-                           response observed during the scanning of single fuel ments set forth in Part 70. Inventory procedures                                     plates and comparing each response to a calibration acceptable to the Regulatory +,afffor complying with                                 based on the response to known calibration standards.
+,aff for complying with thesc pi 'wisions of Part 70 are detailed in Regulatory Guide 5.13. "Conduct of Nuclear Material Physical Invcntories." For certain nuclear reactors, the fuel consists of highly enriched uranium fabricated into flat or bowed plates. Typically, these plates are relatively thin so that a significant percentage of the U-235 gamma rays ptle-trate the fuel cladding.


When the measurement condi-tions are properly controlled and corrections are made for variations in the attenuation of the gamma rays, a measurement of the U-235 gamma rays can be used as an acceptable measurement of the distribution and the total U-235 content of each fuel plate. In lieu of assaying the product fuel plates, fuel plate core compacts may be assayed through the procedures detailed in this guide, provided steps are taken to ensure the traceability and integrity of encapsulation of each assayed fuel plate core compact. This guide describes features of a gamma ray spectrometry system acceptable to the Regulatory staff for nondestructive assay of high-enrichment uranium fuel plates or fuel plate core compacts.
thesc pi 'wisions of Part 70 are detailed in Regulatory Guide 5.13. "Conduct of Nuclear Material Physical                                            1. GAMMA RAY MEASUREMENT SYSTEM
Invcntories."
      For certain nuclear reactors, the fuel consists of                              1.1 GAMMA RAY DETECTION SYSTEM
highly enriched uranium fabricated into flat or bowed plates. Typically, these plates are relatively thin so that a                        1.1.1 Gamma Ray Detector significant percentage of the U-235 gamma rays ptle- trate the fuel cladding. When the measurement condi-                                     High-resolution gamma ray detectors, i.e., intrinsic or tions are properly controlled and corrections are made                               lithium-drifted germanium, provide resolution beyond for variations in the attenuation of the gamma rays, a                               that required for this assay application. While the measurement of the U-235 gamma rays can be used as an                                 performance of such detectors is more than adequate, acceptable measurement of the distribution and the total                             their low intrinsic detection efficiency, extensive opera- U-235 content of each fuel plate. In lieu of assaying the                             tional and maintenance requirements, and high cost product fuel plates, fuel plate core compacts may be                                 make them unattractive for this application.


==B. DISCUSSION==
assayed through the procedures detailed in this guide, provided steps are taken to ensure the traceability and                                  Most ,sodium iodide [Nal (TI)] scintillation detectors are capable of sufficient energy resolution to be used for integrity of encapsulation of each assayed fuel plate core the measurement of the 185.7-keV gamma rays. The compact. This guide describes features of a gamma ray detector diameter is determined by the fuel plate width spectrometry system acceptable to the Regulatory staff and the scanning method selected (see Section B.I.2 of for nondestructive assay of high-enrichment uranium this guide). The thickness of the Nal crystal is selected fuel plates or fuel plate core compacts.
The number, energy, and intensity of gamma rays associated with the decay of U-235 provide the basis for nondestructive assay of high-enrichment fuel plates by gamma ray spectrometry (Ref. 1). The 185.7-keV gamma ray is the most useful U-235 gamma ray for this application;
it is emitted at the rate of 4.25 x 104 gamma rays per second per gram of U-235. Lower-energy gamma rays emitted by U-235 are less pene-trating and more sensitive to errors due to fluctuations in clad and core thickness.


In general, more accurate fuel plate assays may be made by measuring only the activity attributable to the 185.7-keV
to avoid unnecessary sensitivity to gamma rays above the  
U-235 gamma ray.Assay measurements are made by integrating the response observed during the scanning of single fuel plates and comparing each response to a calibration based on the response to known calibration standards.


1. GAMMA RAY MEASUREMENT
==B. DISCUSSION==
SYSTEM 1.1 GAMMA RAY DETECTION
185-keV region which produce a background in the
SYSTEM 1.1.1 Gamma Ray Detector High-resolution gamma ray detectors, i.e., intrinsic or lithium-drifted germanium, provide resolution beyond that required for this assay application.
                                                                                      185-keV energy region as a result of Compton scattering.


While the performance of such detectors is more than adequate, their low intrinsic detection efficiency, extensive opera-tional and maintenance requirements, and high cost make them unattractive for this application.
The number, energy, and intensity of gamma rays                                      For measurements to be reproducible, it is necessary associated with the decay of U-235 provide the basis for                             to assure that the detection system is stabilized on the USAEC REGULATORY GUIDES                                      Cop.- of published guids may be obtained by request indicintng the dinirsom deired to the US. Atomic Erw Commismson. Vlhington. D.C. 20545.


Most ,sodium iodide [Nal (TI)] scintillation detectors are capable of sufficient energy resolution to be used for the measurement of the 185.7-keV
RegulatmrV Guide are ssued to iescribe and make availabte to the puublic            Attlntion: Director of Regulatory Standstills. Comments wed suggestions for nalhods c.acptable to tht AEC Regulatory st&ff of imiplemnting specific parts of    ifl3hmtflts in thes guides we o fiurqlpd and should be sent to the Secretary the Commnisson* s regulations, to delineate technqlus      .sead by the staff in  of the Comnssmion, US. Atomic EnoqW Commission. Washington, D.C. 20545.
gamma rays. The detector diameter is determined by the fuel plate width and the scanning method selected (see Section B.I.2 of this guide). The thickness of the Nal crystal is selected to avoid unnecessary sensitivity to gamma rays above the 185-keV region which produce a background in the 185-keV energy region as a result of Compton scattering.


For measurements to be reproducible, it is necessary to assure that the detection system is stabilized on the USAEC REGULATORY
oealuat-0n specific problems or postulated accidents, or to provide guidenws to     Attention: Do-kteting and SorveceSection.
GUIDES Cop.- of published guids may be obtained by request indicintng the dinirsom deired to the US. Atomic Erw Commismson.


Vlhington.
aml)icents. Regulatory Guides wit not substitutes for regulations and comNpflanio with them is not re*uired. Methods and sofutions diffrt      from tfeor lit out in The guides are          in the following ten broaeddivisions:
                                                                                                      ,ssued t.  guides well beaasipgtobl if they piroind a basis for the findingl requisits to the iiufnt*ior oiminuenOt of a permit or licnese by the Commtissson.                  1. Powr Reectorn                           


D.C. 2054
===6. Products===
 
                                                                                      2. Research and Test Ractors                
===5. RegulatmrV ===
Guide are ssued to iescribe and make availabte to the puublic Attlntion:
Director of Regulatory Standstills.
 
Comments wed suggestions for nalhods c.acptable to tht AEC Regulatory st&ff of imiplemnting specific parts of ifl3hmtflts in thes guides we o fiurqlpd and should be sent to the Secretary the s regulations, to delineate technqlus .sead by the staff in of the Comnssmion, US. Atomic EnoqW Commission.
 
Washington, D.C. 20545.oealuat-0n specific problems or postulated accidents, or to provide guidenws to Attention:
Do-kteting and Sorvece Section.aml)icents.
 
Regulatory Guides wit not substitutes for regulations and comNpflanio with them is not Methods and sofutions diffrt from tfeor lit out in The guides are ,ssued in the following ten broaed divisions:
t. guides well bea asipgtobl if they piroind a basis for the findingl requisits to the or oiminuenOt of a permit or licnese by the Commtissson.
 
1. Powr Reectorn 6. Products 2. Research and Test Ractors  


===7. Tranpomrtation===
===7. Tranpomrtation===
3. Fuels isid Materi- Fac;itisi a. O=upetiona!  
                                                                                      3.     isid Materi- Fac;itisi Fuels                                    a. O=upetiona! Meeilh Pubfb*ied guides will be revised periodicafly. as approprate. to accomn oal           4. Environmenetal end Siting                 9. Antitrust Review comments and to reflect new ,ntormition or expoerine.                                 5. Mot'earits and Plant Protection         1
Meeilh guides will be revised periodicafly.
 
as approprate.
 
to accomn oal 4. Environmenetal end Siting 9. Antitrust Review comments and to reflect new ,ntormition or expoerine.
 
5. Mot'earits and Plant Protection  
10. Generaf intended portion of the gamma ray spectrum during measurements.
 
Internally "seeded" Nal crystals which contain a radioactive source (typically Am-241) to produce a reference energy pulse art commercially available.
 
The detection system is stabilized on the reference, and the amplifier gain is automatically cor-rected to assure that that energy and the rest of the spectrum remain fixed in position..1.2 Gamma Ray Collimator To ensure that the only gamma ray activity detected originates from a well-defined segment of the fuel plate, the detector is shielded from extraneous background radiations and collimated to define the area "seen" by the detector crystal. The collimator consists of a disk of appropriate shielding material.
 
A slit is machined through the center of the disk which will allow only those gamma rays emitted within the slit opening to strike the detector.
 
The disk thickness is a minimum of six mean free path lengths to effectively stop all gamma rays emitted from outside the view area. To prevent gamma rays from striking the crystal around the edges of the collimator disk, the disk diameter exceeds the crystal diameter by at least twice the crystal depth.The probability of detection for gamma rays emitted at the center of the collimator slit is greater than that for gamma rays emitted near the ends of the slit. This effect becomes increasingly important at small detector-to- plate spacing, especially when scanning near the edge of a plate. To minimize this detection nonuniformity and to minimize the sensitivity to jitter, the detector-to-plate distance can be made large, especially with respect to the dimensions of the slit opening. As an alternative means of reducing the detection nonuniformity-across the slit, the slit opening can be divided into channels by inserting a honeycomb baffle into the slit or by fabricating the collimator by drilling holes through the disk in a pattern which ensures that each hole is surrounded by a minimum wall thickness of 0.2 mean free path length. A 7:0-cm-thick iron disk with holes less than 0.5 cm in diameter drilled in a pattern having 0.2 cm of wall between adjacent holes is one example of a collimator that would perform satisfactorily.
 
