Regulatory Guide 5.53: Difference between revisions

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{{Adams
{{Adams
| number = ML003739240
| number = ML13064A081
| issue date = 02/29/1984
| issue date = 02/28/1984
| title = Qualification,Calibration & Error Estimation Methods for Nondestructive Assay
| title = Qualification, Calibration, and Error Estimation Methods for Nondestrutive Assay
| author name =  
| author name =  
| author affiliation = NRC/RES
| author affiliation = NRC/RES
Line 10: Line 10:
| license number =  
| license number =  
| contact person =  
| contact person =  
| document report number = RG-5.53 Rev 1
| document report number = RG-5.053, Rev. 1
| document type = Regulatory Guide
| document type = Regulatory Guide
| page count = 10
| page count = 10
}}
}}
{{#Wiki_filter:Revision 1*
{{#Wiki_filter:Revision 1*
                                                                                                                              February 1984 U.S. NUCLEAR REGULATORY COMMISSION
February 1984 U.S. NUCLEAR REGULATORY COMMISSION
                        REGULATORY GUIDE
REGULATORY GUIDE
                        OFFICE OF NUCLEAR REGULATORY RESEARCH
OFFICE OF NUCLEAR REGULATORY RESEARCH
                                                      REGULATORY GUIDE 5.53 (Task SG 049-4)
REGULATORY GUIDE 5.53 (Task SG 049-4)
                            QUALIFICATION, CALIBRATION, AND ERROR ESTIMATION
QUALIFICATION, CALIBRATION, AND ERROR ESTIMATION
                                          METHODS FOR NONDESTRUCTIVE ASSAY
METHODS FOR NONDESTRUCTIVE ASSAY


==A. INTRODUCTION==
==A. INTRODUCTION==
Section70.58, "Fundamental Nuclear Material Con- trols," of 10 CFR Part 70, "Domestic Licensing of Special Nuclear Material," requires certain licensees to establish a measurement quality assurance program for material control and accounting. Specifically, paragraph 70.58(f)
requires that a program be established, maintained, and followed for the maintenance of acceptable measurement quality in terms of measurement bias and for the evalua- tion and control of the quality of the measurement system.
Nondestructive assay (NDA)
constitutes a unique measurement technology. When applied under appropriate rigorous controls, it can enhance the ability of the material control and accounting system to detect unaccounted-for loss or diversion of special nuclear material (SNM) to unauthorized uses. This guide describes methods and procedures acceptable to the NRC staff for meeting the provisions of paragraph 70.58(f) of 10 CFR Part 70 as it relates to the use of nondestructive assay.
Any guidance in this document related to information collection activities has been cleared under 0MB Clearance No. 3150-0009.
==B. DISCUSSION==
Nondestructive assay has been applied to virtually every chemical or physical form of special nuclear material encountered in contemporary reactor fuel processing.
Special considerations are required to achieve high- accuracy assay results and to properly estimate the errors associated with NDA applications.
Recognizing these considerations, the American National Standards Institute has developed a standard, ANSI N15.20-1975, "Guide to Calibrating Nondestructive Assay Systems."1 This standard
1Copies may be obtained from the American National Standards Institute, 1430 Broadway, New York, New York 10018.
was reviewed and reaffirmed without modification in
was reviewed and reaffirmed without modification in
                                                                        1980. This guide endorses the entire standard as supple Section 70.58, "Fundamental Nuclear Material Con                  mented in the regulatory position.
1980. This guide endorses the entire standard as supple- mented in the regulatory position.
 
==C. REGULATORY POSITION==
The methods, procedures, and guidance relating to the application of NDA in ANSI N1S.20-1975, "Guide to Calibrating Nondestructive Assay Systems," are accept- able to the NRC staff for use in material protection programs as supplemented by the following.
 
===1. METHOD SELECTION===
Prior to selecting an assay method, a study should be made to determine the required performance for that appli- cation. The specific NDA method should be selected to provide results that are compatible with plant material balance requirements.
 
Methods to enhance attainable performance should be considered (e.g., container selec- tion and packaging procedures for bulk materials discussed in Regulatory Guide 5.11,
"Nondestructive Assay of Special Nuclear Material Contained in Scrap and Waste" 2 ).
2. INSTRUMENT SPECIFICATIONS
An evaluation of each new NDA application, including the proposed placement of the instrument, should be conducted prior to procurement. Studies of existing NDA
applications should be conducted periodically to evaluate their performance and substantiate the basis for their continued use. The impact of each of the measurement-to- measurement sources of error encountered in practice or anticipated should be established as a part of each of these efforts.
 
The substantial number of changes in this revision has made it impractical to indicate the changes with lines in the margin.
 
2A proposed revision to this guide has been issued for comment as Task SG 043-4.
 
USNRC REGULATORY GUIDES
Regulatory Guides are issued to describe and make available to the public methods acceptable to the N RC staff of implementing specific parts of the Commission's regulations to delineate tech- niques used by the staff in evaluating specific 'problems or postu- lated accidents or to provide guidance to applicants. Regulatory Guides are no* substitutes for regulations, and compliance with them is not required. Methods and solutions different from those set out in the guides will be acceptable if they provide a basis for the findings requisite, to the issuance or continuance of a permit or license by the Commission.
 
This guide was issued after consideration of comments received from the public. Comments and suggestions for improvements in these guides are encouraged at all times, and guides will be revised, as appropriate, to accommodate comments and to reflect new informa- tion or exoerience.
 
Comments should be sent to the Secretary of the Commission, U.S. Nuclear Regulatory Commission, Washington, D.C. 20555, Attention: Docketing and Service Branch.
 
The guides are issued in the following ten broad divisions:
 
===1. Power Reactors ===
 
===6. Products===
2. Research and Test Reactors
 
===7. Transportation===
3. Fuels and Materials Facilities
 
===8. Occupational Health===
4. Environmental and Siting
9. Antitrust and Financial Review
5. Materials and Plant Protection 10. General Copies of issued guides may be purchased at the current Government Printing Office price. A subscription service for future guides in spe- cific divisions is available through the Government Printing Office.
 
Information on the subscription service and current GPO prices may be obtained by writing the U.S. Nuclear Regulatory Commission, Washington, D.C. 20555, Attention: Publications Sales Manager.
 
A decision should be made to reduce each potentially significant source of error through (1) appropriate instrument design considerations, (2) operational controls, or (3) supple- mentary measurements made to establish bias corrections (see also Reference 1). Instrument procurement specifica- tions and operational instructions should be developed and followed to reflect each error-reduction decision.
 
To minimize operator-related errors and to promote uni- farm measurement practices, NDA instruments used for fixed- station operations should be automated to control (1) data acquisition and analysis, (2) diagnostic testing of instrument performance stability and calibration validity, and (3) calcu- lation of associated error estimates. It is recognized that, for some less complicated NDA measurements, consistency of operation may be achieved through the implementation of carefully written and tested standard operating procedures.
 
Instruments should be tested to ensure that they meet procurement specifications prior to calibration.
 
===3. OPERATORS===
Adequate operator qualification requirements are crucial to proper calibration and effective measurement control of an NDA instrument. The qualification require- ments should include a general knowledge of the assay technique being used and an understanding of the typical behavior and the limitations of the instrument and the technique. A knowledge of the external factors to which the measurement technique is sensitive (factors such as matrix composition, background, material forms, and container type) is also necessary. Only then can proper standards be chosen for calibration and measurement control data be interpreted effectively.


trols," of 10 CFR Part 70, "Domestic Licensing of Special
If the operators have only a general knowledge of external factors, the NDA measurement program must be overseen by a director with a detailed knowledge of all related factors. Only qualified operators should be permit- ted to make SNM assays.


