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{{#Wiki_filter:U.S. ATOMIC ENERGY COMMISSIONREGULATORY GIDIRECTORATE OF REGULATORY STANDARDSREGULATORY GUIDE 5.38NONDESTRUCTIVE ASSAY OF HIGH-ENRICHMENT URANIUMFUEL PLATES BY GAMMA RAY SPECTROMETRYSeptember 1974JIDE
{{#Wiki_filter:U.S. ATOMIC ENERGY COMMISSION
REGULATORY
GI DIRECTORATE
OF REGULATORY  
STANDARDS REGULATORY
GUIDE 5.38 NONDESTRUCTIVE
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 morethan 350 grams of contained U-235 to conduct aphysical inventory of all special nuclear material in hispossession at intervals not to exceed 12 months. Eachlicensee authorized to possess more than one effectivekilogram of high-enrichment uranium is required toconduct measured physical inventories of his specialnuclear materials at bimonthly intervals. Further, theselicensees are required to conduct their nuclear materialphysical inventories in compliance with specific require-ments set forth in Part 70. Inventory proceduresacceptable to the Regulatory +,aff for complying withthesc pi 'wisions of Part 70 are detailed in RegulatoryGuide 5.13. "Conduct of Nuclear Material PhysicalInvcntories."For certain nuclear reactors, the fuel consists ofhighly enriched uranium fabricated into flat or bowedplates. Typically, these plates are relatively thin so that asignificant percentage of the U-235 gamma rays ptle-trate the fuel cladding. When the measurement condi-tions are properly controlled and corrections are madefor variations in the attenuation of the gamma rays, ameasurement of the U-235 gamma rays can be used as anacceptable measurement of the distribution and the totalU-235 content of each fuel plate. In lieu of assaying theproduct fuel plates, fuel plate core compacts may beassayed through the procedures detailed in this guide,provided steps are taken to ensure the traceability andintegrity of encapsulation of each assayed fuel plate corecompact. This guide describes features of a gamma rayspectrometry system acceptable to the Regulatory stafffor nondestructive assay of high-enrichment uraniumfuel plates or fuel plate core compacts.
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.
 
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  
+,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.