A large number of small-diameter holes is preferable to a few large-diameter holes.1.1.3 Multiple Detectors Several detectors may be used to shorten the mea-surement time. The detectors can be positioned to simultaneously measure different segments of a single fuel plate or to simultaneously measure additional fuel plates. In some cases it may be useful to sum the response from two detectors positioned on opposite sides of a plate to increase counting efficiency.
 
In such cases it is essential that the response of such detectors be balanced-and checked at frequent intervals.
 
1.2 SCANNING TECIINIQUES
It is critical that the scanningapparatds for ,'oviog t:, plates relative to the detector provide a uniforn;.reproducible scan. The importance of a well-constructed, mechanically stable conveyor cannot be overemphasized.
 
Either the detector can be moved and the plate held stationary, or the plate can be moved past a fixed detector.
 
Care must be exercised to maintain fl detector-to-plate spacing within close tolerance, minimize errors caused by the inverse-square dcpen(!of detection on distance.
 
This is especially important in the case of close spacing, which is sometimes desirable to maximize the count rate. Various commercial conveying systems have been used and found to be adequate.
 
Such.systems may significantly reduce the cost of de..,7!i, g and building new scanning mechanisms.
 
High-precision tool equipment such as milling machines, lathes, and x-y scanning tables can be investigated.
 
Numerically con-trolled units offer additional advantages when they can be incorporated into a scanning system. This is particu-larly true when an automated scanning system is being developed.
 
Fuel plate core compacts may be sufficiently small permit total assay without scanning in a fixed-geometry counting system. The scanning techniques for fuel plates discussed in the following subsections can also be used for core compacts when total fixed compact counting is not possible.1.2.1 Linear Total Scan The detector collimation consists of a rectangular opening which extends across the width of the fuel plates beyond the edges of the uranium core contained within the plate cladding.
 
Scanning the total plate is accomplished by starting the count sequence on the end of a -plate and continuing to count until the entire length of plate has been scanned.To ensure that gamma rays emitted anywhere across the face of the fuel plate have an equal probability of being detected, it is necesary that the diameter of the detector crystal exceed the plate width or that the detector be positioned away from the plate.Use of the spot oi cizcalar collimator scan technique eliminates or reduces to insignificance most of these edge effects.1.2.2 Sweeping Spot Scan (Ref. 2)If the collimator channel width is smaller than the fuel plate width, the viewing area (spot) can be swept across the plate as the detector scans along the length of the plate. This scanning technique can be readily adapted to scanning bowed plates through the use of a cam which is designed to maintain the detector-to-plate distance constant over the entire geometry of the fuel plate. The collimator channel dimensions can be selected to provide compatible information on the uniformity of 5.38-2 the fuel plate which is frequently obtained by comparing fixed (static) spot counts at a variety of locations to reference counts.1.2.3 Sampled Increment Assay When used in conjunction with radiographic dimen-sional measurements performed on all fuel plates, the U-235 content of a fuel plate can be measured by scanning the ends of each fuel plate and sampling the balance of the plate. It is necessary to measure the dimensions of the fuel core loading radiographically, through gamma ray scanning along the length of the plate, or by spot scanning the fuel plate ends and measuring the distance between end spots where the fuel loading stops. The U-235 content of the plate is then determined by averaging the results of sample spot measurements of the U-235 content per unit area at a number of sites along the plate and multiplying this average value by the measured area of the fuel core. The radiograph of each plate is examined to ensure that the core filter is uniform.The collimator shape and dimensions can be selected to provide compatible information on the uniformity of the fuel plate.1.3 COMPUTER CONTROL The reproducibility of measurements can be im-proved and the measurement time per fuel plate can be reduced by using a computer to control the fuel plate scanning operation.
 
The computer can be used to control data acquisition by accumulating counts ac-cording to a predetermined scheme. Also, the computer can be used for data analysis, including background corrections and intermachine normalization, calibration, error analysis, and diagnostic test measurements and analyses.
 
Report preparation and data recording for subsequent analysis are also readily accomplished through an appropriately designed computer-controlled system.
 
===2. INTERPRETATION ===
OF MEASUREMENT
DATA The three factors discussed below may give rise to significant errors in interpreting measurement data.2.1 ENRICHMENT
vARIATIONS
Licensees authorized to possess highly enriched uranium are required to account for element and isotope as prescribed in §70.51. Under the conditions detailed in this guide, the U-235 content of individual plates is measured.
 
To determine the total uranium content of each plate, the U-235 enrichment must be known from separate measurements.
 
Enrichment variations may alter the radiation back-ground in the gamma ray energy region of interest.Uranium-238 decays by alpha-particle .emission to Th-234. Thorium-234 then decays by beta-particle emis-sion with a half-life of 24.1 days to Pa-234 which, in turn, decays by beta-particle emission to U-234. Ap-proximately
1% of the Pa-234 decays are followed by high-energy (e.g., 1001 keV, 766 keV) gamma rays.These gamma rays frequently lose energy through Compton scattering and may appear in the 185-keV spectral region. It is important to note that activity from Pa-234 may be altered by disturbing the equilibrium between U-235 and Th-234, as frequently occurs in uranium chemical conversion processes.
 
The interference due to variations in U-238 daughter activity becomes less important as the enrichment of U-235 increases.
 
At enrichment levels above 90%, this problem can essen-tially be ignored.2.2 RADIATION
ATTENUATION
The number of U-235 gamma rays which escape from the fuel plate (and are thus available for detection)
without losing energy depends on the characteristics of the fuel plate core and cladding.
 
Gamma rays from U-235 are attenuated in the uranium, in the cladding, and in the inert material that may be added with the uranium to form the core of the fuel plate. Through well-controlled product tolerance limits, each of these potential sources of signal variability can be controlled to permit accurate accountability assays.2.2.1 Self-Attenuation The uranium photon attenuation coefficient for gamma ray energies corresponding to U-235 emissions is quite large (Ref. 3). Small changes in uranium density resulting from increased fuel loading or from variations in the manufacturing process can significantly change the number of gamma rays which escape from the fuel plate.2.2.2 Gadding Attentuation Small variations in cladding thickness may cause significant attenuation variations.


Variations in cladding attenuation can be measured by a simple gamma ray absorption test using thin sheets of cladding material as absorbers and varying the clad thickness over the range of thicknesses to be encountered in normal product variability.
===0. Generaf===


2.2.3 Core Friler Attenuation Radiation intensity measurements may be made of plates fabricated with different ratios of uranium to filler to show the effects of this type of attenuation.
intended portion of the gamma ray spectrum during                  1.2 SCANNING TECIINIQUES
measurements. Internally "seeded" Nal crystals which contain a radioactive source (typically Am-241) to                      It is critical that the scanningapparatds for ,'oviogt:,
produce a reference energy pulse art commercially                    plates relative to the detector provide a uniforn;.
  available. The detection system is stabilized on the                reproducible scan. The importance of a well-constructed, reference, and the amplifier gain is automatically cor-            mechanically stable conveyor cannot be overemphasized.


If significant effects are noted, plates can be categorized by core composition characteristics and the assay system can be independently calibrated for each category of fuel plates.5.38-3
rected to assure that that energy and the rest of the              Either the detector can be moved and the plate held spectrum remain fixed in position.                                  stationary, or the plate can be moved past a fixed detector. Care must be exercised to maintain fl
2.2.4 Attenuation Corrections When the thickness of the core and cladding of each plate is known, an attenuation correction can be applied to improve the accuracy of the assay. Ultrasonic gauging may provide such a measure, provided the metallo-graphic zones within the plate are sufficiently defined to provide a detectable interface.
  .1.2 Gamma Ray Collimator                                          detector-to-plate spacing within close tolerance, minimize errors caused by the inverse-square dcpen(!
                                                                      of detection on distance. This is especially important in To ensure that the only gamma ray activity detected              the case of close spacing, which is sometimes desirable to originates from a well-defined segment of the fuel plate,           maximize the count rate. Various commercial conveying the detector is shielded from extraneous background systems have been used and found to be adequate. Such.


The alternative attenuation- correction is based on a micrometer measurement of the total thickness of each plate. The clad thickness of a plate is estimated by subtracting the mean core thickness of the product plates, which is determined by periodically sampling product plates and cutting a cross section to permit visual measurement of clad and core thickness.
radiations and collimated to define the area "seen" by systems may significantly reduce the cost of de..,7!i, g the detector crystal. The collimator consists of a disk of and building new scanning mechanisms. High-precision appropriate shielding material. A slit is machined tool equipment such as milling machines, lathes, and x-y through the center of the disk which will allow only scanning tables can be investigated. Numerically con- those gamma rays emitted within the slit opening to trolled units offer additional advantages when they can strike the detector. The disk thickness is a minimum of be incorporated into a scanning system. This is particu- six mean free path lengths to effectively stop all gamma larly true when an automated scanning system is being rays emitted from outside the view area. To prevent developed.


2.3 INTERFERING
gamma rays from striking the crystal around the edges of Fuel plate core compacts may be sufficiently small the collimator disk, the disk diameter exceeds the crystal permit total assay without scanning in a fixed-geometry diameter by at least twice the crystal depth.
RADIATIONS
As noted in Section B.2.1 of this guide, an internal background variation may arise from changes in the amount of U.238 present in a fuel plate or from changes in the ratio of Th-234 to U-238 resulting from fuel manufacturing processes.


Fluctuations in the internal background cause the response of the unknown items to be different from the calibration standards, thereby creating a measurement bias. Such interferences can be compensated by measuring additional regions of the gamma ray spectrum.Other interfering radiations may come from external sources, from fuel plates awaiting assay, or from nearby radiation sources used for other measurements.
counting system. The scanning techniques for fuel plates The probability of detection for gamma rays emitted discussed in the following subsections can also be used at the center of the collimator slit is greater than that for for core compacts when total fixed compact counting is gamma rays emitted near the ends of the slit. This effect becomes increasingly important at small detector-to-                not possible.