==C. REGULATORY POSITION==
===4. STABILITY TESTING===
Nuclear Material," requires certain licensees to establish a measurement quality assurance program for material The methods, procedures, and guidance relating to the control and accounting. Specifically, paragraph 70.58(f)
A preventive maintenance program should be devised and implemented to ensure the long-term stability and reliability of each instrument.
requires that a program be established, maintained, and                application of NDA in ANSI N15.20-1975, "Guide to followed for the maintenance of acceptable measurement                  Calibrating Nondestructive Assay Systems," are accept quality in terms of measurement bias and for the evalua                able to the NRC staff for use in material protection tion and control of the quality of the measurement                      programs as supplemented by the following.


system.
As part of an ongoing program of measurement control, more working standards 3 should be fabricated to period-
3Working standards are used to check the performance of an NDA instrument. They should be nominally representative of the items to be assayed. They should be fabricated and handled to ensure their internal integrity so that deviations in the measured response of the assay system can be attributed to the instrument.


===1. METHOD SELECTION===
As stated in ANSI Ni5.20-1975, working standards built to meet these requirements are not acceptable as calibration standards.
    Nondestructive assay (NDA) constitutes a unique measurement technology. When applied under appropriate                      Prior to selecting an assay method, a study should be rigorous controls, it can enhance the ability of the material          made to determine the required performance for that appli control and accounting system to detect unaccounted-for                cation. The specific NDA method should be selected to loss or diversion of special nuclear material (SNM) to                  provide results that are compatible with plant material unauthorized uses. This guide describes methods and                    balance requirements. Methods to enhance attainable procedures acceptable to the NRC staff for meeting the                  performance should be considered (e.g., container selec provisions of paragraph 70.58(f) of 10 CFR Part 70 as it                tion and packaging procedures for bulk materials discussed relates to the use of nondestructive assay.                            in Regulatory Guide 5.11, "Nondestructive Assay of
                                                                                                                                            2 Special Nuclear Material Contained in Scrap and Waste" ).
    Any guidance in this document related to information
                                                                        2. INSTRUMENT SPECIFICATIONS
collection activities has been cleared under 0MB Clearance No. 3150-0009.


An evaluation of each new NDA application, including
Calibration standards are defined in ANSI N15.20-1975 as "physically and chemically similar to the items to be assayed, for which the mass of the nuclide(s) of interest and all properties to which the measurement technique is sensitive are known." Calibration standards can be used as working standards, but working standards cannot be used as calibration standards. When calibration standards meet thle requirements for working standards, licensees may elect to maintain only calibration standards. However, calibration standards may deteriorate through extensive use or may be prohibitively expensive for stability monitoring purposes.


==B. DISCUSSION==
ically test the performance stability of the instrument.
the proposed placement of the instrument, should be conducted prior to procurement. Studies of existing NDA
      Nondestructive assay has been applied to virtually                applications should be conducted periodically to evaluate every chemical or physical form of special nuclear material            their performance and substantiate the basis for their encountered in contemporary reactor fuel processing.                    continued use. The impact of each of the measurement-to Special considerations are required to achieve high                    measurement sources of error encountered in practice accuracy assay results and to properly estimate the errors            or anticipated should be established as a part of each of associated with NDA applications. Recognizing these                    these efforts.


considerations, the American National Standards Institute has developed a standard, ANSI N15.20-1975, "Guide to Calibrating Nondestructive Assay Systems."' This standard                    The substantial number of changes in this revision has made it impractical to indicate the changes with lines in the margin.
Each working standard should contain a different amount of the species of SNM to be assayed. Current licensing review criteria require the use of four working standards.


2
On a rotating basis, one or two of these standards are used to check the system each day.
      1                                                                        A proposed revision to this guide has been issued for comment Copies may be obtained from the American National Standards Institute, 1430 Broadway, New York, New York 10018.                    as Task SG 043-4.


USNRC    REGULATORY GUIDES                            Comments should be sent to the Secretary of the Commission, U.S. Nuclear Regulatory Commission, Washington, D.C. 20555, Attention: Docketing and Service Branch.
It should be noted that, in general, a working standard need not be fabricated from the same type of material being assayed. Even a material from a different radioactive species may be acceptable if carefully chosen and pre- pared. The essential requirements for a working standard are that (1) the radiation characteristics of the working stan- dard are sufficiently stable to ensure that fluctuations in instrument response during measurement control can con- fidently be attributed to aberrations in instrument param- eters rather than to variations in source characteristics and
(2) the working standard induces a response in the NDA
instrument that is characteristic of the expected response to real assay material. The most convenient means of achieving this "representative response" characteristic is to use mate- rial similar to the material that will be assayed.


Regulatory Guides are issued to describe and make available to the public methods acceptable to the NRC staff of implementing              The guides are issued in the following ten broad divisions:
A study should be made to determine the frequency with which the working standards are to be measured. If there is some instability, a working standard should be measured before and after each assay of an unknown item, and the calibration should be normalized to reflect the average of the before-assay and after-assay tests. In general, excessive instabilities should not be tolerated;
specific parts of the Commission's regulations, to delineate tech niques used by the staff in evaluating specific problems or postu      1. Power Reactors                  6. Products lated accidents or to provide guidance to applicants. Regulatory        2.  Research and Test Reactors      7. Transportation Guides are noi substitutes for regulations, and compliance with        3.  Fuels and Materials Facilities  8. Occupational Health them is not required. Methods and solutions different from those set    4.  Environmental  and  Siting    9. Antitrust and Financial Review out in the guides will be acceptable if they provide a basis for the   5.  Materials and Plant Protection 10. General findings requisite. to the issuance or continuance of a permit or license by the Commission.
they should be remedied by frequent recalibration. If instabilities persist, an alternative technique, an alternative instrument, or another measurement environment should be sought. In any case, a working standard should be measured a minimum of twice per shift, once at the beginning of the shift and again at some random time during the shift.


Copies of issued guides may be purchased at thecurrent Government This guide was issued after consideration of comments received from    Printing Office price. A subscription service for future guides in spe the public. Comments and suggestions for improvements in these          cific divisions is available through the Government Printing Office.
As a general principle, working standards should be run with a frequency directly proportional to the frequency of measurements (i.e.,
increase as the measurement frequency increases and decrease as the measurement frequency decreases). Also, the quantity of SNM in the standards measurements should closely follow the quanti- ties of SNM being measured (ie., the frequency of high- SNM-content working standards measurements increases as the frequency of assays of like items increases). These procedures provide a useful estimate of the bias when determined at the end of the inventory period. In addition, working standards should be run frequently enough for each measurement system so that no one system could contribute excessively to the inventory difference (ID) by being out of control for an extended period. A minimum of 16 control measurements should be made per material balance period. Assuming two systems having equal material flows in SNM quantity and number of items, the system with the greater uncertainty per measurement should run more working standards to reduce its potential impact on the ID.


Information on the subscription service and current GPO prices may guides are encouraged at all times, and guides will be revised, as     be obtained by writing the U.S. Nuclear Regulatory Commission, appropriate, to accommodate comments and to reflect new informa tion or experience.                                                    Washington, D.C. 20555, Attention: Publications Sales Manager.
Each response to a working standard should be compared to the previous calibration data as well as to the mean value
5.53-2


A decision should be made to reduce each potentially                    ically test the performance stability of the instrument.
of previous measurements of that working standard (under the same calibration) that were accumulated during the preceding material balance period. The difference should be plotted on a control chart. Control chart limits should be established at 0.05 and 0.001 levels of significance. When- ever control data exceed the 0.05 control limits, the test should be repeated. Whenever the control data exceed the
0.001 control limits, normal assay operations should cease.


significant source of error through (1) appropriate instrument              Each working standard should contain a different amount design considerations, (2) operational controls, or (3) supple              of the species of SNM to be assayed. Current licensing mentary measurements made to establish bias corrections                      review criteria require the use of four working standards.
Normal operations should not resume until the out-of- control performance has been remedied and the instrument has been recalibrated.


(see also Reference 1). Instrument procurement specifica On a rotating basis, one or two of these standards are used tions and operational instructions should be developed and                  to check the system each day.
The control chart of the working standard responses should be examined at frequent intervals to detect indica- tions of drift, which should be compensated. The frequency for such examinations should be determined by the operat- ing characteristics of each instrument. The minimum frequency for examining the control chart of a regularly used instrument for indications of drift should be once per week.


followed to reflect each error-reduction decision.
===5. CALIBRATION===
Calibration of NDA instruments should be accomplished by measuring the response to calibration standards as described in ANSI N15.20-1975.