==B. DISCUSSION==
==B. DISCUSSION==
The number, energy, and intensity of gamma raysassociated with the decay of U-235 provide the basis fornondestructive assay of high-enrichment fuel plates bygamma ray spectrometry (Ref. 1). The 185.7-keVgamma ray is the most useful U-235 gamma ray for thisapplication; it is emitted at the rate of 4.25 x 104gamma 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 fluctuationsin clad and core thickness. In general, more accurate fuelplate assays may be made by measuring only the activityattributable to the 185.7-keV U-235 gamma ray.Assay measurements are made by integrating theresponse observed during the scanning of single fuelplates and comparing each response to a calibrationbased on the response to known calibration standards.1. GAMMA RAY MEASUREMENT SYSTEM1.1 GAMMA RAY DETECTION SYSTEM1.1.1 Gamma Ray DetectorHigh-resolution gamma ray detectors, i.e., intrinsic orlithium-drifted germanium, provide resolution beyondthat required for this assay application. While theperformance of such detectors is more than adequate,their low intrinsic detection efficiency, extensive opera-tional and maintenance requirements, and high costmake them unattractive for this application.Most ,sodium iodide [Nal (TI)] scintillation detectorsare capable of sufficient energy resolution to be used forthe measurement of the 185.7-keV gamma rays. Thedetector diameter is determined by the fuel plate widthand the scanning method selected (see Section B.I.2 ofthis guide). The thickness of the Nal crystal is selectedto avoid unnecessary sensitivity to gamma rays above the185-keV region which produce a background in the185-keV energy region as a result of Compton scattering.For measurements to be reproducible, it is necessaryto assure that the detection system is stabilized on theUSAEC REGULATORY GUIDES Cop.- of published guids may be obtained by request indicintng the dinirsomdeired 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 fornalhods 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 Secretarythe 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 comNpflaniowith 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 tothe or oiminuenOt of a permit or licnese by the Commtissson. 1. Powr Reectorn 6. Products2. Research and Test Ractors 7. Tranpomrtation3. Fuels isid Materi- Fac;itisi a. O=upetiona! Meeilhguides will be revised periodicafly. as approprate. to accomn oal 4. Environmenetal end Siting 9. Antitrust Reviewcomments and to reflect new ,ntormition or expoerine. 5. Mot'earits and Plant Protection 10. Generaf intended portion of the gamma ray spectrum duringmeasurements. Internally "seeded" Nal crystals whichcontain a radioactive source (typically Am-241) toproduce a reference energy pulse art commerciallyavailable. The detection system is stabilized on thereference, and the amplifier gain is automatically cor-rected to assure that that energy and the rest of thespectrum remain fixed in position..1.2 Gamma Ray CollimatorTo ensure that the only gamma ray activity detectedoriginates from a well-defined segment of the fuel plate,the detector is shielded from extraneous backgroundradiations and collimated to define the area "seen" bythe detector crystal. The collimator consists of a disk ofappropriate shielding material. A slit is machinedthrough the center of the disk which will allow onlythose gamma rays emitted within the slit opening tostrike the detector. The disk thickness is a minimum ofsix mean free path lengths to effectively stop all gammarays emitted from outside the view area. To preventgamma rays from striking the crystal around the edges ofthe collimator disk, the disk diameter exceeds the crystaldiameter by at least twice the crystal depth.The probability of detection for gamma rays emittedat the center of the collimator slit is greater than that forgamma rays emitted near the ends of the slit. This effectbecomes increasingly important at small detector-to-plate spacing, especially when scanning near the edge ofa plate. To minimize this detection nonuniformity andto minimize the sensitivity to jitter, the detector-to-platedistance can be made large, especially with respect to thedimensions of the slit opening. As an alternative meansof reducing the detection nonuniformity-across the slit,the slit opening can be divided into channels by insertinga honeycomb baffle into the slit or by fabricating thecollimator by drilling holes through the disk in a patternwhich ensures that each hole is surrounded by aminimum wall thickness of 0.2 mean free path length. A7:0-cm-thick iron disk with holes less than 0.5 cm indiameter drilled in a pattern having 0.2 cm of wallbetween adjacent holes is one example of a collimatorthat would perform satisfactorily. A large number ofsmall-diameter holes is preferable to a few large-diameterholes.1.1.3 Multiple DetectorsSeveral detectors may be used to shorten the mea-surement time. The detectors can be positioned tosimultaneously measure different segments of a singlefuel plate or to simultaneously measure additional fuelplates. In some cases it may be useful to sum theresponse from two detectors positioned on oppositesides of a plate to increase counting efficiency. In suchcases it is essential that the response of such detectors bebalanced-and checked at frequent intervals.1.2 SCANNING TECIINIQUESIt 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 