This is not expected to be a major problem and can be controlled through (1) removing radiation sources, (2) shielding the detectors, and (3) monitoring the back-ground at frequent intervals.
plate spacing, especially when scanning near the edge of a plate. To minimize this detection nonuniformity and
                                                                      1.2.1 Linear Total Scan to minimize the sensitivity to jitter, the detector-to-plate The detector collimation consists of a rectangular distance can be made large, especially with respect to the opening which extends across the width of the fuel dimensions of the slit opening. As an alternative means plates beyond the edges of the uranium core contained of reducing the detection nonuniformity-across the slit, within the plate cladding. Scanning the total plate is the slit opening can be divided into channels by inserting accomplished by starting the count sequence on the end a honeycomb baffle into the slit or by fabricating the              of a -plate and continuing to count until the entire length collimator by drilling holes through the disk in a pattern of plate has been scanned.


===3. CALIBRATION ===
which ensures that each hole is surrounded by a To ensure that gamma rays emitted anywhere across minimum wall thickness of 0.2 mean free path length. A
AND VERIFICATION
                                                                    the face of the fuel plate have an equal probability of
3.1 INITIAL OPERATIONS
7:0-cm-thick iron disk with holes less than 0.5 cm in              being detected, it is necesary that the diameter of the diameter drilled in a pattern having 0.2 cm of wall detector crystal exceed the plate width or that the between adjacent holes is one example of a collimator detector that would perform satisfactorily. A large number of                    Use ofbethe positioned away from the plate.
Calibration and the verification of assay predictions is an ongoing effort where performance is periodically monitored and the calibration relationship is modified to improve the accuracy of assay predictions.


During initial operations, two means of basing preliminary calibrations are appropriate.
spot oi cizcalar collimator scan technique small-diameter holes is preferable to a few large-diameter eliminates or reduces to insignificance most of these holes.


3.1.1 Foil Calibration Technique Methods for calibrating scanning systems for high-enrichment uranium fuel plates through the assay of prepared uranium and clad foils are described in Refer-ence 2. This method may be used in place of or in addition to the -technique described in the following subsection.
edge effects.


uranium, U-235, inert matrix, and cladding are accu-rately measured and that these parameters bracket the nominal range of product plates anticipated to fall within manufacturing tolerances.
1.1.3 Multiple Detectors                                            1.2.2 Sweeping Spot Scan (Ref. 2)
    Several detectors may be used to shorten the mea-                    If the collimator channel width is smaller than the surement time. The detectors can be positioned to                    fuel plate width, the viewing area (spot) can be swept simultaneously measure different segments of a single                across the plate as the detector scans along the length of fuel plate or to simultaneously measure additional fuel              the plate. This scanning technique can be readily plates. In some cases it may be useful to sum the                    adapted to scanning bowed plates through the use of a response from two detectors positioned on opposite                  cam which is designed to maintain the detector-to-plate sides of a plate to increase counting efficiency. In such            distance constant over the entire geometry of the fuel cases it is essential that the response of such detectors be        plate. The collimator channel dimensions can be selected balanced-and checked at frequent intervals.                          to provide compatible information on the uniformity of
                                                              5.38-2


3.2 ROUTINE OPERATIONS
the fuel plate which is frequently obtained by comparing        Uranium-238 decays by alpha-particle .emission to fixed (static) spot counts at a variety of locations to        Th-234. Thorium-234 then decays by beta-particle emis- reference counts.                                               sion with a half-life of 24.1 days to Pa-234 which, in turn, decays by beta-particle emission to U-234. Ap-
The performance of the assay system is periodically monitored to ensure that the performance of the assay system has not shifted since its last calibration.
1.2.3 Sampled Increment Assay                                  proximately 1% of the Pa-234 decays are followed by high-energy (e.g., 1001 keV, 766 keV) gamma rays.


Control limits for acceptable performance can be established for the response to an appropriate working standard.
When used in conjunction with radiographic dimen-          These gamma rays frequently lose energy through sional measurements performed on all fuel plates, the          Compton scattering and may appear in the 185-keV
U-235 content of a fuel plate can be measured by                spectral region. It is important to note that activity from scanning the ends of each fuel plate and sampling the          Pa-234 may be altered by disturbing the equilibrium balance of the plate. It is necessary to measure the            between U-235 and Th-234, as frequently occurs in dimensions of the fuel core loading radiographically,          uranium chemical conversion processes. The interference through gamma ray scanning along the length of the              due to variations in U-238 daughter activity becomes less plate, or by spot scanning the fuel plate ends and              important as the enrichment of U-235 increases. At measuring the distance between end spots where the fuel        enrichment levels above 90%, this problem can essen- loading stops. The U-235 content of the plate is then          tially be ignored.


The control chart of the responses to the working standard can be checked for indications of short-term instrument drift or malfunction.
determined by averaging the results of sample spot measurements of the U-235 content per unit area at a            2.2 RADIATION ATTENUATION
number of sites along the plate and multiplying this average value by the measured area of the fuel core. The           The number of U-235 gamma rays which escape from radiograph of each plate is examined to ensure that the        the fuel plate (and are thus available for detection)
core filter is uniform.                                        without losing energy depends on the characteristics of The collimator shape and dimensions can be selected        the fuel plate core and cladding. Gamma rays from to provide compatible information on the uniformity of         U-235 are attenuated in the uranium, in the cladding, the fuel plate.                                                 and in the inert material that may be added with the uranium to form the core of the fuel plat


The control chart can also be analyzed to detect long-term shifts within the measurement-to-measurement control limits that may be corrected by recalibrating the system. Severe changes in instrument performance are investigated promptly and their causes remedied.To ensure that the calibration remains valid during normal operations and that accuracy estimates are rigorously justified, assay predictions are periodically compared with more accurate measurements of the content of typical fuel plates (see Section C.4 of this guide). Guidance on methods to relate this assay to the national measurement system and to reconcile verifi-cation measurements will be addressed in separate regulatory guides.*C. REGULATORY
====e. Through====
POSITION The content and distribution of U-235 in high-enrichment uranium plates can be measured through the gamma ray assay methods described in this guide.Combining this measurement with the results of an independent measurement of the U-235 enrichment enables the total uranium content of the fuel plates to be measured.
1.3 COMPUTER CONTROL                                          well-controlled product tolerance limits, each of these potential sources of signal variability can be controlled The reproducibility of measurements can be im-             to permit accurate accountability assays.


The factors presented below should be taken into consideration for this assay method to be acceptable to the Regulatory staff.I. MEASUREMENT
proved and the measurement time per fuel plate can be reduced by using a computer to control the fuel plate          2.2.1 Self-Attenuation scanning operation. The computer can be used to control data acquisition by accumulating counts ac-                The uranium photon attenuation coefficient for cording to a predetermined scheme. Also, the computer          gamma ray energies corresponding to U-235 emissions is can be used for data analysis, including background            quite large (Ref. 3). Small changes in uranium density corrections and intermachine normalization, calibration,        resulting from increased fuel loading or from variations error analysis, and diagnostic test measurements and            in the manufacturing process can significantly change analyses. Report preparation and data recording for            the number of gamma rays which escape from the fuel subsequent analysis are also readily accomplished              plate.
SYSTEM 1.1 GAMMA RAY MEASUREMENT
SYSTEM 1.1.1 Gamma Ray Detector A thallium-activated sodium iodide scintillation detector or series of detectors is recommended for this assay application.


When more than one detector is to be incorporated into the scan system, the performance characteristics of the detectors should be matched. The diameter of the crystal should be larger than the projected view onto the crystal face through the*For example, regulatory guides related to measurement quality amurance and calibration of nondestructive a&say systems are being developed.
through an appropriately designed computer-controlled system.                                                        2.2.2 Gadding Attentuation
  2. INTERPRETATION OF MEASUREMENT DATA                            Small variations in cladding thickness may cause significant attenuation variations. Variations in cladding attenuation can be measured by a simple gamma ray The three factors discussed below may give rise to        absorption test using thin sheets of cladding material as significant errors in interpreting measurement data.            absorbers and varying the clad thickness over the range of thicknesses to be encountered in normal product
2.1 ENRICHMENT vARIATIONS                                      variability.


3.1.2 Fabricated Calibration Plates Calibration standard fuel plates can be fabricated using special precautions to ensure that the amounts of 5.38-4 collimator channel. The thickness of the crystal should hc noi more than onc inch. The crystal should contain an internal cesium iodide seed which is doped with a suilable alpha-emittcr for spectral stabilization.
Licensees authorized to possess highly enriched            2.2.3 Core Friler Attenuation uranium are required to account for element and isotope as prescribed in §70.51. Under the conditions detailed              Radiation intensity measurements may be made of in this guide, the U-235 content of individual plates is        plates fabricated with different ratios of uranium to measured. To determine the total uranium content of            filler to show the effects of this type of attenuation. If each plate, the U-235 enrichment must be known from            significant effects are noted, plates can be categorized by separate measurements.                                         core composition characteristics and the assay system Enrichment variations may alter the radiation back-        can be independently calibrated for each category of ground in the gamma ray energy region of interest.             fuel plates.


The seed should produce approximately
5.38-3
1,000 counts per second at the reference energy.1.1.2 Collimator A collimator should be fabricated of appropriate gamma ray shielding material such as iron, lead, or tungsten.


The shielding should completely surround the detector and photomultiplier assembly and should be sufficiently thick to completely block extraneous radi-ations from the detector.
2.2.4 Attenuation Corrections                                      uranium, U-235, inert matrix, and cladding are accu- rately measured and that these parameters bracket the When the thickness of the core and cladding of each            nominal range of product plates anticipated to fall plate is known, an attenuation correction can be applied          within manufacturing tolerances.


The response variation from the center of the collimator opening to its edge should be less than 1%.1.1.3 Electronic Apparatus All electronic systems should be powered by filtered, highly regulated power supplies.
to improve the accuracy of the assay. Ultrasonic gauging may provide such a measure, provided the metallo-                  3.2 ROUTINE OPERATIONS
  graphic zones within the plate are sufficiently defined to provide a detectable interface.                                      The performance of the assay system is periodically The alternative attenuation- correction is based on a          monitored to ensure that the performance of the assay micrometer measurement of the total thickness of each            system has not shifted since its last calibration. Control plate. The clad thickness of a plate is estimated by              limits for acceptable performance can be established for subtracting the mean core thickness of the product                the response to an appropriate working standard. The plates, which is determined by periodically sampling              control chart of the responses to the working standard product plates and cutting a cross section to permit              can be checked for indications of short-term instrument visual measurement of clad and core thickness.                     drift or malfunction. The control chart can also be analyzed    to  detect    long-term    shifts  within  the
2.3 INTERFERING RADIATIONS                                        measurement-to-measurement control limits that may be corrected by recalibrating the system. Severe changes in As noted in Section B.2.1 of this guide, an internal          instrument performance are investigated promptly and background variation may arise from changes in the                their causes remedied.