It should be noted that, in general, a working standard To minimize operator-related errors and to promote uni                need not be fabricated from the same type of material form measurement practices, NDA instruments used for fixed                  being assayed. Even a material from a different radioactive station operations should be automated to control (1) data                  species may be acceptable if carefully chosen and pre acquisition and analysis, (2) diagnostic testing of instrument              pared. The essential requirements for a working standard performance stability and calibration validity, and (3) calcu                are that (1) the radiation characteristics of the working stan lation of associated error estimates. It is recognized that,                dard are sufficiently stable to ensure that fluctuations in for some less complicated NDA measurements, consistency                      instrument response during measurement control can con of operation may be achieved through the implementation                      fidently be attributed to aberrations in instrument param of carefully written and tested standard operating procedures.              eters rather than to variations in source characteristics and
The nuclear material content of these standards should be characterized through established assay procedures (e.g., chemical assays) that are calibrated relative to national standards or nationally accepted measurement systems. The calibration standards should represent the unknown items in all physical and chemical characteristics that affect the response of the instrument. Calibration data should be obtained by averag- ing the responses from repeated measurements of the calibration standards and should be corrected to remove observed nonrandom variations.
                                                                              (2) the working standard induces a response in the NDA
      Instruments should be tested to ensure that they meet                  instrument that is characteristic of the expected response to procurement specifications prior to calibration.                            real assay material. The most convenient means of achieving this "representative response" characteristic is to use mate
3. OPERATORS                                                                rial similar to the material that will be assayed.


Adequate operator qualification requirements are A study should be made to determine the frequency crucial to proper calibration and effective measurement with which the working standards are to be measured. If control of an NDA instrument. The qualification require                      there is some instability, a working standard should be ments should include a general knowledge of the assay measured before and after each assay of an unknown technique being used and an understanding of the typical                    item, and the calibration should be normalized to reflect behavior and the limitations of the instrument and the the average of the before-assay and after-assay tests. In technique. A knowledge of the external factors to which general, excessive instabilities should not be tolerated;
Recalibration of an instrument is required following repair or replacement of parts if measurement of one or more working standards shows the instrument response to have changed. In addition, the calibration should be checked following a power outage or any unusual mechanical or electrical shock to the system. Recalibration data are also required if the characteristics of the items to be assayed change to the extent that previous calibration standards no longer adequately represent the unknown items.
the measurement technique is sensitive (factors such as they should be remedied by frequent recalibration. If matrix composition, background, material forms, and                          instabilities persist, an alternative technique, an alternative container type) is also necessary. Only then can proper instrument, or another measurement          environment should standards be chosen for calibration and measurement                          be sought. In any case, a working          standard should be control data be interpreted effectively.                                    measured a minimum of twice per              shift, once at the beginning of the shift and again at        some random time If the operators have only a general knowledge of                      during the shift.


external factors, the NDA measurement program must be overseen by a director with a detailed knowledge of all As a general principle, working standards should be run related factors. Only qualified operators should be permit with a frequency directly proportional to the frequency ted to make SNM assays.                                                      of measurements (i.e., increase as the measurement frequency increases and decrease as the measurement
Criteria for segregating and packaging different forms of SNM should be developed and implemented. Each material category should be established to enhance assay perform- ance, consistent with safety requirements and subsequent processing needs. Guidance for material categorization is provided in Regulatory Guides 5.11, "Nondestructive Assay of Special Nuclear Material Contained in Scrap and Waste," 2 and 5.34, "Nondestructive Assay for Plutonium in Scrap Material by Spontaneous Fission Detection." 4 For all categories of materials to be assayed, with the exception of small-content miscellaneous categories (e.g.,
4. STABILITY TESTING                                                        frequency decreases). Also, the quantity of SNM in the standards measurements should closely follow the quanti A preventive maintenance program should be devised                      ties of SNM being measured (i.e., the frequency of high and implemented to ensure the long-term stability and                       SNM-content working standards measurements increases reliability of each instrument.                                              as the frequency of assays of like items increases). These procedures provide a useful estimate of the bias when As part of an ongoing Iprogram of measurement control, determined at the end of the inventory period. In addition, more working standards should be fabricated to period                        working standards should be run frequently enough for
4A proposed revision to this guide has been issued for comment as Task SG 046-4.
    3 Working standards are used to check the performance                  each measurement system so that no one system could of an      contribute excessively to the inventory difference (ID) by NDA instrument. They should be nominally representative of the items to be assayed. They should be fabricated and handled to              being out of control for an extended period. A minimum ensure their internal integrity so that deviations in the measured response of the assay system can be attributed to the instrument.          of 16 control measurements should be made per material As stated in ANSI Nl5.20-1975, working standards built to meet these requirements are not acceptable as calibration standards.             balance period. Assuming two systems having equal material Calibration standards are defined in ANSI N 15.20-1975 as "physically      flows in SNM quantity and number of items, the system and chemically similar to the items to be assayed, for which the mass of the nuclide(s) of interest and all properties to which the          with the greater uncertainty per measurement should run measurement technique is sensitive are known." Calibrationstandards        more working standards to reduce its potential impact on can be used as working standards, but working standards cannot be used as calibration standards. When calibration standards meet          the ID.


the requirements for working standards, licensees may elect to maintain only calibration standards. However, calibration standards may deteriorate through extensive use or may be prohibitively                    Each response to a working standard should be compared expensive for stability monitoring purposes.                                to the previous calibration data as well as to the mean value
furnace liner bricks, contaminated tools, or machine parts),
                                                                      5.53-2
the calibration relationship should be determined by a suitable method such as a least-squares fit to an appropriate function as described in ANSI N15.20-1975. The graphical calibration method is acceptable only for miscellaneous categories of material that contain a total of no more than
0.1 effective kilograms of SNM in each category during a material balance period. The combined contribution from all assays calibrated through the graphical method should be less than 10 percent of the total plant standard error (estimator) of inventory difference (SEID).
6. CALIBRATION STANDARDS
Calibration standards should be obtained to serve as the basis for the initial calibration of each instrument for each separate measurement technique or category of material.


of previous measurements of that working standard (under                  furnace liner bricks, contaminated tools, or machine parts),
The number of standards in each set should be greater than the number of free parameters in the calibration function for that set. It is recognized that, in some special cases, one set of calibration standards may suffice for more than one measurement technique or material category with proper analysis of the raw calibration data. Furthermore, if the NDA instrument is intended for use over a very narrow range of SNM loadings, a more restricted range of SNM
the same calibration) that were accumulated during the                    the calibration relationship should be determined by a preceding material balance period. The difference should be              suitable method such as a least-squares fit to an appropriate plotted on a control chart. Control chart limits should be                function as described in ANSI N15.20-1975. The graphical established at 0.05 and 0.001 levels of significance. When                calibration method is acceptable only for miscellaneous ever control data exceed the 0.05 control limits, the test                categories of material that contain a total of no more than should be repeated. Whenever the control data exceed the                  0.1 effective kilograms of SNM in each category during a
content in the calibration standards (confined to bracket the expected assay range) would prove adequate. The calibration standards should be completely characterized, including the mass and isotopic composition of the species of SNM to be assayed and all physical or chemical variables to which the response of the instrument is sensitive.
0.001 control limits, normal assay operations should cease.              material balance period. The combined contribution from Normal operations should not resume until the out-of                      all assays calibrated through the graphical method should control performance has been remedied and the instrumefit                be less than 10 percent of the total plant standard error has been recalibrated.                                                    (estimator) of inventory difference (SEID).
    The control chart of the working standard responses                  6. CALIBRATION STANDARDS
should be examined at frequent intervals to detect indica tions of drift, which should be compensated. The frequency                    Calibration standards should be obtained to serve as the for such examinations should be determined by the operat                  basis for the initial calibration of each instrument for each ing characteristics of each instrument. The minimum                      separate measurement technique or category of material.