heldstationary, or the plate can be moved past a fixeddetector. Care must be exercised to maintain fldetector-to-plate spacing within close tolerance,minimize errors caused by the inverse-square dcpen(!of detection on distance. This is especially important inthe case of close spacing, which is sometimes desirable tomaximize the count rate. Various commercial conveyingsystems have been used and found to be adequate. Such.systems may significantly reduce the cost of de..,7!i, gand building new scanning mechanisms. High-precisiontool equipment such as milling machines, lathes, and x-yscanning tables can be investigated. Numerically con-trolled units offer additional advantages when they canbe incorporated into a scanning system. This is particu-larly true when an automated scanning system is beingdeveloped.Fuel plate core compacts may be sufficiently smallpermit total assay without scanning in a fixed-geometrycounting system. The scanning techniques for fuel platesdiscussed in the following subsections can also be usedfor core compacts when total fixed compact counting isnot possible.1.2.1 Linear Total ScanThe detector collimation consists of a rectangularopening which extends across the width of the fuelplates beyond the edges of the uranium core containedwithin the plate cladding. Scanning the total plate isaccomplished by starting the count sequence on the endof a -plate and continuing to count until the entire lengthof plate has been scanned.To ensure that gamma rays emitted anywhere acrossthe face of the fuel plate have an equal probability ofbeing detected, it is necesary that the diameter of thedetector crystal exceed the plate width or that thedetector be positioned away from the plate.Use of the spot oi cizcalar collimator scan techniqueeliminates or reduces to insignificance most of theseedge effects.1.2.2 Sweeping Spot Scan (Ref. 2)If the collimator channel width is smaller than thefuel plate width, the viewing area (spot) can be sweptacross the plate as the detector scans along the length ofthe plate. This scanning technique can be readilyadapted to scanning bowed plates through the use of acam which is designed to maintain the detector-to-platedistance constant over the entire geometry of the fuelplate. The collimator channel dimensions can be selectedto provide compatible information on the uniformity of5.38-2 the fuel plate which is frequently obtained by comparingfixed (static) spot counts at a variety of locations toreference counts.1.2.3 Sampled Increment AssayWhen used in conjunction with radiographic dimen-sional measurements performed on all fuel plates, theU-235 content of a fuel plate can be measured byscanning the ends of each fuel plate and sampling thebalance of the plate. It is necessary to measure thedimensions of the fuel core loading radiographically,through gamma ray scanning along the length of theplate, or by spot scanning the fuel plate ends andmeasuring the distance between end spots where the fuelloading stops. The U-235 content of the plate is thendetermined by averaging the results of sample spotmeasurements of the U-235 content per unit area at anumber of sites along the plate and multiplying thisaverage value by the measured area of the fuel core. Theradiograph of each plate is examined to ensure that thecore filter is uniform.The collimator shape and dimensions can be selectedto provide compatible information on the uniformity ofthe fuel plate.1.3 COMPUTER CONTROLThe reproducibility of measurements can be im-proved and the measurement time per fuel plate can bereduced by using a computer to control the fuel platescanning operation. The computer can be used tocontrol data acquisition by accumulating counts ac-cording to a predetermined scheme. Also, the computercan be used for data analysis, including backgroundcorrections and intermachine normalization, calibration,error analysis, and diagnostic test measurements andanalyses. Report preparation and data recording forsubsequent analysis are also readily accomplishedthrough an appropriately designed computer-controlledsystem.2. INTERPRETATION OF MEASUREMENT DATAThe three factors discussed below may give rise tosignificant errors in interpreting measurement data.2.1 ENRICHMENT vARIATIONSLicensees authorized to possess highly enricheduranium are required to account for element and isotopeas prescribed in §70.51. Under the conditions detailedin this guide, the U-235 content of individual plates ismeasured. To determine the total uranium content ofeach plate, the U-235 enrichment must be known fromseparate measurements.Enrichment variations may alter the radiation back-ground in the gamma ray energy region of interest.Uranium-238 decays by alpha-particle .emission toTh-234. Thorium-234 then decays by beta-particle emis-sion with a half-life of 24.1 days to Pa-234 which, inturn, decays by beta-particle emission to U-234. Ap-proximately 1% of the Pa-234 decays are followed byhigh-energy (e.g., 1001 keV, 766 keV) gamma rays.These gamma rays frequently lose energy throughCompton scattering and may appear in the 185-keVspectral region. It is important to note that activity fromPa-234 may be altered by disturbing the equilibriumbetween U-235 and Th-234, as frequently occurs inuranium chemical conversion processes. The interferencedue to variations in U-238 daughter activity becomes lessimportant as the enrichment of U-235 increases. Atenrichment