The ambient tempera-ture and humidity in the vicinity of the scanning system should be controlled so that permitted fluctuations do not significantly affect the assay measurements.
amount of U.238 present in a fuel plate or from changes                To ensure that the calibration remains valid during in the ratio of Th-234 to U-238 resulting from fuel                normal operations and that accuracy estimates are manufacturing processes. Fluctuations in the internal              rigorously justified, assay predictions are periodically background cause the response of the unknown items to              compared with more accurate measurements of the be different from the calibration standards, thereby              content of typical fuel plates (see Section C.4 of this creating a measurement bias. Such interferences can be            guide). Guidance on methods to relate this assay to the compensated by measuring additional regions of the                national measurement system and to reconcile verifi- gamma ray spectrum.                                                cation measurements      will be addressed in separate Other interfering radiations may come from external            regulatory guides.*
sources, from fuel plates awaiting assay, or from nearby radiation sources used for other measurements. This is not expected to be a major problem and can be                                   


All electronic circuitry in signal-processing components should feature temperature compensation.
==C. REGULATORY POSITION==
controlled through (1) removing radiation sources,
(2) shielding the detectors, and (3) monitoring the back-              The content and distribution of U-235 in high- ground at frequent intervals.                                    enrichment uranium plates can be measured through the gamma ray assay methods described in this guide.


Residual sen-sitivity to fluctuations in the, ambient environment should be tested and monitored periodically.
3. CALIBRATION AND VERIFICATION                          Combining this measurement with the results of an independent measurement of the U-235 enrichment
3.1 INITIAL OPERATIONS                                            enables the total uranium content of the fuel plates to be measured. The factors presented below should be taken into consideration for this assay method to be Calibration and the verification of assay predictions is an ongoing effort where performance is periodically               acceptable to the Regulatory staff.


The capability for multichannel gamma ray pulse height analysis with cathode ray tube spectral display should be provided.
monitored and the calibration relationship is modified to improve the accuracy of assay predictions. During initial                        I. MEASUREMENT SYSTEM
operations, two means of basing preliminary calibrations are appropriate.                                                  1.1 GAMMA RAY MEASUREMENT SYSTEM
3.1.1 Foil Calibration Technique                                  1.1.1 Gamma Ray Detector Methods for calibrating scanning systems for high-                A thallium-activated sodium iodide scintillation enrichment uranium fuel plates through the assay of                detector or series of detectors is recommended for this prepared uranium and clad foils are described in Refer-          assay application. When more than one detector is to be ence 2. This method may be used in place of or in                incorporated into the scan system, the performance characteristics of the detectors should be matched. The addition to the -technique described in the following subsection.                                                      diameter of the crystal should be larger than the projected view onto the crystal face through the
3.1.2 Fabricated Calibration Plates
                                                                  *For example, regulatory guides related to measurement quality Calibration standard fuel plates can be fabricated              amurance and calibration of nondestructive a&say systems are using special precautions to ensure that the amounts of            being developed.


Signal-processing electronics capable of stabilizing on the alpha radiations emitted within the doped cesium iodide seed should be provided to stabilize the energy spectrum.1.2 SCANNING SYSTEM A mechanically sound, highly reproducible scanning system should be employed.
5.38-4


Scanning should be accom-plished by one of the three techniques discussed in Section B. 1.2 of this guide.1.3 COMPUTER CONTROL A dedicated minicomputer to control data acquisi-tion, analysis, calibration, diagnostic testing, and report preparation -should be employed for this assay appli-cation.1.4 MULTIPLE SCANNING ASSAY SYSTEMS When more than ornc scanning system is employed, assay response should be normalized so that each instrument provides consistent results. Verification data to establish the systeniatic assay error for each assay system should be obtained with the same plate.
collimator channel. The thickness of the crystal should                    2. MEASUREMENT INTERPRETATION
hc noi more than onc inch. The crystal should contain an internal cesium iodide seed which is doped with a                  2.1 ENRICHMENT VARIATIONS
suilable alpha-emittcr for spectral stabilization. The seed should produce approximately 1,000 counts per second                    Procedures should be developed to ensure that the at the reference energy.                                            enrichment of the plates being scanned is known through separate measurements. Fuel plates generally
1.1.2 Collimator                                                    satisfy the gamma ray penetrability criteria for quantita- tive U-235 assay; they do not satisfy the criteria for A collimator should be fabricated of appropriate                nondestructive enrichment measurement through gamma gamma ray shielding material such as iron, lead, or                ray spectrometry.* Facilities processing more than one uranium enrichment should maintain strict isotopic tungsten. The shielding should completely surround the detector and photomultiplier assembly and should be                 control and characterize the enrichment through appri.,-
sufficiently thick to completely block extraneous radi-            priate measurement methods.


===2. MEASUREMENT ===
ations from the detector. The response variation from the center of the collimator opening to its edge should            2.2 ATTENUATION CORRECTIONS
INTERPRETATION
be less than 1%.
2.1 ENRICHMENT
                                                                        Attenuation variations arising from plate-to-plate changes in core thickness, composition,-and clad thick-
VARIATIONS
1.1.3 Electronic Apparatus                                          ness should be determined over the range of product tolerance specifications. When such variations cause the All electronic systems should be powered by filtered,          assay error to exceed the error realized without the highly regulated power supplies. The ambient tempera-              variations by 50% or more, procedures should be ture and humidity in the vicinity of the scanning system          implemented to measure and apply a correction to the should be controlled so that permitted fluctuations do              assay of each plate.
Procedures should be developed to ensure that the enrichment of the plates being scanned is known through separate measurements.


Fuel plates generally satisfy the gamma ray penetrability criteria for quantita-tive U-235 assay; they do not satisfy the criteria for nondestructive enrichment measurement through gamma ray spectrometry.*
not significantly affect the assay measurements. All electronic circuitry in signal-processing components                2.3 RADIATION INTERFERENCES
Facilities processing more than one uranium enrichment should maintain strict isotopic control and characterize the enrichment through appri.,-priate measurement methods.2.2 ATTENUATION
should feature temperature compensation. Residual sen- sitivity to fluctuations in the, ambient environment                    A clear plastic template which shows an acceptable should be tested and monitored periodically.                      spectrum display should be prepared. When radioactive The capability for multichannel gamma ray pulse                interference may be encountered, the assay spectrum height analysis with cathode ray tube spectral display              should be compared at appropriate intervals to the should be provided. Signal-processing electronics capable          reference spectrum for indications of interference. Bick- of stabilizing on the alpha radiations emitted within the          ground radiation should be measured periodically during doped cesium iodide seed should be provided to stabilize            each operating shift.
CORRECTIONS
Attenuation variations arising from plate-to-plate changes in core thickness, composition,-and clad thick-ness should be determined over the range of product tolerance specifications.


When such variations cause the assay error to exceed the error realized without the variations by 50% or more, procedures should be implemented to measure and apply a correction to the assay of each plate.2.3 RADIATION
the energy spectrum.
INTERFERENCES
A clear plastic template which shows an acceptable spectrum display should be prepared.


When radioactive interference may be encountered, the assay spectrum should be compared at appropriate intervals to the reference spectrum for indications of interference.
3. MEASUREMENT CALIBRATION
1.2 SCANNING SYSTEM
                                                                        During initial operations, the assay system should m, A mechanically sound, highly reproducible scanning            calibrated either by the foil calibration method or with system should be employed. Scanning should be accom-                specially prepared sample fuel plates as described mn plished by one of the three techniques discussed in                  Section B.3.1 of this guide.


Bick-ground radiation should be measured periodically during each operating shift.
Section B. 1.2 of this guide.


===3. MEASUREMENT ===
4. RANDOM AND SYSTEMATIC ASSAY ERRORS
CALIBRATION
1.3 COMPUTER CONTROL
During initial operations, the assay system should m, calibrated either by the foil calibration method or with specially prepared sample fuel plates as described mn Section B.3.1 of this guide.4. RANDOM AND SYSTEMATIC  
                                                                    4.1 RANDOM ERROR ESTIMATION
ASSAY ERRORS 4.1 RANDOM ERROR ESTIMATION
    A dedicated minicomputer to control data acquisi- tion, analysis, calibration, diagnostic testing, and report              A replicate assay program should be established to generate data for the evaluation of random assay errOrs preparation -should be employed for this assay appli- during each material balance period. During each bi- cation.
A replicate assay program should be established to generate data for the evaluation of random assay errOrs during each material balance period. During each bi-monthly interval, a minimum of fifteen plates should be selected for replicate assay. The second assay of each plate selected for replicate assay should be made at least four hours after the first assay. Replicate assay diffet-ences should be collected and analyzed at the end (if the*Criteria for uranium gamma ray enrichment arff given in Regulatory Guide 5.21, "Nondestructrvr ltiranwurn.235 Enrichment Assay by Gamma Ray
" 5.38-5 material balance period. The single-measurement stan-dard deviation of the relative replicate assay differences should be computed as described in Reference
4.4.2 SYSTEMATIC
ERROR ESTIMATION
The systematic error associated with the assay of all fuel plates fabricated during a material balance period should be determined through one of the procedures*
presented below.4.2.1 Propagation through the Calibration Function To estimate the systematic assay error through the calibration function, the calibration should be based on the regression analysis of an appropriate function to the calibration data. Uncertainties in the reference values of the calibration standards should be factored into the fit, and the errors propagated as demonstrated in Reference 5.To ensure the validity of the predictions, the stable performance of the instrument should be monitored and normalized through the response to appropriate working standards which are assayed at frequent intervals.