frequency for examining the control chart of a regularly                  The number of standards in each set should be greater used instrument for indications of drift should be once per              than the number of free parameters in the calibration week.                                                                     function for that set. It is recognized that, in some special cases, one set of calibration standards may suffice for more
In general, the mass of SNM contained in the standards should extend over the range of loadings encountered in routine assays. This is especially true for NDA instruments whose responses are not linear functions of SNM content (e.g., some neutron-based NDA instruments). However, if the assay response (after application of appropriate correc- tions) is known to be highly linear and to have zero offset (i.e., zero response for zero SNM content), it may be more advantageous to avoid using standards with low loading, where calibration precision would suffer because of low count rates. In such a case, calibration in the upper half of the range of expected SNM loadings, combined with the constraint of zero response for zero loading, can produce a higher precision calibration than a least-squares fitting of measured responses to the standard over the full range of expected loadings, including values at low concentrations of SNM. If such a calibration procedure is used, careful initial establishment of the zero offset and instrument linearity followed by occasional verification of both assumptions is strongly recommended.
5. CALIBRATION                                                          than one measurement technique or material category with proper analysis of the raw calibration data. Furthermore, if Calibration of NDA instruments should be accomplished                the NDA instrument is intended for use over a very narrow by measuring the response to calibration standards as                    range of SNM loadings, a more restricted range of SNM
described in ANSI N15.20-1975. The nuclear material                      content in the calibration standards (confined to bracket content of these standards should be characterized through                the expected assay range) would prove adequate. The established assay procedures (e.g., chemical assays) that are            calibration standards should be completely characterized, calibrated relative to national standards or nationally                  including the mass and isotopic composition of the species accepted measurement systems. The calibration standards                  of SNM to be assayed and all physical or chemical variables should represent the unknown items in all physical and                   to which the response of the instrument is sensitive.


chemical characteristics that affect the response of the instrument. Calibration data should be obtained by averag                    In general, the mass of SNM contained in the standards ing the responses from repeated measurements of the                      should extend over the range of loadings encountered in calibration standards and should be corrected to remove                  routine assays. This is especially true for NDA instruments observed nonrandom variations.                                            whose responses are not linear functions of SNM content (e.g., some neutron-based NDA instruments). However, if Recalibration of an instrument is required following repair          the assay response (after application of appropriate correc or replacement of parts if measurement of one or more                    tions) is known to be highly linear and to have zero offset working standards shows the instrument response to have                  (i.e., zero response for zero SNM content), it may be more changed. In addition, the calibration should be checked                  advantageous to avoid using standards with low loading, following a power outage or any unusual mechanical or                    where calibration precision would suffer because of low electrical shock to the system. Recalibration data are also              count rates. In such a case, calibration in the upper half of required if the characteristics of the items to be assayed                the range of expected SNM loadings, combined with change to the extent that previous calibration standards no              the constraint of zero response for zero loading, can produce longer adequately represent the unknown items.                            a higher precision calibration than a least-squares fitting of measured responses to the standard over the full range of Criteria for segregating and packaging different forms of            expected loadings, including values at low concentrations of SNM should be developed and implemented. Each material                    SNM. If such a calibration procedure is used, careful initial category should be established to enhance assay perform                  establishment of the zero offset and instrument linearity ance, consistent with safety requirements and subsequent                  followed by occasional verification of both assumptions processing needs. Guidance for material categorization                    is strongly recommended. Such verification could be is provided in Regulatory Guides 5.11, "Nondestructive                    accomplished by an occasional extended measurement of a Assay of Special Nuclear Material Contained in Scrap and                  low-loading standard.
Such verification could be accomplished by an occasional extended measurement of a low-loading standard.


Waste," 2 and 5.34, "Nondestructive Assay for Plutonium in Scrap Material by Spontaneous Fission Detection."
Unless isotopic composition is being measured, the isotopic composition of the material used in all calibration standards should be similar to the isotopic composition of the material being assayed. This is especially important for
                                                                  4            Unless isotopic composition is being measured, the isotopic composition of the material used in all calibration For all categories of materials to be assayed, with the                standards should be similar to the isotopic composition of exception of small-content miscellaneous categories (e.g.,                the material being assayed. This is especially important for
5 The term "effective kilogram" is defined in paragraph 70.4(t)
      4A proposed revision to this guide has been issued for comment            SThe term "effective kilogram" is defined in paragraph 70.4(t)
of 10 CFR Part 70.
  as Task SG 046-4.                                                          of 10 CFR Part 70.


5.53-3
5.53-3


assays employing passive neutron coincidence counting or               7.2 Analytical Estimation Through the Calibration calorimetry. When the isotopic composition changes so that                 Relationship the response per gram of SNM differs by 10 percent or more from the value of the calibration standards, the                     When the calibration standards can be shown to represent material should be identified as a new material category.             adequately the unknown items, the bias associated with the The NDA system should be recalibrated for that category               NDA of an inventory of items can be estimated through the using new calibration standards made up using the new                 calibration relationship as demonstrated in ANSI N15.20
assays employing passive neutron coincidence counting or calorimetry. When the isotopic composition changes so that the response per gram of SNM differs by 10 percent or more from the value of the calibration standards, the material should be identified as a new material category.
isotopic composition. When the change in response per                 1975. The calibration standards should be fabricated from gram is less than 10 percent, a bias correction should be             different batches of material. The uncertainty associated determined and applied to the assay data.                            with the content of SNM elements and response-related isotopes contained in each calibration standard should be The uncertainty in the bias correction should be deter            based on an extensive characterization as described in mined and accounted for in estimating the total assay                ANSI N15.20-1975. The uncertainty associated with the, uncertainty. Appropriate error propagation procedures are            contained mass of the response-related isotopes should be described in Regulatory Guide 5.18, "Limit of Error                  included in the calibration as described in the standard.
 
The NDA system should be recalibrated for that category using new calibration standards made up using the new isotopic composition. When the change in response per gram is less than 10 percent, a bias correction should be determined and applied to the assay data.


Concepts and Principles of Calculation in Nuclear Materials           Further, the element uncertainty should be factored into Control."                                                            the estimated total assay uncertainty.
The uncertainty in the bias correction should be deter- mined and accounted for in estimating the total assay uncertainty. Appropriate error propagation procedures are described in Regulatory Guide 5.18, "Limit of Error Concepts and Principles of Calculation in Nuclear Materials Control."
When the response is sensitive to ingrowth or decay of a daughter product, the procedures described in the preced- ing paragraphs are appropriate and should be applied.


When the response is sensitive to ingrowth or decay of a              Using this procedure, it is necessary to periodically daughter product, the procedures described in the preced              ensure that the calibration standards adequately represent ing paragraphs are appropriate and should be applied.                  the unknown items. This can be accomplished by isolating and characterizing the extraneous interference factors Once fabricated, the calibration standards should be             that affect the response of the instrument. Typically, this handled with extreme care to attempt to ensure that the               separation and characterization is most easily accomplished distribution of contents remains fixed. It should be noted           when the items are either finished fuel items or uniform that solution standards lose their integrity over time because         containers of feed or intermediate product material.
Once fabricated, the calibration standards should be handled with extreme care to attempt to ensure that the distribution of contents remains fixed. It should be noted that solution standards lose their integrity over time because of evaporation and diffusion (Ref. 2) and radiolysis (Ref. 3).
Calibration standards prepared by the mixing of different powders or densities tend to stratify or segregate. The containers should be tumbled periodically to reblend the constituents. Calibration standards should be used only when developing the initial calibration or when recalibrat- ing the instrument following a repair or power outage.


of evaporation and diffusion (Ref. 2) and radiolysis (Ref. 3).
Working standards should be used to test the continued stability of the instrument (see footnote 3).
Calibration standards prepared by the mixing of different                To ensure that the calibration standards continue to powders or densities tend to stratify or segregate. The                adequately represent unknown items, key parameters 6 that containers should be tumbled periodically to reblend                  affect the observed response (i.e., item-to-item variations)
The degree of effort that should be expended in fabricat- ing the calibration standards depends on the method used to estimate the assay uncertainty, as described in the next section.
the constituents. Calibration standards should be used only            should be monitored through separate tests. Measurements when developing the initial calibration or when recalibrat            of the key parameters should be compiled and analyzed at ing the instrument following a repair or power outage.                least twice a month to catch any large instrument drift. For Working standards should be used to test the continued               more timely measurement control, a superior approach stability of the instrument (see footnote 3).                         would be to perform such analyses on a continuing basis and repeat measurements of unknowns where standards The degree of effort that should be expended in fabricat         exceed control limits. This latter approach minimizes the ing the calibration standards depends on the method used             backfitting of measurement data and provides a timely to estimate the assay uncertainty, as described in the next           basis for measurement control.


section.
7. METHODS FOR ESTIMATING UNCERTAINTY
Instrument errors associated with NDA should be estimated periodically by means of replicate assays as described in ANSI N15.20-1975.