levels above 90%, this problem can essen-tially be ignored.2.2 RADIATION ATTENUATIONThe number of U-235 gamma rays which escape fromthe fuel plate (and are thus available for detection)without losing energy depends on the characteristics ofthe fuel plate core and cladding. Gamma rays fromU-235 are attenuated in the uranium, in the cladding,and in the inert material that may be added with theuranium to form the core of the fuel plate. Throughwell-controlled product tolerance limits, each of thesepotential sources of signal variability can be controlledto permit accurate accountability assays.2.2.1 Self-AttenuationThe uranium photon attenuation coefficient forgamma ray energies corresponding to U-235 emissions isquite large (Ref. 3). Small changes in uranium densityresulting from increased fuel loading or from variationsin the manufacturing process can significantly changethe number of gamma rays which escape from the fuelplate.2.2.2 Gadding AttentuationSmall variations in cladding thickness may causesignificant attenuation variations. Variations in claddingattenuation can be measured by a simple gamma rayabsorption test using thin sheets of cladding material asabsorbers and varying the clad thickness over the rangeof thicknesses to be encountered in normal productvariability.2.2.3 Core Friler AttenuationRadiation intensity measurements may be made ofplates fabricated with different ratios of uranium tofiller to show the effects of this type of attenuation. Ifsignificant effects are noted, plates can be categorized bycore composition characteristics and the assay systemcan be independently calibrated for each category offuel plates.5.38-3  
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;  
2.2.4 Attenuation CorrectionsWhen the thickness of the core and cladding of eachplate is known, an attenuation correction can be appliedto improve the accuracy of the assay. Ultrasonic gaugingmay provide such a measure, provided the metallo-graphic zones within the plate are sufficiently defined toprovide a detectable interface.The alternative attenuation- correction is based on amicrometer measurement of the total thickness of eachplate. The clad thickness of a plate is estimated bysubtracting the mean core thickness of the productplates, which is determined by periodically samplingproduct plates and cutting a cross section to permitvisual measurement of clad and core thickness.2.3 INTERFERING RADIATIONSAs noted in Section B.2.1 of this guide, an internalbackground variation may arise from changes in theamount of U.238 present in a fuel plate or from changesin the ratio of Th-234 to U-238 resulting from fuelmanufacturing processes. Fluctuations in the internalbackground cause the response of the unknown items tobe different from the calibration standards, therebycreating a measurement bias. Such interferences can becompensated by measuring additional regions of thegamma ray spectrum.Other interfering radiations may come from externalsources, from fuel plates awaiting assay, or from nearbyradiation sources used for other measurements. This isnot expected to be a major problem and can becontrolled through (1) removing radiation sources,(2) shielding the detectors, and (3) monitoring the back-ground at frequent intervals.3. CALIBRATION AND VERIFICATION3.1 INITIAL OPERATIONSCalibration and the verification of assay predictions isan ongoing effort where performance is periodicallymonitored and the calibration relationship is modified toimprove the accuracy of assay predictions. During initialoperations, two means of basing preliminary calibrationsare appropriate.3.1.1 Foil Calibration TechniqueMethods for calibrating scanning systems for high-enrichment uranium fuel plates through the assay ofprepared uranium and clad foils are described in Refer-ence 2. This method may be used in place of or inaddition to the -technique described in the followingsubsection.uranium, U-235, inert matrix, and cladding are accu-rately measured and that these parameters bracket thenominal range of product plates anticipated to fallwithin manufacturing tolerances.3.2 ROUTINE OPERATIONSThe performance of the assay system is periodicallymonitored to ensure that the performance of the assaysystem has not shifted since its last calibration. Controllimits for acceptable performance can be established forthe response to an appropriate working standard. Thecontrol chart of the responses to the working standardcan be checked for indications of short-term instrumentdrift or malfunction. The control chart can also beanalyzed to detect long-term shifts within themeasurement-to-measurement control limits that may becorrected by recalibrating the system. Severe changes ininstrument performance are investigated promptly andtheir causes remedied.To ensure that the calibration remains valid duringnormal operations and that accuracy estimates arerigorously justified, assay predictions are periodicallycompared with more accurate measurements of thecontent of typical fuel plates (see Section C.4 of thisguide). Guidance on methods to relate this assay to thenational measurement system and to reconcile verifi-cation measurements will be addressed in separateregulatory guides.*
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  
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  
SYSTEM 1.1 GAMMA RAY DETECTION  
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.
 