The frequency for assaying working standards should be determined through testing, but should not be lower than one test during each two-hour assay interval for spot response stability and one full scan test during each operating shift. Indications of shifting instrument perfor-mance should be investigated and remedied, and the instrument should be recalibrated to ensure the validity of subsequent measurements.
monthly interval, a minimum of fifteen plates should be selected for replicate assay. The second assay of each
1.4 MULTIPLE SCANNING ASSAY SYSTEMS                                plate selected for replicate assay should be made at least four hours after the first assay. Replicate assay diffet- When more than ornc scanning system is employed,               ences should be collected and analyzed at the end (if the assay response should be normalized so that each instrument provides consistent results. Verification data          *Criteria for uranium gamma ray enrichment measurenicTi*r.    arff to establish the systeniatic assay error for each assay              given in Regulatory Guide 5.21, "Nondestructrvr ltiranwurn.235 system should be obtained with the same plate.                        Enrichment Assay by Gamma Ray Spectromelr\* "
                                                            5.38-5


In order to ensure that the calibration standards continue to adequately represent the unknown fuel plates, key production parameters which affect the observed response should be monitored through separate tests. Data should be compiled and analyzed at the close of each material balance period. When a production parameter shifts from previously established values, the impact of the shift on the response of the assay instrument should be determined through an appropriate experiment or. calculation (Ref. 6). A bias correction should be determined and applied to all items assayed from the point of the parameter change. The uncertainty in the bias should be combined with the systematic error predicted through the calibration function.
material balance period. The single-measurement stan-                A minimum of one new calibration standard fuel plate dard deviation of the relative replicate assay differences          should be introduced during each six-month period.


When the bias exceeds 3% of the plate contents in a single material balance period, when a trend of 1.5% or more is observed in three consecutive material balance periods, ,)r when the uncertainty in the observed bias is sufficient to increase the limit of error of the assay above 0.5%, new calibration standards should be obtained, and the scanning system should be recalibrated.
should be computed as described in Reference 4.


As a further check on the continued validity of the calibration standards, a program to periodically intro-duce new calibration standards should be implemented.
4.2.2 Comparative Evaluation
  4.2 SYSTEMATIC ERROR ESTIMATION
                                                                            When two measurements are made on each of a series The systematic error associated with the assay of all            of items and the accuracy of ono of the methods used is fuel plates fabricated during a material balance period              considerably greater than the other, the corresponding should be determined through one of the procedures*                  predictions can be compared to establish an estimate of presented below.                                                    bias between the measurement methods and to estimate the error. associated with the lens-accurate measurement
  4.2.1 Propagation through the Calibration Function                    method. To precisely determine the systematic error in the nondestructive assay, the fuel plates selected for To estimate the systematic assay error through the                comparative measurements should be randomly selected calibration function, the calibration should be based on             but should span the range of U-235 contents en- the regression analysis of an appropriate function to the           countered in normal production. The selected fuel plates calibration data. Uncertainties in the reference values of           may be rejected from the process stream for failing to the calibration standards should be factored into the fit,          meet quality assurance requirements. Each plate should and the errors propagated as demonstrated in Reference              be repeatedly assayed to reduce the random asay error
  5.                                                                  to less than 10% of the estimated or previously To ensure the validity of the predictions, the stable            established systematic error. To determine its U-235 and performance of the instrument should be monitored and                total uranium content, the plate should be completely normalized through the response to appropriate working                dissolved and the resulting solution should be analyzed standards which are assayed at frequent intervals. The                by high-accuracy chemical and mass spectrometric pro- frequency for assaying working standards should be                   cedures.


*These methods will be discussed in detail in a regulatory guide ,n preparation entitled "Calibration and Error Estimation Pr:ccduir"s fcr Nondestructi-e Asay." A minimum of one new calibration standard fuel plate should be introduced during each six-month period.4.2.2 Comparative Evaluation When two measurements are made on each of a series of items and the accuracy of ono of the methods used is considerably greater than the other, the corresponding predictions can be compared to establish an estimate of bias between the measurement methods and to estimate the error. associated with the lens-accurate measurement method. To precisely determine the systematic error in the nondestructive assay, the fuel plates selected for comparative measurements should be randomly selected but should span the range of U-235 contents en-countered in normal production.
determined through testing, but should not be lower                      For one material balance period during the initial than one test during each two-hour assay interval for                implementation of this guide; a product fuel plate spot response stability and one full scan test during each            should be randomly selected twice each week for an operating shift. Indications of shifting instrument perfor-         accuracy verification measurement. Following this initial mance should be investigated and remedied, and the                   implementation period, facilities manufacturing 100 or instrument should be recalibrated to ensure the validity              more fuel plates per week may reduce the verification of subsequent measurements.                                          frequency to one plate per week and pool the verifi- In order to ensure that the calibration standards                cation data for two consecutive material balance periods.


The selected fuel plates may be rejected from the process stream for failing to meet quality assurance requirements.
continue to adequately represent the unknown fuel                     LoW-throughput facilities manufacturing lesa than 100
plates, key production parameters which affect the                    plates per week should verify at least 4 plates per observed response should be monitored through separate                material balance period through the procedures de- tests. Data should be compiled and analyzed at the close              scribed above. At the close of each material balance of each material balance period. When a production                    period, data should be pooled to include only the 15 parameter shifts from previously established values, the             most current data points.


Each plate should be repeatedly assayed to reduce the random asay error to less than 10% of the estimated or previously established systematic error. To determine its U-235 and total uranium content, the plate should be completely dissolved and the resulting solution should be analyzed by high-accuracy chemical and mass spectrometric pro-cedures.For one material balance period during the initial implementation of this guide; a product fuel plate should be randomly selected twice each week for an accuracy verification measurement.
impact of the shift on the response of the assay                          When the U-235 contents of the plates assayed using a instrument should be determined through an appropriate                common calibration relationship varies over a ranpg of experiment or. calculation (Ref. 6). A bias correction                +/-5% or more about the average of all plate loadings, the should be determined and applied to all items assayed                  systematic error should be estimated as described in from the point of the parameter change. The uncertainty              paragraph 1. below; when plate loadings are tightly in the bias should be combined with the systematic error              clustered about a nominal value, the systematic error predicted through the calibration function. When the                  should be estimated as described in paragraph 2.


Following this initial implementation period, facilities manufacturing
bias exceeds 3% of the plate contents in a single material balance period, when a trend of 1.5% or more is                            1. At the close of the reporting period, the assay observed in three consecutive material balance periods,              value for each plate is plotted against the verified
100 or more fuel plates per week may reduce the verification frequency to one plate per week and pool the verifi-cation data for two consecutive material balance periods.LoW-throughput facilities manufacturing lesa than 100 plates per week should verify at least 4 plates per material balance period through the procedures de-scribed above. At the close of each material balance period, data should be pooled to include only the 15 most current data points.When the U-235 contents of the plates assayed using a common calibration relationship varies over a ranpg of+/-5% or more about the average of all plate loadings, the systematic error should be estimated as described in paragraph
,)r when the uncertainty in the observed bias is sufficient          quantity. The verification data plot is examined for to increase the limit of error of the assay above 0.5%,              indications of nonlinearity or obvious outlier data.
1. below; when plate loadings are tightly clustered about a nominal value, the systematic error should be estimated as described in paragraph
2.1. At the close of the reporting period, the assay value for each plate is plotted against the verified quantity.


The verification data plot is examined for indications of nonlinearity or obvious outlier data.Anomalous indications should be investigated and remedied.A linear regression analysis should be performed on the comparison data. The intercept should be tested against zero for an indication of a constant measurement bias. The slope shouid be tested against unity for an indication of a proportional bias. When bias is indicated, assays performed during the preceding operating period should be compensated.
new calibration standards should be obtained, and the                Anomalous indications should be investigated and scanning system should be recalibrated.                               remedied.


The systematic error should be 5.38-6 estimated as the standard error associated with the verification line.2. When all plates contain essentially the same U-235 content, the difference in the mean content values should be tested against zero as an indication of bias, and the systematic error associated with an inventory of plates should be quoted as the standard deviation of the mean difference.
As a further check on the continued validity of the                  A linear regression analysis should be performed on calibration standards, a program to periodically intro-               the comparison data. The intercept should be tested duce new calibration standards should be implemented.                against zero for an indication of a constant measurement bias. The slope shouid be tested against unity for an
*These methods will be discussed in detail in a regulatory guide      indication of a proportional bias. When bias is indicated,
  ,n preparation entitled "Calibration and Error Estimation          assays performed during the preceding operating period Pr:ccduir"s fcr Nondestructi-e Asay."                              should be compensated. The systematic error should be
                                                              5.38-6


For individual plates, the systematic error should be quoted as the standard deviation of the difference distribution.
estimated as the standard error associated with the                1. Each core compact should carry a unique identifi- verification line.                                              cation. Accountability records should be created for each compact. The fuel plate should carry an identifica-
    2. When all plates contain essentially the same U-235      tion corresponding to the compact identification.


5. CORE COMPACT ASSAY Final product assay in high-enrichment fuel plate manufacturing can also be accomplished through assay-ing each core compact following the procedures detailed in this guide and the following supplemental criteria: 1. Each core compact should carry a unique identifi-cation. Accountability records should be created for each compact. The fuel plate should carry an identifica- tion corresponding to the compact identification.
content, the difference in the mean content values should be tested against zero as an indication of bias, and the systematic error associated with an inventory of          2. Each fuel plate should be radiographically exam- plates should be quoted as the standard deviation of the      ined to ensure that the entire compact has been mean difference. For individual plates, the systematic        encapsulated.


2. Each fuel plate should be radiographically exam-ined to ensure that the entire compact has been encapsulated.
error should be quoted as the standard deviation of the difference distribution.


3. Each fuel plate should be checked with a gamma ray probe to qualitatively ensure that the plate core is uranium of the nominal product enrichment.
3. Each fuel plate should be checked with a gamma
                5. CORE COMPACT ASSAY                          ray probe to qualitatively ensure that the plate core is uranium of the nominal product enrichment.