When the mean value of a parameter shifts from its
Three methods are acceptable to estimate the uncertain- ties associated with calibrations and bias corrections for NDA. The first two procedures, graphical estimation and analytical estimation through the calibration relationship, are detailed in ANSI N15.20-1975. The third procedure, comparative evaluation, is not described in the standard.
7. METHODS FOR ESTIMATING UNCERTAINTY                                previously established value, the impact of the shift on the response of the assay instrument should be measured Instrument errors associated with NDA should be                  through an appropriate experiment or calculation (Ref. 4).
estimated periodically by means of replicate assays as                An appropriate bias correction should be determined and described in ANSI N15.20-1975.                                        applied to all items that were assayed after the best estimate of when the parameter changed. The uncertainty in that Three methods are acceptable to estimate the uncertain           bias estimate should be combined with the uncertainty in ties associated with calibrations and bias corrections for           the assay values as predicted through the calibration function NDA. The first two procedures, graphical estimation and               to estimate the total assay uncertainty.


analytical estimation through the calibration relationship, are detailed in ANSI N15.20-1975. The third procedure,                    The uncertainty due to a bias correction may significantly comparative evaluation, is not described in the standard.            increase the standard error of the assay. In severe cases, the effect may increase the SEID above the level acceptable for the total plant. In such cases, new calibration standards
7.1 Graphical Estimation Use of the graphical error estimation technique should result in a conservative error estimate that is acceptable for miscellaneous unusual assay categories, as described in Regulatory Position 5 of this guide.
7.1 Graphical Estimation                                              should be obtained and the assay system should be recali brated.


Use of the graphical error estimation technique should result in a conservative error estimate that is acceptable for           6 See Section 5.4 of ANSI N15.20-1975. See Regulatory miscellaneous unusual assay categories, as described in                                                                                Posi tion 6 of this guide for provisions to include the effects of changing Regulatory Position 5 of this guide.                                  isotopic compositions.
7.2 Analytical Estimation Through the Calibration Relationship When the calibration standards can be shown to represent adequately the unknown items, the bias associated with the NDA of an inventory of items can be estimated through the calibration relationship as demonstrated in ANSI N15.20-
1975. The calibration standards should be fabricated from different batches of material The uncertainty associated with the content of SNM elements and response-related isotopes contained in each calibration standard should be based on an extensive characterization as described in ANSI N15.20-1975. The uncertainty associated with the, contained mass of the response-related isotopes should be included in the calibration as described in the standard.
 
Further, the element uncertainty should be factored into the estimated total assay uncertainty.
 
Using this procedure, it is necessary to periodically ensure that the calibration standards adequately represent the unknown items. This can be accomplished by isolating and characterizing the extraneous interference factors that affect the response of the instrument. Typically, this separation and characterization is most easily accomplished when the items are either finished fuel items or uniform containers of feed or intermediate product material.
 
To ensure that the calibration standards continue to adequately represent unknown items, key parameters6 that affect the observed response (i.e., item-to-item variations)
should be monitored through separate tests. Measurements of the key parameters should be compiled and analyzed at least twice a month to catch any large instrument drift. For more timely measurement control, a superior approach would be to perform such analyses on a continuing basis and repeat measurements of unknowns where standards exceed control limits. This latter approach minimizes the backfitting of measurement data and provides a timely basis for measurement control.
 
When the mean value of a parameter shifts from its previously established value, the impact of the shift on the response of the assay instrument should be measured through an appropriate experiment or calculation (Ref. 4).
An appropriate bias correction should be determined and applied to all items that were assayed after the best estimate of when the parameter changed. The uncertainty in that bias estimate should be combined with the uncertainty in the assay values as predicted through the calibration function to estimate the total assay uncertainty.
 
The uncertainty due to a bias correction may significantly increase the standard error of the assay. In severe cases,. the effect may increase the SEID above the level acceptable for the total plant. In such cases, new calibration standards should be obtained and the assay system should be recali- brated.
 
6 See Section 5.4 of ANSI N15.20-1975.
 
See Regulatory Posi- tion 6 of this guide for provisions to include the effects of changing isotopic compositions.


5.53-4
5.53-4


As a further check on the continued validity of the cali           2. For plutonium-bearing items only, each item can be bration standards, a program to periodically introduce new         assayed through calorimetric procedures (see Reference 5).
As a further check on the continued validity of the cali- bration standards, a program to periodically introduce new calibration standards should be implemented. The rate of replacement of standards with fresh material depends on the intrinsic durability and stability of the standard in question. Some solution standards lose their calibrated concentration values in a matter of days or weeks. On the other hand, standard fuel rods are much more durable and may last indefinitely with careful handling. In any case, calibration standards should be replaced with new standards at a rate sufficiently above their failure rate to ensure continued high quality in the instrument calibration.
calibration standards should be implemented. The rate of           Large items should be subdivided into smaller containers.
 
7.3 Comparative Evaluation The procedure described in this section is not included in ANSI N15.20-1975 but is appropriate for determining the validity of the calibration of NDA instruments.
 
When two measurement methods are used for each of a series of items and one of the methods is considerably more accurate than the other, corresponding measurements can be usefully compared. The comparison can be used to establish an estimate of bias between the measurement methods. The comparison can also be used to estimate the total uncertainty associated with the less accurate measure-
*ment method.
 
To determine the uncertainty associated with the NDA
of an inventory of items using this method, unknown items should be randomly selected for comparative measurements.
 
The SNM content of the items selected should span the range of contents normally encountered, subject to the qualification pointed out in Regulatory Position 6. Random error should be estimated through replicate analyses. To estimate the remaining contributions to the total assay uncertainty, each item should be repeatedly assayed to reduce the random assay error to less than 10 percent of the estimated or previously established total uncertainty.
 
Then, to determine the SNM content of each item selected for comparative evaluation, one of the following procedures should be employed:
1. Each item should be completely dissolved, independ- ently, and the resulting solution should be analyzed by high-accuracy elemental and isotopic assay procedures, which in turn are calibrated relative to national standards or nationally accepted measurement systems. It should be recognized that dissolution residues may be present in such a procedure. These residues should also be assayed for a complete analysis. Items composed of an aggregate of similar units, e.g., fuel rods containing discrete pellets, should be opened and the contained units should be weighed, pulverized, blended, and sampled for assay through appro- priate high-accuracy elemental and isotopic assay proce- dures. The emptied container should be examined for indications of residual accumulations and cleaned, leached, or assayed nondestructively to determine the residual SNM
content.


replacement of standards with fresh material depends on            Each small container should be assayed calorimetrically.
2. For plutonium-bearing items only, each item can be assayed through calorimetric procedures (see Reference 5).
Large items should be subdivided into smaller containers.


the intrinsic durability and stability of the standard in          Samples should be taken from at least three of the smaller question. Some solution standards lose their calibrated            containers. The samples should be measured by micro concentration values in a matter of days or weeks. On the          calorimetry and then assayed through highly accurate other hand, standard fuel rods are much more durable and            elemental and isotopic procedures that, in turn, are calibrated may last indefinitely with careful handling. In any case,          relative to national standards or nationally accepted measure calibration standards should be replaced with new standards        ment systems (Ref. 6). The isotopic measurement data at a rate sufficiently above their failure rate to ensure          should be examined for evidence of nonhomogeneous continued high quality in the instrument calibration.              isotopic content. Isotopically nonhomogeneous materials should be blended and reanalyze
Each small container should be assayed calorimetrically.