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.
 
Most ,sodium iodide [Nal (TI)] scintillation detectors are capable of sufficient energy resolution to be used for the measurement of the 185.7-keV  
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  
GUIDES Cop.- of published guids may be obtained by request indicintng the dinirsom deired to the US. Atomic Erw Commismson.
 
Vlhington.
 
D.C. 2054
 
===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===
3. Fuels isid Materi- Fac;itisi a. O=upetiona!  
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.
 
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.
 
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  
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.
 
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.
 
2.3 INTERFERING  
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.
 
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.
 
===3. CALIBRATION ===
AND VERIFICATION
3.1 INITIAL OPERATIONS
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.
 
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.
 
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.
 
3.2 ROUTINE OPERATIONS
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.
 
Control limits for acceptable performance can be established for the response to an appropriate working standard.
 
The control chart of the responses to the working standard can be checked for indications of short-term instrument drift or malfunction.
 
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
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.
 
The factors presented below should be taken into consideration for this assay method to be acceptable to the Regulatory staff.I. MEASUREMENT
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.
 
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.
 
The seed should produce approximately
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.
 
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.
 
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.
 
All electronic circuitry in signal-processing components should feature temperature compensation.
 
Residual sen-sitivity to fluctuations in the, ambient environment should be tested and monitored periodically.
 
The capability for multichannel gamma ray pulse height analysis with cathode ray tube spectral display should be provided.
 
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.
 
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.
 
===2. MEASUREMENT ===
INTERPRETATION
2.1 ENRICHMENT
VARIATIONS
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.*
Facilities processing more than one uranium enrichment should maintain strict isotopic control and characterize the enrichment through appri.,-priate measurement methods.2.2 ATTENUATION
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
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.
 
Bick-ground radiation should be measured periodically during each operating shift.
 
===3. MEASUREMENT ===
CALIBRATION
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
ASSAY ERRORS 4.1 RANDOM ERROR ESTIMATION
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.
 
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.
 
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.
 
As a further check on the continued validity of the calibration standards, a program to periodically intro-duce new calibration standards should be implemented.
 
*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.
 
The selected fuel plates may be rejected from the process stream for failing to meet quality assurance requirements.
 
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.
 
Following this initial implementation period, facilities manufacturing
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
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.
 
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.
 
For individual plates, the systematic error should be quoted as the standard deviation of the difference distribution.
 
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.
 
2. Each fuel plate should be radiographically exam-ined to ensure that the entire compact has been encapsulated.
 
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.
 
4. Calibration and error evaluation should follow the procedures for fuel plate assa
 
====y. 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
29 (1969).4. John L. Jaech, "Statistical Methods in Nuclear Materials Control," TID-26298
(1973).5. American National Standard N15.20, "Guide to Calibrating Nondestructive Assay Systems," in preparation.