4. Calibration and error evaluation should follow the procedures for fuel plate assa
Final product assay in high-enrichment fuel plate manufacturing can also be accomplished through assay- ing each core compact following the procedures detailed            4. Calibration and error evaluation should follow the in this guide and the following supplemental criteria:          procedures for fuel plate assay.


====y. REFERENCES====
REFERENCES
I. J.E. Cline, R.J. Gehrke, and L.D. Mclsaac, "Gamma Rays Emitted by the Fissionable Nuclides and Asso-ciated Isotopes," ANCR-1029 (July 1972).2. N.S. Beyer, "Assay of U-235 in Nuclear Reactor Fuel Elements by Gamma Ray Scintillation Spec-trometry," Proc. 4th Intl. Conf. on Nondestructive Testing, London, 1963.3. J.H. Hubbell, "Photon Cross Sections, Attenuation Coefficients, and Energy Absorption Coefficients from 10 keV to 100 GeV," Nat. Bur. Stds.NSRDS-NBS
I. J.E. Cline, R.J. Gehrke, and L.D. Mclsaac, "Gamma           4. John L. Jaech, "Statistical Methods in Nuclear Rays Emitted by the Fissionable Nuclides and Asso-             Materials Control," TID-26298 (1973).
29 (1969).4. John L. Jaech, "Statistical Methods in Nuclear Materials Control," TID-26298
    ciated Isotopes," ANCR-1029 (July 1972).                   5. American National Standard N15.20, "Guide to
(1973).5. American National Standard N15.20, "Guide to Calibrating Nondestructive Assay Systems," in preparation.
2. N.S. Beyer, "Assay of U-235 in Nuclear Reactor Fuel             Calibrating Nondestructive Assay Systems," in Elements by Gamma Ray Scintillation Spec-                       preparation. Copies of the draft standard may be trometry," Proc. 4th Intl. Conf. on Nondestructive             obtained from Institute of Nuclear Materials Manage- Testing, London, 1963.                                           ment, 505 King Avenue, Columbus, Ohio 43201
3. J.H. Hubbell, "Photon Cross Sections, Attenuation               (Attention: H.L. Toy).
  Coefficients, and Energy Absorption Coefficients             6. See, for example, R.A. Forster, D.B. Smith, and H.O.


Copies of the draft standard may be obtained from Institute of Nuclear Materials Manage-ment, 505 King Avenue, Columbus, Ohio 43201 (Attention:
from 10 keV to 100 GeV," Nat. Bur. Stds.                       Menlove, "Error Analysis of a Cf-252 Fuel Rod Assay NSRDS-NBS 29 (1969).                                            System,'" LA-5317 (1974).
H.L. Toy).6. See, for example, R.A. Forster, D.B. Smith, and H.O.Menlove, "Error Analysis of a Cf-252 Fuel Rod Assay System,'" LA-5317 (1974).5.38-7}}
                                                        5.38-7}}


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Nondestructive Assay of High-Enrichment Uranium Fuel Plates by Gamma Ray Spectrometry
ML13064A076
Person / Time
Issue date: 09/30/1974
From:
US Atomic Energy Commission (AEC)
To:
References
RG-5.038
Download: ML13064A076 (7)


September 1974 U.S. ATOMIC ENERGY COMMISSION

REGULATORY

DIRECTORATE OF REGULATORY STANDARDS

GI JIDE

REGULATORY GUIDE 5.38 NONDESTRUCTIVE ASSAY OF HIGH-ENRICHMENT URANIUM

FUEL PLATES BY GAMMA RAY SPECTROMETRY

A. INTRODUCTION

nondestructive assay of high-enrichment fuel plates by Part 70 of Title 10 of the Code of Federal Regula- gamma ray spectrometry (Ref. 1). The 185.7-keV

tions requires each licensee authorized to possess more gamma ray is the most useful U-235 gamma ray for this than 350 grams of contained U-235 to conduct a application; it is emitted at the rate of 4.25 x 104 gamma rays per second per gram of U-235. Lower- physical inventory of all special nuclear material in his possession at intervals not to exceed 12 months. Each energy gamma rays emitted by U-235 are less pene- trating and more sensitive to errors due to fluctuations licensee authorized to possess more than one effective kilogram of high-enrichment uranium is required to in clad and core thickness. In general, more accurate fuel conduct measured physical inventories of his special plate assays may be made by measuring only the activity nuclear materials at bimonthly intervals. Further, these attributable to the 185.7-keV U-235 gamma ray.

licensees are required to conduct their nuclear material Assay measurements are made by integrating the physical inventories in compliance with specific require- response observed during the scanning of single fuel ments set forth in Part 70. Inventory procedures plates and comparing each response to a calibration acceptable to the Regulatory +,afffor complying with based on the response to known calibration standards.

thesc pi 'wisions of Part 70 are detailed in Regulatory Guide 5.13. "Conduct of Nuclear Material Physical 1. GAMMA RAY MEASUREMENT SYSTEM

Invcntories."

For certain nuclear reactors, the fuel consists of 1.1 GAMMA RAY DETECTION SYSTEM

highly enriched uranium fabricated into flat or bowed plates. Typically, these plates are relatively thin so that a 1.1.1 Gamma Ray Detector significant percentage of the U-235 gamma rays ptle- trate the fuel cladding. When the measurement condi- High-resolution gamma ray detectors, i.e., intrinsic or tions are properly controlled and corrections are made lithium-drifted germanium, provide resolution beyond for variations in the attenuation of the gamma rays, a that required for this assay application. While the measurement of the U-235 gamma rays can be used as an performance of such detectors is more than adequate, acceptable measurement of the distribution and the total their low intrinsic detection efficiency, extensive opera- U-235 content of each fuel plate. In lieu of assaying the tional and maintenance requirements, and high cost product fuel plates, fuel plate core compacts may be make them unattractive for this application.

assayed through the procedures detailed in this guide, provided steps are taken to ensure the traceability and Most ,sodium iodide [Nal (TI)] scintillation detectors are capable of sufficient energy resolution to be used for integrity of encapsulation of each assayed fuel plate core the measurement of the 185.7-keV gamma rays. The compact. This guide describes features of a gamma ray detector diameter is determined by the fuel plate width spectrometry system acceptable to the Regulatory staff and the scanning method selected (see Section B.I.2 of for nondestructive assay of high-enrichment uranium this guide). The thickness of the Nal crystal is selected fuel plates or fuel plate core compacts.

to avoid unnecessary sensitivity to gamma rays above the

B. DISCUSSION

185-keV region which produce a background in the

185-keV energy region as a result of Compton scattering.

The number, energy, and intensity of gamma rays For measurements to be reproducible, it is necessary associated with the decay of U-235 provide the basis for to assure that the detection system is stabilized on the USAEC REGULATORY GUIDES Cop.- of published guids may be obtained by request indicintng the dinirsom deired to the US. Atomic Erw Commismson. Vlhington. D.C. 20545.

RegulatmrV Guide are ssued to iescribe and make availabte to the puublic Attlntion: Director of Regulatory Standstills. Comments wed suggestions for nalhods c.acptable to tht AEC Regulatory st&ff of imiplemnting specific parts of ifl3hmtflts in thes guides we o fiurqlpd and should be sent to the Secretary the Commnisson* s regulations, to delineate technqlus .sead by the staff in of the Comnssmion, US. Atomic EnoqW Commission. Washington, D.C. 20545.

oealuat-0n specific problems or postulated accidents, or to provide guidenws to Attention: Do-kteting and SorveceSection.

aml)icents. Regulatory Guides wit not substitutes for regulations and comNpflanio with them is not re*uired. Methods and sofutions diffrt from tfeor lit out in The guides are in the following ten broaeddivisions:

,ssued t. guides well beaasipgtobl if they piroind a basis for the findingl requisits to the iiufnt*ior oiminuenOt of a permit or licnese by the Commtissson. 1. Powr Reectorn

6. Products

2. Research and Test Ractors

7. Tranpomrtation

3. isid Materi- Fac;itisi Fuels a. O=upetiona! Meeilh Pubfb*ied guides will be revised periodicafly. as approprate. to accomn oal 4. Environmenetal end Siting 9. Antitrust Review comments and to reflect new ,ntormition or expoerine. 5. Mot'earits and Plant Protection 1

0. Generaf

intended portion of the gamma ray spectrum during 1.2 SCANNING TECIINIQUES

measurements. Internally "seeded" Nal crystals which contain a radioactive source (typically Am-241) to It is critical that the scanningapparatds for ,'oviogt:,

produce a reference energy pulse art commercially plates relative to the detector provide a uniforn;.

available. The detection system is stabilized on the reproducible scan. The importance of a well-constructed, reference, and the amplifier gain is automatically cor- mechanically stable conveyor cannot be overemphasized.

rected to assure that that energy and the rest of the Either the detector can be moved and the plate held spectrum remain fixed in position. stationary, or the plate can be moved past a fixed detector. Care must be exercised to maintain fl

.1.2 Gamma Ray Collimator detector-to-plate spacing within close tolerance, minimize errors caused by the inverse-square dcpen(!

of detection on distance. This is especially important in To ensure that the only gamma ray activity detected the case of close spacing, which is sometimes desirable to originates from a well-defined segment of the fuel plate, maximize the count rate. Various commercial conveying the detector is shielded from extraneous background systems have been used and found to be adequate. Such.

radiations and collimated to define the area "seen" by systems may significantly reduce the cost of de..,7!i, g the detector crystal. The collimator consists of a disk of and building new scanning mechanisms. High-precision appropriate shielding material. A slit is machined tool equipment such as milling machines, lathes, and x-y through the center of the disk which will allow only scanning tables can be investigated. Numerically con- those gamma rays emitted within the slit opening to trolled units offer additional advantages when they can strike the detector. The disk thickness is a minimum of be incorporated into a scanning system. This is particu- six mean free path lengths to effectively stop all gamma larly true when an automated scanning system is being rays emitted from outside the view area. To prevent developed.

gamma rays from striking the crystal around the edges of Fuel plate core compacts may be sufficiently small the collimator disk, the disk diameter exceeds the crystal permit total assay without scanning in a fixed-geometry diameter by at least twice the crystal depth.