====d. On the basis of the====
Samples should be taken from at least three of the smaller containers. The samples should be measured by micro- calorimetry and then assayed through highly accurate elemental and isotopic procedures that, in turn, are calibrated relative to national standards or nationally accepted measure- ment systems (Ref. 6). The isotopic measurement data should be examined for evidence of nonhomogeneous isotopic content. Isotopically nonhomogeneous materials should be blended and reanalyzed. On the basis of the average grams of plutonium per watt of the samples meas- ured by microcalorimetry, the total amount of plutonium in each of the smaller containers should be determined. The total plutonium content of the items selected for compar- ison is then estimated as the combined contents of the smaller containers.
7.3 Comparative Evaluation                                          average grams of plutonium per watt of the samples meas ured by microcalorimetry, the total amount of plutonium The procedure described in this section is not included        in each of the smaller containers should be determined. The in ANSI N15.20-1975 but is appropriate for determining the          total plutonium content of the items selected for compar validity of the calibration of NDA instruments.                    ison is then estimated as the combined contents of the smaller containers.


When two measurement methods are used for each of a series of items and one of the methods is considerably more            For the first full material balance period during the accurate than the other, corresponding measurements can            initial implementation of this guide, two items from each be usefully compared. The comparison can be used to                category of assay items should be randomly selected each establish an estimate of bias between the measurement              week for a check of the validity of the instrument cali methods. The comparison can also be used to estimate the            bration. Following this initial implementation period, total uncertainty associated with the less accurate measure        licensees may reduce the verification measurement frequency
For the first full material balance period during the initial implementation of this guide, two items from each category of assay items should be randomly selected each week for a check of the validity of the instrument cali- bration. Following this initial implementation period, licensees may reduce the verification measurement frequency to two items per month per category. When fewer than 100
,ment method.                                                        to two items per month per category. When fewer than 100
new items of a given category are created per week, at least two of the item-comparison verification measurements should be made per material balance period per category through the procedures described above. In such cases, to provide an adequate data base to update the uncertainty estimates for NDA, licensees may pool the verification data provided the measurements are in statistical control, i.e.,
                                                                    new items of a given category are created per week, at To determine the uncertainty associated with the NDA            least two of the item-comparison verification measurements of an inventory of items using this method, unknown items          should be made per material balance period per category should be randomly selected for comparative measurements.          through the procedures described above. In such cases, to The SNM content of the items selected should span the              provide an adequate data base to update the uncertainty range of contents normally encountered, subject to the            estimates for NDA, licensees may pool the verification data qualification pointed out in Regulatory Position 6. Random        provided the measurements are in statistical control, i.e.,
when repeated samples from the portion of the measure- ment system under test behave as random samples from a stable probability distribution. Under such conditions, data sets may be combined provided the parameters based on the current set of data and the previous set of data are not significantly different on the basis of acceptable statistical tests.
  error should be estimated through replicate analyses. To          when repeated samples from the portion of the measure estimate the remaining contributions to the total assay            ment system under test behave as random samples from a uncertainty, each item should be repeatedly assayed to            stable probability distribution. Under such conditions, data reduce the random assay error to less than 10 percent of          sets may be combined provided the parameters based on the estimated or previously established total uncertainty.        the current set of data and the previous set of data are not Then, to determine the SNM content of each item selected          significantly different on the basis of acceptable statistical for comparative evaluation, one of the following procedures        tests.


should be employed:
As an alternative to this selection criterion, licensees may elect the latter frequency for a specific category when it can be demonstrated that the contribution to the SEID
                                                                          As an alternative to this selection criterion, licensees
from that category is less than 100 grams in any mate- rial balance period.
      1. Each item should be completely dissolved, independ          may elect the latter frequency for a specific category when ently, and the resulting solution should be analyzed by            it can be demonstrated that the contribution to the SEID
  high-accuracy elemental and isotopic assay procedures,            from that category is less than 100 grams in any mate which in turn are calibrated relative to national standards        rial balance period.


or nationally accepted measurement systems. It should be recognized that dissolution residues may be present in such            At the close of the reporting period, differences between a procedure. These residues should also be assayed for a            assay values and verification values should be recorded and complete analysis. Items composed of an aggregate of              tested for outliers. Methods for detecting outliers are similar units, e.g., fuel rods containing discrete pellets,        described in ANSI/ASTM E178-80, "Practice for Dealing with should be opened and the contained units should be weighed,        Outlying Observations." 7 See also Regulatory Guide 5.36, pulverized, blended, and sampled for assay through appro            "Recommended Practice for Dealing with Outlying Observa priate high-accuracy elemental and isotopic assay proce            tions," for further details.
At the close of the reporting period, differences between assay values and verification values should be recorded and tested for outliers. Methods for detecting outliers are described in ANSI/ASTM E 178-80, "Practice for Dealing with Outlying Observations."'7 See also Regulatory Guide 5.36,
"Recommended Practice for Dealing with Outlying Observa- tions," for further details.


dures. The emptied container should be examined for indications of residual accumulations and cleaned, leached,
7 Copies may be obtained from the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pennsylvania 19103.
                                                                          7 or assayed nondestructively to determine the residual SNM                Copies may be obtained from the American Society for Testing content.                                                            and Materials, 1916 Race Street, Philadelphia, Pennsylvania 19103.


5.53-5
5.53-5


A straight line with a nonzero intercept should be fitted         that may influence the response of the assay system should to the nondestructive assay vs. verification measurement             be investigated. The investigation should also address the data as described in ANSI N15.20-1975. The slope and                 comparative measurement method, including sampling, intercept should be jointly tested for one and zero, respec         sample handling, analytical procedures, interference com tively, using the "F" ratio at the 5 percent significance level     pensation, and calibration validity. Results from the investi (Ref. 7). If this result is significant, separate tests on the                                                                     I
A straight line with a nonzero intercept should be fitted to the nondestructive assay vs. verification measurement data as described in ANSI N15.20-1975. The slope and intercept should be jointly tested for one and zero, respec- tively, using the "F" ratio at the 5 percent significance level (Ref. 7). If this result is significant, separate tests on the slope equal to one and the intercept equal to zero should be made to determine the presence of either proportional or constant bias or both. When bias is indicated, the assay results during the preceeding operating period should be corrected. The variance associated with the bias corrections should be estimated by the standard error of estimate of the verification line. This variance must be included in the estimate of the variance of an assay result as described in ANSI N15.20-1975.
                                                                    gation, if they show the NDA system to have been incorrectly slope equal to one and the intercept equal to zero should be         calibrated, should be employed to recalibrate the instrument made to determine the presence of either proportional or             for the forthcoming material balance period. Conversely, constant bias or both. When bias is indicated, the assay             when the source of bias can be attributed to errors in the results during the preceeding operating period should be            comparative measurements, bias corrections should not be corrected. The variance associated with the bias corrections         made to the items assayed by NDA. Results from such should be estimated by the standard error of estimate of             investigations should be documented, and the documents the verification line. This variance must be included in the         should be maintained in accordance with Regulatory estimate of the variance of an assay result as described in         Position 8 of this guide.
 
Whenever a bias exceeding 50 percent of its estimated uncertainty is indicated, its cause should be investigated.


ANSI N15.20-1975.
This investigation should include a review of the assump- tions factored into the NDA system's calibration. In partic- ular, instrument stability and the stability of parameters that may influence the response of the assay system should be investigated. The investigation should also address the comparative measurement method, including sampling, sample handling, analytical procedures, interference com- pensation, and calibration validity. Results from the investi- gation, if they show the NDA system to have been incorrectly calibrated, should be employed to recalibrate the instrument for the forthcoming material balance period. Conversely, when the source of bias can be attributed to errors in the comparative measurements, bias corrections should not be made to the items assayed by NDA. Results from such investigations should be documented, and the documents should be maintained in accordance with Regulatory Position 8 of this guide.


===8. RECORDS RETENTION===
===8. RECORDS RETENTION===
    Whenever a bias exceeding 50 percent of its estimated uncertainty is indicated, its cause should be investigated.              All records generated in connection with the activities This investigation should include a review of the assump            discussed in this guide, including control charts, should be tions factored into the NDA system's calibration. In partic          retained for a period of 5 years, as specified in para ular, instrument stability and the stability of parameters          graph 70.5 1(e)(4)(iii) of 10 CFR Part 70.
All records generated in connection with the activities discussed in this guide, including control charts, should be retained for a period of 5 years, as specified in para- graph 70.5 1(e)(4)(iii) of 10 CFR Part 70.