==C. REGULATORY POSITION==
Copies of the draft standard may be obtained from Institute of Nuclear Materials Manage-ment, 505 King Avenue, Columbus, Ohio 43201 (Attention:  
The content and distribution of U-235 in high-enrichment uranium plates can be measured through thegamma ray assay methods described in this guide.Combining this measurement with the results of anindependent measurement of the U-235 enrichmentenables the total uranium content of the fuel plates tobe measured. The factors presented below should betaken into consideration for this assay method to beacceptable to the Regulatory staff.I. MEASUREMENT SYSTEM1.1 GAMMA RAY MEASUREMENT SYSTEM1.1.1 Gamma Ray DetectorA thallium-activated sodium iodide scintillationdetector or series of detectors is recommended for thisassay application. When more than one detector is to beincorporated into the scan system, the performancecharacteristics of the detectors should be matched. Thediameter of the crystal should be larger than theprojected view onto the crystal face through the*For example, regulatory guides related to measurement qualityamurance and calibration of nondestructive a&say systems arebeing developed.3.1.2 Fabricated Calibration PlatesCalibration standard fuel plates can be fabricatedusing special precautions to ensure that the amounts of5.38-4 collimator channel. The thickness of the crystal shouldhc noi more than onc inch. The crystal should contain aninternal cesium iodide seed which is doped with asuilable alpha-emittcr for spectral stabilization. The seedshould produce approximately 1,000 counts per secondat the reference energy.1.1.2 CollimatorA collimator should be fabricated of appropriategamma ray shielding material such as iron, lead, ortungsten. The shielding should completely surround thedetector and photomultiplier assembly and should besufficiently thick to completely block extraneous radi-ations from the detector. The response variation fromthe center of the collimator opening to its edge shouldbe less than 1%.1.1.3 Electronic ApparatusAll electronic systems should be powered by filtered,highly regulated power supplies. The ambient tempera-ture and humidity in the vicinity of the scanning systemshould be controlled so that permitted fluctuations donot significantly affect the assay measurements. Allelectronic circuitry in signal-processing componentsshould feature temperature compensation. Residual sen-sitivity to fluctuations in the, ambient environmentshould be tested and monitored periodically.The capability for multichannel gamma ray pulseheight analysis with cathode ray tube spectral displayshould be provided. Signal-processing electronics capableof stabilizing on the alpha radiations emitted within thedoped cesium iodide seed should be provided to stabilizethe energy spectrum.1.2 SCANNING SYSTEMA mechanically sound, highly reproducible scanningsystem should be employed. Scanning should be accom-plished by one of the three techniques discussed inSection B. 1.2 of this guide.1.3 COMPUTER CONTROLA dedicated minicomputer to control data acquisi-tion, analysis, calibration, diagnostic testing, and reportpreparation -should be employed for this assay appli-cation.1.4 MULTIPLE SCANNING ASSAY SYSTEMSWhen more than ornc scanning system is employed,assay response should be normalized so that eachinstrument provides consistent results. Verification datato establish the systeniatic assay error for each assaysystem should be obtained with the same plate.2. MEASUREMENT INTERPRETATION2.1 ENRICHMENT VARIATIONSProcedures should be developed to ensure that theenrichment of the plates being scanned is knownthrough separate measurements. Fuel plates generallysatisfy the gamma ray penetrability criteria for quantita-tive U-235 assay; they do not satisfy the criteria fornondestructive enrichment measurement through gammaray spectrometry.* Facilities processing more than oneuranium enrichment should maintain strict isotopiccontrol and characterize the enrichment through appri.,-priate measurement methods.2.2 ATTENUATION CORRECTIONSAttenuation variations arising from plate-to-platechanges in core thickness, composition,-and clad thick-ness should be determined over the range of producttolerance specifications. When such variations cause theassay error to exceed the error realized without thevariations by 50% or more, procedures should beimplemented to measure and apply a correction to theassay of each plate.2.3 RADIATION INTERFERENCESA clear plastic template which shows an acceptablespectrum display should be prepared. When radioactiveinterference may be encountered, the assay spectrumshould be compared at appropriate intervals to thereference spectrum for indications of interference. Bick-ground radiation should be measured periodically duringeach operating shift.3. MEASUREMENT CALIBRATIONDuring initial operations, the assay system should m,calibrated either by the foil calibration method or withspecially prepared sample fuel plates as described mnSection B.3.1 of this guide.4. RANDOM AND SYSTEMATIC ASSAY ERRORS4.1 RANDOM ERROR ESTIMATIONA replicate assay program should be established togenerate data for the evaluation of random assay errOrsduring each material balance period. During each bi-monthly interval, a minimum of fifteen plates should beselected for replicate assay. The second assay of eachplate selected for replicate assay should be made at leastfour 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 arffgiven in Regulatory Guide 5.21, "Nondestructrvr ltiranwurn.235Enrichment Assay by Gamma Ray "5.38-5 material balance period. The single-measurement stan-dard deviation of the relative replicate assay differencesshould be computed as described in Reference 4.4.2 SYSTEMATIC ERROR ESTIMATIONThe systematic error associated with the assay of allfuel plates fabricated during a material balance periodshould be determined through one of the procedures*presented below.4.2.1 Propagation through the Calibration FunctionTo estimate the systematic assay error through thecalibration function, the calibration should be based onthe regression analysis of an appropriate function to thecalibration data. Uncertainties in the reference values ofthe calibration standards should be factored into the fit,and the errors propagated as demonstrated in Reference5.To ensure the validity of the predictions, the stableperformance of the instrument should be monitored andnormalized through the response to appropriate workingstandards which are assayed at frequent intervals. Thefrequency for assaying working standards should bedetermined through testing, but should not be lowerthan one test during each two-hour assay interval forspot response stability and one full scan test during eachoperating shift. Indications