counting system. The scanning techniques for fuel plates The probability of detection for gamma rays emitted discussed in the following subsections can also be used at the center of the collimator slit is greater than that for for core compacts when total fixed compact counting is gamma rays emitted near the ends of the slit. This effect becomes increasingly important at small detector-to- not possible.

plate spacing, especially when scanning near the edge of a plate. To minimize this detection nonuniformity and

1.2.1 Linear Total Scan to minimize the sensitivity to jitter, the detector-to-plate The detector collimation consists of a rectangular distance can be made large, especially with respect to the opening which extends across the width of the fuel dimensions of the slit opening. As an alternative means plates beyond the edges of the uranium core contained of reducing the detection nonuniformity-across the slit, within the plate cladding. Scanning the total plate is the slit opening can be divided into channels by inserting accomplished by starting the count sequence on the end a honeycomb baffle into the slit or by fabricating the of a -plate and continuing to count until the entire length collimator by drilling holes through the disk in a pattern of plate has been scanned.

which ensures that each hole is surrounded by a To ensure that gamma rays emitted anywhere across minimum wall thickness of 0.2 mean free path length. A

the face of the fuel plate have an equal probability of

7:0-cm-thick iron disk with holes less than 0.5 cm in being detected, it is necesary that the diameter of the diameter drilled in a pattern having 0.2 cm of wall detector crystal exceed the plate width or that the between adjacent holes is one example of a collimator detector that would perform satisfactorily. A large number of Use ofbethe positioned away from the plate.

spot oi cizcalar collimator scan technique small-diameter holes is preferable to a few large-diameter eliminates or reduces to insignificance most of these holes.

edge effects.

1.1.3 Multiple Detectors 1.2.2 Sweeping Spot Scan (Ref. 2)

Several detectors may be used to shorten the mea- If the collimator channel width is smaller than the surement time. The detectors can be positioned to fuel plate width, the viewing area (spot) can be swept simultaneously measure different segments of a single across the plate as the detector scans along the length of fuel plate or to simultaneously measure additional fuel the plate. This scanning technique can be readily plates. In some cases it may be useful to sum the adapted to scanning bowed plates through the use of a response from two detectors positioned on opposite cam which is designed to maintain the detector-to-plate sides of a plate to increase counting efficiency. In such distance constant over the entire geometry of the fuel cases it is essential that the response of such detectors be plate. The collimator channel dimensions can be selected balanced-and checked at frequent intervals. to provide compatible information on the uniformity of

5.38-2

the fuel plate which is frequently obtained by comparing Uranium-238 decays by alpha-particle .emission to fixed (static) spot counts at a variety of locations to Th-234. Thorium-234 then decays by beta-particle emis- reference counts. sion with a half-life of 24.1 days to Pa-234 which, in turn, decays by beta-particle emission to U-234. Ap-

1.2.3 Sampled Increment Assay proximately 1% of the Pa-234 decays are followed by high-energy (e.g., 1001 keV, 766 keV) gamma rays.

When used in conjunction with radiographic dimen- These gamma rays frequently lose energy through sional measurements performed on all fuel plates, the Compton scattering and may appear in the 185-keV

U-235 content of a fuel plate can be measured by spectral region. It is important to note that activity from scanning the ends of each fuel plate and sampling the Pa-234 may be altered by disturbing the equilibrium balance of the plate. It is necessary to measure the between U-235 and Th-234, as frequently occurs in dimensions of the fuel core loading radiographically, uranium chemical conversion processes. The interference through gamma ray scanning along the length of the due to variations in U-238 daughter activity becomes less plate, or by spot scanning the fuel plate ends and important as the enrichment of U-235 increases. At measuring the distance between end spots where the fuel enrichment levels above 90%, this problem can essen- loading stops. The U-235 content of the plate is then tially be ignored.

determined by averaging the results of sample spot measurements of the U-235 content per unit area at a 2.2 RADIATION ATTENUATION

number of sites along the plate and multiplying this average value by the measured area of the fuel core. The The number of U-235 gamma rays which escape from radiograph of each plate is examined to ensure that the the fuel plate (and are thus available for detection)

core filter is uniform. without losing energy depends on the characteristics of The collimator shape and dimensions can be selected the fuel plate core and cladding. Gamma rays from to provide compatible information on the uniformity of U-235 are attenuated in the uranium, in the cladding, the fuel plate. and in the inert material that may be added with the uranium to form the core of the fuel plat

e. Through

1.3 COMPUTER CONTROL well-controlled product tolerance limits, each of these potential sources of signal variability can be controlled The reproducibility of measurements can be im- to permit accurate accountability assays.

proved and the measurement time per fuel plate can be reduced by using a computer to control the fuel plate 2.2.1 Self-Attenuation scanning operation. The computer can be used to control data acquisition by accumulating counts ac- The uranium photon attenuation coefficient for cording to a predetermined scheme. Also, the computer gamma ray energies corresponding to U-235 emissions is can be used for data analysis, including background quite large (Ref. 3). Small changes in uranium density corrections and intermachine normalization, calibration, resulting from increased fuel loading or from variations error analysis, and diagnostic test measurements and in the manufacturing process can significantly change analyses. Report preparation and data recording for the number of gamma rays which escape from the fuel subsequent analysis are also readily accomplished plate.

through an appropriately designed computer-controlled system. 2.2.2 Gadding Attentuation

2. INTERPRETATION OF MEASUREMENT DATA Small variations in cladding thickness may cause significant attenuation variations. Variations in cladding attenuation can be measured by a simple gamma ray The three factors discussed below may give rise to absorption test using thin sheets of cladding material as significant errors in interpreting measurement data. absorbers and varying the clad thickness over the range of thicknesses to be encountered in normal product

2.1 ENRICHMENT vARIATIONS variability.

Licensees authorized to possess highly enriched 2.2.3 Core Friler Attenuation uranium are required to account for element and isotope as prescribed in §70.51. Under the conditions detailed Radiation intensity measurements may be made of in this guide, the U-235 content of individual plates is plates fabricated with different ratios of uranium to measured. To determine the total uranium content of filler to show the effects of this type of attenuation. If each plate, the U-235 enrichment must be known from significant effects are noted, plates can be categorized by separate measurements. core composition characteristics and the assay system Enrichment variations may alter the radiation back- can be independently calibrated for each category of ground in the gamma ray energy region of interest. fuel plates.

5.38-3

2.2.4 Attenuation Corrections uranium, U-235, inert matrix, and cladding are accu- rately measured and that these parameters bracket the When the thickness of the core and cladding of each nominal range of product plates anticipated to fall plate is known, an attenuation correction can be applied within manufacturing tolerances.

to improve the accuracy of the assay. Ultrasonic gauging may provide such a measure, provided the metallo- 3.2 ROUTINE OPERATIONS

graphic zones within the plate are sufficiently defined to provide a detectable interface. The performance of the assay system is periodically The alternative attenuation- correction is based on a monitored to ensure that the performance of the assay micrometer measurement of the total thickness of each system has not shifted since its last calibration. Control plate. The clad thickness of a plate is estimated by limits for acceptable performance can be established for subtracting the mean core thickness of the product the response to an appropriate working standard. The plates, which is determined by periodically sampling control chart of the responses to the working standard product plates and cutting a cross section to permit can be checked for indications of short-term instrument visual measurement of clad and core thickness. drift or malfunction. The control chart can also be analyzed to detect long-term shifts within the

2.3 INTERFERING RADIATIONS measurement-to-measurement control limits that may be corrected by recalibrating the system. Severe changes in As noted in Section B.2.1 of this guide, an internal instrument performance are investigated promptly and background variation may arise from changes in the their causes remedied.

amount of U.238 present in a fuel plate or from changes To ensure that the calibration remains valid during in the ratio of Th-234 to U-238 resulting from fuel normal operations and that accuracy estimates are manufacturing processes. Fluctuations in the internal rigorously justified, assay predictions are periodically background cause the response of the unknown items to compared with more accurate measurements of the be different from the calibration standards, thereby content of typical fuel plates (see Section C.4 of this creating a measurement bias. Such interferences can be guide). Guidance on methods to relate this assay to the compensated by measuring additional regions of the national measurement system and to reconcile verifi- gamma ray spectrum. cation measurements will be addressed in separate Other interfering radiations may come from external regulatory guides.*

sources, from fuel plates awaiting assay, or from nearby radiation sources used for other measurements. This is not expected to be a major problem and can be

C. REGULATORY POSITION

controlled through (1) removing radiation sources,

(2) shielding the detectors, and (3) monitoring the back- The content and distribution of U-235 in high- ground at frequent intervals. enrichment uranium plates can be measured through the gamma ray assay methods described in this guide.

3. CALIBRATION AND VERIFICATION Combining this measurement with the results of an independent measurement of the U-235 enrichment

3.1 INITIAL OPERATIONS enables the total uranium content of the fuel plates to be measured. The factors presented below should be taken into consideration for this assay method to be Calibration and the verification of assay predictions is an ongoing effort where performance is periodically acceptable to the Regulatory staff.

monitored and the calibration relationship is modified to improve the accuracy of assay predictions. During initial I. MEASUREMENT SYSTEM

operations, two means of basing preliminary calibrations are appropriate. 1.1 GAMMA RAY MEASUREMENT SYSTEM

3.1.1 Foil Calibration Technique 1.1.1 Gamma Ray Detector Methods for calibrating scanning systems for high- A thallium-activated sodium iodide scintillation enrichment uranium fuel plates through the assay of detector or series of detectors is recommended for this prepared uranium and clad foils are described in Refer- assay application. When more than one detector is to be ence 2. This method may be used in place of or in incorporated into the scan system, the performance characteristics of the detectors should be matched. The addition to the -technique described in the following subsection. diameter of the crystal should be larger than the projected view onto the crystal face through the

3.1.2 Fabricated Calibration Plates

  • For example, regulatory guides related to measurement quality Calibration standard fuel plates can be fabricated amurance and calibration of nondestructive a&say systems are using special precautions to ensure that the amounts of being developed.