5.53-6
5.53-6


REFERENCES
REFERENCES
                                                                4. R. A. Forster, D. B. Smith, and H. 0. Menlove, "Error
1. T. E. Shea, "Reduction, Control, and Estimation of Nondestructive Assay Errors," Nuclear Materials Manage- ment, Vol. III, No. 3, 1974.
1. T. E. Shea, "Reduction, Control, and Estimation of Analysis of a Cf-252 Fuel-Rod-Assay System," Los Nondestructive Assay Errors," Nuclear MaterialsManage Alamos Scientific Laboratory, LA-5317, 1974.
 
2. G. J. Curtis, J. E. Rein, and S. S. Yamamura, "Compara- tive Study of Different Methods of Packaging Liquid Reagents," Analytical Chemistry, Vol. 45, No. 6, p. 996,
1973.
 
3. J. R. Weiss and E. E. Pietri, "Calculation of Hydrogen Generation from Pu-Induced Alpha Radiolysis of Nitric, Sulfuric, and Perchloric Acids," Radiation Effects, Vol.


ment, Vol III, No. 3, 1974.
19, p. 191, 1973.


5. U.S. Nuclear Regulatory Commission, "Calorimetric
4. R. A. Forster, D. B. Smith, and H. 0. Menlove, "Error Analysis of a Cf-252 Fuel-Rod-Assay System," Los Alamos Scientific Laboratory, LA-5317, 1974.
2. G. J. Curtis, J. E. Rein, and S. S. Yamamura, "'Compara          Assay for Plutonium," NUREG-0228, 1977.


tive Study of Different Methods of Packaging Liquid Reagents," Analytical Chemistry, Vol. 45, No. 6, p. 996,
S. U.S.
                                                                6. F. S. Stephens et al., "Methods for the Accountability
  1973.


of Plutonium Dioxide," U.S. Nuclear Regulatory Com mission, WASH-1335, 1975.
Nuclear Regulatory Commission, "Calorimetric Assay for Plutonium," NUREG-0228, 1977.


3. J. R. Weiss and E. E. Pietri, "Calculation of Hydrogen Generation from Pu-Induced Alpha Radiolysis of Nitric,
6. F. S. Stephens et al., "Methods for the Accountability of Plutonium Dioxide," U.S. Nuclear Regulatory Com- mission, WASH-1335, 1975.
                                                                7. F. A. Graybill, An Introduction to Linear Statistical Sulfuric, and Perchloric Acids," Radiation Effects, Vol.        Models, McGraw-Hill, New York, Vol. I, p. 128, 1961.


19, p. 191, 1973.
7. F. A. Graybill, An Introduction to Linear Statistical Models, McGraw-Hill, New York, Vol. 1, p. 128, 1961.


5.53-7
5.53-7


BIBLIOGRAPHY
BIBLIOGRAPHY
Alvar, K., H. Lukens, and N. Lurie, "Standard Containers           This book provides a complete discussion of for SNM Storage, Transfer, and Measurement," U.S. Nu                 statistical procedures and describes a variety of clear Regulatory Commission, NUREG/CR-1847, 1980.                    statistical tests of experimental data. Examples are provided.
Alvar, K., H. Lukens, and N. Lurie, "Standard Containers for SNM Storage, Transfer, and Measurement," U.S. Nu- clear Regulatory Commission, NUREG/CR-1847, 1980.


This report details the variations of container properties (especially wall thicknesses) and their effects on NDA measurements. A candidate                     Reilly, T. D., and M. L. Evans, "Measurement Reliability list of standard containers, each sufficiently               for Nuclear Material Assay," Nuclear Materials Manage uniform to cause less than 0.2 percent variation             ment, Vol. VI, No. 2, 1977.
This report details the variations of container properties (especially wall thicknesses) and their effects on NDA measurements. A candidate list of standard containers, each sufficiently uniform to cause less than 0.2 percent variation in assay results, is given, along with comments on the value and impact of container standardization.


in assay results, is given, along with comments on the value and impact of container standardization.              This paper provides an overview of experience in nuclear material assay by analytical chemistry, Brouns, R. J., F. P. Roberts, and U. L. Upson, "Considera           calorimetry, and nondestructive assay. Ranges tions for Sampling Nuclear Materials for SNM Accounting             of accuracy and precision obtained in the assay Measurements," U.S. Nuclear Regulatory Commission,                 of nuclear material are given.
Brouns, R. J., F. P. Roberts, and U. L. Upson, "Considera- tions for Sampling Nuclear Materials for SNM Accounting Measurements,"  
U.S. Nuclear Regulatory Commission, NUREG/CR-0087, 1978.


NUREG/CR-0087, 1978.
This report presents principles and guidelines for sampling nuclear materials to measure chemical and isotopic content of the material. Develop- ment of sampling plans and procedures that maintain random and systematic errors of sampling within acceptable limits for SNM
accounting purposes are emphasized.


This report presents principles and guidelines for            Sher, R., and S. Untermeyer, The Detection of Fissionable sampling nuclear materials to measure chemical                Materials by Nondestructive Means, American Nuclear and isotopic content of the material. Develop                Society Monograph, 1980.
Cooper, B. E., Statistics for Experimentalists, Pergamon Press, New York, 1969.


ment of sampling plans and procedures that maintain random and systematic errors of                        This book contains a helpful overview of a wide sampling within acceptable limits for SNM                      variety of nondestructive assay techniques for accounting purposes are emphasized.                              special nuclear material. In addition, it contains a rather extensive discussion of error estimation Cooper, B. E., Statistics for Experimentalists, Pergamon            and measurement control techniques, as well as a Press, New York, 1969.                                              presentation on measurement statistics.
This book provides a complete discussion of statistical procedures and describes a variety of statistical tests of experimental data. Examples are provided.


h
Reilly, T. D., and M. L. Evans, "Measurement Reliability for Nuclear Material Assay," Nuclear Materials Manage- ment, Vol. VI, No. 2, 1977.
                                                          5.53-8


VALUE/IMPACT STATEMENT
This paper provides an overview of experience in nuclear material assay by analytical chemistry, calorimetry, and nondestructive assay. Ranges of accuracy and precision obtained in the assay of nuclear material are given.
1. PROPOSED ACTION                                                    1.3.4 Public
 
1.1 Description                                                      No impact on the public can be foreseen.
Sher, R., and S. Untermeyer, The Detection of Fissionable Materials by Nondestructive Means, American Nuclear Society Monograph, 1980.


Licensees authorized to possess at any one time more          1.4 Decision than one effective kilogram of special nuclear material (SNM) are required in paragraph 70.58(f) of 10 CFR Part 70            The guide should be revised to reflect the affirmation of to establish, maintain, and follow a program for the main          ANSI N15.20-1975 in 1980 and to make it more consistent tenance of acceptable measurement quality in terms of              with current usage.
This book contains a helpful overview of a wide variety of nondestructive assay techniques for special nuclear material. In addition, it contains a rather extensive discussion of error estimation and measurement control techniques, as well as a presentation on measurement statistics.


measurement bias and for the evaluation and control of the quality of the measurement syste
5.53-8


====m.      ====
VALUE/IMPACT STATEMENT


===2. TECHNICAL APPROACH===
===1. PROPOSED ACTION===
    This guide describes methods and procedures acceptable            Not applicable.
1.3.4 Public
1.1 Description No impact on the public can be foreseen.


to the NRC staff for meeting the provisions of para graph 70.58(f) of 10 CFR Part 70 for nondestructive assay         
Licensees authorized to possess at any one time more than one effective kilogram of special nuclear material (SNM) are required in paragraph 70.5 8(f) of 10 CFR Part 70
to establish, maintain, and follow a program for the main- tenance of acceptable measurement quality in terms of measurement bias and for the evaluation and control of the quality of the measurement system.


===3. PROCEDURAL APPROACH===
This guide describes methods and procedures acceptable to the NRC staff for meeting the provisions of para- graph 70.58(f) of 10 CFR Part 70 for nondestructive assay (NDA) systems.
(NDA) systems.