of shifting instrument perfor-mance should be investigated and remedied, and theinstrument should be recalibrated to ensure the validityof subsequent measurements.In order to ensure that the calibration standardscontinue to adequately represent the unknown fuelplates, key production parameters which affect theobserved response should be monitored through separatetests. Data should be compiled and analyzed at the closeof each material balance period. When a productionparameter shifts from previously established values, theimpact of the shift on the response of the assayinstrument should be determined through an appropriateexperiment or. calculation (Ref. 6). A bias correctionshould be determined and applied to all items assayedfrom the point of the parameter change. The uncertaintyin the bias should be combined with the systematic errorpredicted through the calibration function. When thebias exceeds 3% of the plate contents in a single materialbalance period, when a trend of 1.5% or more isobserved in three consecutive material balance periods,,)r when the uncertainty in the observed bias is sufficientto increase the limit of error of the assay above 0.5%,new calibration standards should be obtained, and thescanning system should be recalibrated.As a further check on the continued validity of thecalibration standards, a program to periodically intro-duce new calibration standards should be implemented.*These methods will be discussed in detail in a regulatory guide,n preparation entitled "Calibration and Error EstimationPr:ccduir"s fcr Nondestructi-e Asay."A minimum of one new calibration standard fuel plateshould be introduced during each six-month period.4.2.2 Comparative EvaluationWhen two measurements are made on each of a seriesof items and the accuracy of ono of the methods used isconsiderably greater than the other, the correspondingpredictions can be compared to establish an estimate ofbias between the measurement methods and to estimatethe error. associated with the lens-accurate measurementmethod. To precisely determine the systematic error inthe nondestructive assay, the fuel plates selected forcomparative measurements should be randomly selectedbut should span the range of U-235 contents en-countered in normal production. The selected fuel platesmay be rejected from the process stream for failing tomeet quality assurance requirements. Each plate shouldbe repeatedly assayed to reduce the random asay errorto less than 10% of the estimated or previouslyestablished systematic error. To determine its U-235 andtotal uranium content, the plate should be completelydissolved and the resulting solution should be analyzedby high-accuracy chemical and mass spectrometric pro-cedures.For one material balance period during the initialimplementation of this guide; a product fuel plateshould be randomly selected twice each week for anaccuracy verification measurement. Following this initialimplementation period, facilities manufacturing 100 ormore fuel plates per week may reduce the verificationfrequency to one plate per week and pool the verifi-cation data for two consecutive material balance periods.LoW-throughput facilities manufacturing lesa than 100plates per week should verify at least 4 plates permaterial balance period through the procedures de-scribed above. At the close of each material balanceperiod, data should be pooled to include only the 15most current data points.When the U-235 contents of the plates assayed using acommon calibration relationship varies over a ranpg of+/-5% or more about the average of all plate loadings, thesystematic error should be estimated as described inparagraph 1. below; when plate loadings are tightlyclustered about a nominal value, the systematic errorshould be estimated as described in paragraph 2.1. At the close of the reporting period, the assayvalue for each plate is plotted against the verifiedquantity. The verification data plot is examined forindications of nonlinearity or obvious outlier data.Anomalous indications should be investigated andremedied.A linear regression analysis should be performed onthe comparison data. The intercept should be testedagainst zero for an indication of a constant measurementbias. The slope shouid be tested against unity for anindication of a proportional bias. When bias is indicated,assays performed during the preceding operating periodshould be compensated. The systematic error should be5.38-6 estimated as the standard error associated with theverification line.2. When all plates contain essentially the same U-235content, the difference in the mean content valuesshould be tested against zero as an indication of bias,and the systematic error associated with an inventory ofplates should be quoted as the standard deviation of themean difference. For individual plates, the systematicerror should be quoted as the standard deviation of thedifference distribution.5. CORE COMPACT ASSAYFinal product assay in high-enrichment fuel platemanufacturing can also be accomplished through assay-ing each core compact following the procedures detailedin this guide and the following supplemental criteria:1. Each core compact should carry a unique identifi-cation. Accountability records should be created foreach compact. The fuel plate should carry an identifica-tion corresponding to the compact identification.2. Each fuel plate should be radiographically exam-ined to ensure that the entire compact has beenencapsulated.3. Each fuel plate should be checked with a gammaray probe to qualitatively ensure that the plate core isuranium of the nominal product enrichment.4. Calibration and error evaluation should follow theprocedures for fuel plate assay.REFERENCESI. J.E. Cline, R.J. Gehrke, and L.D. Mclsaac, "GammaRays Emitted by the Fissionable Nuclides and Asso-ciated Isotopes," ANCR-1029 (July 1972).2. N.S. Beyer, "Assay of U-235 in Nuclear Reactor FuelElements by Gamma Ray Scintillation Spec-trometry," Proc. 4th Intl. Conf. on NondestructiveTesting, London, 1963.3. J.H. Hubbell, "Photon Cross Sections, AttenuationCoefficients, and Energy Absorption Coefficientsfrom 10 keV to 100 GeV," Nat. Bur. Stds.NSRDS-NBS 29 (1969).4. John L. Jaech, "Statistical Methods in NuclearMaterials Control," TID-26298 (1973).5. American National Standard N15.20, "Guide toCalibrating Nondestructive Assay Systems," inpreparation. Copies of the draft standard may beobtained from Institute of Nuclear Materials Manage-ment, 505 King Avenue, Columbus, Ohio 43201(Attention: 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 AssaySystem,'" LA-5317 (1974).5.38-7  
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}}
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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)