5.38-4

collimator channel. The thickness of the crystal should 2. MEASUREMENT INTERPRETATION

hc noi more than onc inch. The crystal should contain an internal cesium iodide seed which is doped with a 2.1 ENRICHMENT VARIATIONS

suilable alpha-emittcr for spectral stabilization. The seed should produce approximately 1,000 counts per second Procedures should be developed to ensure that the at the reference energy. enrichment of the plates being scanned is known through separate measurements. Fuel plates generally

1.1.2 Collimator satisfy the gamma ray penetrability criteria for quantita- tive U-235 assay; they do not satisfy the criteria for A collimator should be fabricated of appropriate nondestructive enrichment measurement through gamma gamma ray shielding material such as iron, lead, or ray spectrometry.* Facilities processing more than one uranium enrichment should maintain strict isotopic tungsten. The shielding should completely surround the detector and photomultiplier assembly and should be control and characterize the enrichment through appri.,-

sufficiently thick to completely block extraneous radi- priate measurement methods.

ations from the detector. The response variation from the center of the collimator opening to its edge should 2.2 ATTENUATION CORRECTIONS

be less than 1%.

Attenuation variations arising from plate-to-plate changes in core thickness, composition,-and clad thick-

1.1.3 Electronic Apparatus ness should be determined over the range of product tolerance specifications. When such variations cause the All electronic systems should be powered by filtered, assay error to exceed the error realized without the highly regulated power supplies. The ambient tempera- variations by 50% or more, procedures should be ture and humidity in the vicinity of the scanning system implemented to measure and apply a correction to the should be controlled so that permitted fluctuations do assay of each plate.

not significantly affect the assay measurements. All electronic circuitry in signal-processing components 2.3 RADIATION INTERFERENCES

should feature temperature compensation. Residual sen- sitivity to fluctuations in the, ambient environment A clear plastic template which shows an acceptable should be tested and monitored periodically. spectrum display should be prepared. When radioactive The capability for multichannel gamma ray pulse interference may be encountered, the assay spectrum height analysis with cathode ray tube spectral display should be compared at appropriate intervals to the should be provided. Signal-processing electronics capable reference spectrum for indications of interference. Bick- of stabilizing on the alpha radiations emitted within the ground radiation should be measured periodically during doped cesium iodide seed should be provided to stabilize each operating shift.

the energy spectrum.

3. MEASUREMENT CALIBRATION

1.2 SCANNING SYSTEM

During initial operations, the assay system should m, A mechanically sound, highly reproducible scanning calibrated either by the foil calibration method or with system should be employed. Scanning should be accom- specially prepared sample fuel plates as described mn plished by one of the three techniques discussed in Section B.3.1 of this guide.

Section B. 1.2 of this guide.

4. RANDOM AND SYSTEMATIC ASSAY ERRORS

1.3 COMPUTER CONTROL

4.1 RANDOM ERROR ESTIMATION

A dedicated minicomputer to control data acquisi- tion, analysis, calibration, diagnostic testing, and report A replicate assay program should be established to generate data for the evaluation of random assay errOrs preparation -should be employed for this assay appli- during each material balance period. During each bi- cation.

monthly interval, a minimum of fifteen plates should be selected for replicate assay. The second assay of each

1.4 MULTIPLE SCANNING ASSAY SYSTEMS plate selected for replicate assay should be made at least four hours after the first assay. Replicate assay diffet- When more than ornc scanning system is employed, ences should be collected and analyzed at the end (if the assay response should be normalized so that each instrument provides consistent results. Verification data *Criteria for uranium gamma ray enrichment measurenicTi*r. arff to establish the systeniatic assay error for each assay given in Regulatory Guide 5.21, "Nondestructrvr ltiranwurn.235 system should be obtained with the same plate. Enrichment Assay by Gamma Ray Spectromelr\* "

5.38-5

material balance period. The single-measurement stan- A minimum of one new calibration standard fuel plate dard deviation of the relative replicate assay differences should be introduced during each six-month period.

should be computed as described in Reference 4.

4.2.2 Comparative Evaluation

4.2 SYSTEMATIC ERROR ESTIMATION

When two measurements are made on each of a series The systematic error associated with the assay of all of items and the accuracy of ono of the methods used is fuel plates fabricated during a material balance period considerably greater than the other, the corresponding should be determined through one of the procedures* predictions can be compared to establish an estimate of presented below. bias between the measurement methods and to estimate the error. associated with the lens-accurate measurement

4.2.1 Propagation through the Calibration Function method. To precisely determine the systematic error in the nondestructive assay, the fuel plates selected for To estimate the systematic assay error through the comparative measurements should be randomly selected calibration function, the calibration should be based on but should span the range of U-235 contents en- the regression analysis of an appropriate function to the countered in normal production. The selected fuel plates calibration data. Uncertainties in the reference values of may be rejected from the process stream for failing to the calibration standards should be factored into the fit, meet quality assurance requirements. Each plate should and the errors propagated as demonstrated in Reference be repeatedly assayed to reduce the random asay error

5. to less than 10% of the estimated or previously To ensure the validity of the predictions, the stable established systematic error. To determine its U-235 and performance of the instrument should be monitored and total uranium content, the plate should be completely normalized through the response to appropriate working dissolved and the resulting solution should be analyzed standards which are assayed at frequent intervals. The by high-accuracy chemical and mass spectrometric pro- frequency for assaying working standards should be cedures.

determined through testing, but should not be lower For one material balance period during the initial than one test during each two-hour assay interval for implementation of this guide; a product fuel plate spot response stability and one full scan test during each should be randomly selected twice each week for an operating shift. Indications of shifting instrument perfor- accuracy verification measurement. Following this initial mance should be investigated and remedied, and the implementation period, facilities manufacturing 100 or instrument should be recalibrated to ensure the validity more fuel plates per week may reduce the verification of subsequent measurements. frequency to one plate per week and pool the verifi- In order to ensure that the calibration standards cation data for two consecutive material balance periods.

continue to adequately represent the unknown fuel LoW-throughput facilities manufacturing lesa than 100

plates, key production parameters which affect the plates per week should verify at least 4 plates per observed response should be monitored through separate material balance period through the procedures de- tests. Data should be compiled and analyzed at the close scribed above. At the close of each material balance of each material balance period. When a production period, data should be pooled to include only the 15 parameter shifts from previously established values, the most current data points.

impact of the shift on the response of the assay When the U-235 contents of the plates assayed using a instrument should be determined through an appropriate common calibration relationship varies over a ranpg of experiment or. calculation (Ref. 6). A bias correction +/-5% or more about the average of all plate loadings, the should be determined and applied to all items assayed systematic error should be estimated as described in from the point of the parameter change. The uncertainty paragraph 1. below; when plate loadings are tightly in the bias should be combined with the systematic error clustered about a nominal value, the systematic error predicted through the calibration function. When the should be estimated as described in paragraph 2.

bias exceeds 3% of the plate contents in a single material balance period, when a trend of 1.5% or more is 1. At the close of the reporting period, the assay observed in three consecutive material balance periods, value for each plate is plotted against the verified

,)r when the uncertainty in the observed bias is sufficient quantity. The verification data plot is examined for to increase the limit of error of the assay above 0.5%, indications of nonlinearity or obvious outlier data.

new calibration standards should be obtained, and the Anomalous indications should be investigated and scanning system should be recalibrated. remedied.

As a further check on the continued validity of the A linear regression analysis should be performed on calibration standards, a program to periodically intro- the comparison data. The intercept should be tested duce new calibration standards should be implemented. against zero for an indication of a constant measurement bias. The slope shouid be tested against unity for an

  • These methods will be discussed in detail in a regulatory guide indication of a proportional bias. When bias is indicated,

,n preparation entitled "Calibration and Error Estimation assays performed during the preceding operating period Pr:ccduir"s fcr Nondestructi-e Asay." should be compensated. The systematic error should be

5.38-6

estimated as the standard error associated with the 1. Each core compact should carry a unique identifi- verification line. cation. Accountability records should be created for each compact. The fuel plate should carry an identifica-

2. When all plates contain essentially the same U-235 tion corresponding to the compact identification.

content, the difference in the mean content values should be tested against zero as an indication of bias, and the systematic error associated with an inventory of 2. Each fuel plate should be radiographically exam- plates should be quoted as the standard deviation of the ined to ensure that the entire compact has been mean difference. For individual plates, the systematic encapsulated.

error should be quoted as the standard deviation of the difference distribution.

3. Each fuel plate should be checked with a gamma

5. CORE COMPACT ASSAY ray probe to qualitatively ensure that the plate core is uranium of the nominal product enrichment.

Final product assay in high-enrichment fuel plate manufacturing can also be accomplished through assay- ing each core compact following the procedures detailed 4. Calibration and error evaluation should follow the in this guide and the following supplemental criteria: procedures for fuel plate assay.

REFERENCES

I. J.E. Cline, R.J. Gehrke, and L.D. Mclsaac, "Gamma 4. John L. Jaech, "Statistical Methods in Nuclear Rays Emitted by the Fissionable Nuclides and Asso- Materials Control," TID-26298 (1973).

ciated Isotopes," ANCR-1029 (July 1972). 5. American National Standard N15.20, "Guide to

2. N.S. Beyer, "Assay of U-235 in Nuclear Reactor Fuel Calibrating Nondestructive Assay Systems," in Elements by Gamma Ray Scintillation Spec- preparation. Copies of the draft standard may be trometry," Proc. 4th Intl. Conf. on Nondestructive obtained from Institute of Nuclear Materials Manage- Testing, London, 1963. ment, 505 King Avenue, Columbus, Ohio 43201

3. J.H. Hubbell, "Photon Cross Sections, Attenuation (Attention: H.L. Toy).

Coefficients, and Energy Absorption Coefficients 6. See, for example, R.A. Forster, D.B. Smith, and H.O.

from 10 keV to 100 GeV," Nat. Bur. Stds. Menlove, "Error Analysis of a Cf-252 Fuel Rod Assay NSRDS-NBS 29 (1969). System,'" LA-5317 (1974).

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