U.S. ATOMIC ENERGY COMMISSION

REGULATORY

GI DIRECTORATE

OF REGULATORY

STANDARDS REGULATORY

GUIDE 5.38 NONDESTRUCTIVE

ASSAY OF HIGH-ENRICHMENT

URANIUM FUEL PLATES BY GAMMA RAY SPECTROMETRY

September

1974 JIDE

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.

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

+,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.

B. DISCUSSION

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

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

SYSTEM 1.1 GAMMA RAY DETECTION

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.

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.

Most ,sodium iodide [Nal (TI)] scintillation detectors are capable of sufficient energy resolution to be used for the measurement of the 185.7-keV

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

GUIDES Cop.- of published guids may be obtained by request indicintng the dinirsom deired to the US. Atomic Erw Commismson.

Vlhington.

D.C. 2054

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

3. Fuels isid Materi- Fac;itisi a. O=upetiona!

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.

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.

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

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.

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.

2.3 INTERFERING

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.

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.

3. CALIBRATION

AND VERIFICATION

3.1 INITIAL OPERATIONS

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.

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.

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.

3.2 ROUTINE OPERATIONS

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.

Control limits for acceptable performance can be established for the response to an appropriate working standard.

The control chart of the responses to the working standard can be checked for indications of short-term instrument drift or malfunction.

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

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.

The factors presented below should be taken into consideration for this assay method to be acceptable to the Regulatory staff.I. MEASUREMENT

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.

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.

The seed should produce approximately

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.

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.

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.

All electronic circuitry in signal-processing components should feature temperature compensation.

Residual sen-sitivity to fluctuations in the, ambient environment should be tested and monitored periodically.

The capability for multichannel gamma ray pulse height analysis with cathode ray tube spectral display should be provided.

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.

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.

2. MEASUREMENT

INTERPRETATION

2.1 ENRICHMENT

VARIATIONS

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.*

Facilities processing more than one uranium enrichment should maintain strict isotopic control and characterize the enrichment through appri.,-priate measurement methods.2.2 ATTENUATION

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

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.

Bick-ground radiation should be measured periodically during each operating shift.

3. MEASUREMENT

CALIBRATION

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

ASSAY ERRORS 4.1 RANDOM ERROR ESTIMATION

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.

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.

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.

As a further check on the continued validity of the calibration standards, a program to periodically intro-duce new calibration standards should be implemented.

  • 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.

The selected fuel plates may be rejected from the process stream for failing to meet quality assurance requirements.

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.

Following this initial implementation period, facilities manufacturing

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

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.

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.

For individual plates, the systematic error should be quoted as the standard deviation of the difference distribution.

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.

2. Each fuel plate should be radiographically exam-ined to ensure that the entire compact has been encapsulated.

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.

4. Calibration and error evaluation should follow the procedures for fuel plate assa

y. 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

29 (1969).4. John L. Jaech, "Statistical Methods in Nuclear Materials Control," TID-26298

(1973).5. American National Standard N15.20, "Guide to Calibrating Nondestructive Assay Systems," in preparation.

Copies of the draft standard may be obtained from Institute of Nuclear Materials Manage-ment, 505 King Avenue, Columbus, Ohio 43201 (Attention:

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