Of the procedural alternatives considered, revision of the The proposed action would revise the guide, which is           existing regulatory guide was selected as the most advanta still basically sound.                                            geous and cost effective.
The proposed action would revise the guide, which is still basically sound.


1.2 Need                                                           4. STATUTORY CONSIDERATIONS
1.2 Need The regulatory guide endorses ANSI N15.20-1975,
    The regulatory guide endorses ANSI N15.20-1975,               4.1 NRC Authority
"Guide to Calibrating Nondestructive Assay Systems."
"Guide to Calibrating Nondestructive Assay Systems."
This standard was reaffirmed without modification in 1980             Authority for the proposed action is derived from the and the regulatory guide should be revised to indicate this.       Atomic Energy Act of 1954, as amended, and the Energy Further, revisions are needed in some sections to make the         Reorganization Act of 1974, as amended, and implemented guide clearer and more consistent with current thinking.          through the Commission's regulations, in particular § 70.51 of 10 CFR Part 70.
This standard was reaffirmed without modification in 1980
and the regulatory guide should be revised to indicate this.
 
Further, revisions are needed in some sections to make the guide clearer and more consistent with current thinking.


This proposed action is needed to bring Regulatory Guide 5.53 up to date.                                            4.2 Need for NEPA Assessment
This proposed action is needed to bring Regulatory Guide 5.53 up to date.
1.3 Value/Impact                                                      The proposed action is not a major action that may significantly affect the quality of the human environment
    1.3.1 NRC                                                      and does not require an environmental impact statement.


1.3 Value/Impact
1.3.1 NRC
The regulatory positions will be brought up to date.
The regulatory positions will be brought up to date.


S. RELATIONSHIP TO OTHER EXISTING OR
1.3.2 Other Government Agencies Not applicable.
    1.3.2 Other Government Agencies                                   PROPOSED REGULATIONS OR POLICIES
 
    Not applicable.                                                  The proposed action is one of a series of revisions of existing regulatory guides on nondestructive assay techniques.
1.3.3 Industry Since industry is already applying the methods and procedures discussed in the guide, updating these should have no adverse impact.
 
1.4 Decision The guide should be revised to reflect the affirmation of ANSI N15.20-1975 in 1980 and to make it more consistent with current usage.
 
===2. TECHNICAL APPROACH===
Not applicable.
 
===3. PROCEDURAL APPROACH===
Of the procedural alternatives considered, revision of the existing regulatory guide was selected as the most advanta- geous and cost effective.
 
4. STATUTORY CONSIDERATIONS
4.1 NRC Authority Authority for the proposed action is derived from the Atomic Energy Act of 1954, as amended, and the Energy Reorganization Act of 1974, as amended, and implemented through the Commission's regulations, in particular § 70.51 of 10 CFR Part 70.
 
4.2 Need for NEPA Assessment The proposed action is not a major action that may significantly affect the quality of the human environment and does not require an environmental impact statement.
 
5. RELATIONSHIP TO OTHER EXISTING OR
PROPOSED REGULATIONS OR POLICIES
The proposed action is one of a series of revisions of existing regulatory guides on nondestructive assay techniques.


1.3.3 Industry
6. SUMMARY AND CONCLUSIONS
                                                                  6. SUMMARY AND CONCLUSIONS
A revised guide should be prepared to bring Regulatory Guide 5.53 up to date.
    Since industry is already applying the methods and procedures discussed in the guide, updating these should              A revised guide should be prepared to bring Regulatory have no adverse impact.                                            Guide 5.53 up to date.


5.53-9
5.53-9


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Revision as of 10:41, 11 January 2025

Qualification, Calibration, and Error Estimation Methods for Nondestrutive Assay
ML13064A081
Person / Time
Issue date: 02/28/1984
From:
Office of Nuclear Regulatory Research
To:
References
RG-5.053, Rev. 1
Download: ML13064A081 (10)


Revision 1*

February 1984 U.S. NUCLEAR REGULATORY COMMISSION

REGULATORY GUIDE

OFFICE OF NUCLEAR REGULATORY RESEARCH

REGULATORY GUIDE 5.53 (Task SG 049-4)

QUALIFICATION, CALIBRATION, AND ERROR ESTIMATION

METHODS FOR NONDESTRUCTIVE ASSAY

A. INTRODUCTION

Section70.58, "Fundamental Nuclear Material Con- trols," of 10 CFR Part 70, "Domestic Licensing of Special Nuclear Material," requires certain licensees to establish a measurement quality assurance program for material control and accounting. Specifically, paragraph 70.58(f)

requires that a program be established, maintained, and followed for the maintenance of acceptable measurement quality in terms of measurement bias and for the evalua- tion and control of the quality of the measurement system.

Nondestructive assay (NDA)

constitutes a unique measurement technology. When applied under appropriate rigorous controls, it can enhance the ability of the material control and accounting system to detect unaccounted-for loss or diversion of special nuclear material (SNM) to unauthorized uses. This guide describes methods and procedures acceptable to the NRC staff for meeting the provisions of paragraph 70.58(f) of 10 CFR Part 70 as it relates to the use of nondestructive assay.

Any guidance in this document related to information collection activities has been cleared under 0MB Clearance No. 3150-0009.

B. DISCUSSION

Nondestructive assay has been applied to virtually every chemical or physical form of special nuclear material encountered in contemporary reactor fuel processing.

Special considerations are required to achieve high- accuracy assay results and to properly estimate the errors associated with NDA applications.

Recognizing these considerations, the American National Standards Institute has developed a standard, ANSI N15.20-1975, "Guide to Calibrating Nondestructive Assay Systems."1 This standard

1Copies may be obtained from the American National Standards Institute, 1430 Broadway, New York, New York 10018.

was reviewed and reaffirmed without modification in

1980. This guide endorses the entire standard as supple- mented in the regulatory position.

C. REGULATORY POSITION

The methods, procedures, and guidance relating to the application of NDA in ANSI N1S.20-1975, "Guide to Calibrating Nondestructive Assay Systems," are accept- able to the NRC staff for use in material protection programs as supplemented by the following.

1. METHOD SELECTION

Prior to selecting an assay method, a study should be made to determine the required performance for that appli- cation. The specific NDA method should be selected to provide results that are compatible with plant material balance requirements.

Methods to enhance attainable performance should be considered (e.g., container selec- tion and packaging procedures for bulk materials discussed in Regulatory Guide 5.11,

"Nondestructive Assay of Special Nuclear Material Contained in Scrap and Waste" 2 ).

2. INSTRUMENT SPECIFICATIONS

An evaluation of each new NDA application, including the proposed placement of the instrument, should be conducted prior to procurement. Studies of existing NDA

applications should be conducted periodically to evaluate their performance and substantiate the basis for their continued use. The impact of each of the measurement-to- measurement sources of error encountered in practice or anticipated should be established as a part of each of these efforts.

The substantial number of changes in this revision has made it impractical to indicate the changes with lines in the margin.

2A proposed revision to this guide has been issued for comment as Task SG 043-4.

USNRC REGULATORY GUIDES

Regulatory Guides are issued to describe and make available to the public methods acceptable to the N RC staff of implementing specific parts of the Commission's regulations to delineate tech- niques used by the staff in evaluating specific 'problems or postu- lated accidents or to provide guidance to applicants. Regulatory Guides are no* substitutes for regulations, and compliance with them is not required. Methods and solutions different from those set out in the guides will be acceptable if they provide a basis for the findings requisite, to the issuance or continuance of a permit or license by the Commission.

This guide was issued after consideration of comments received from the public. Comments and suggestions for improvements in these guides are encouraged at all times, and guides will be revised, as appropriate, to accommodate comments and to reflect new informa- tion or exoerience.

Comments should be sent to the Secretary of the Commission, U.S. Nuclear Regulatory Commission, Washington, D.C. 20555, Attention: Docketing and Service Branch.

The guides are issued in the following ten broad divisions:

1. Power Reactors

6. Products

2. Research and Test Reactors

7. Transportation

3. Fuels and Materials Facilities

8. Occupational Health

4. Environmental and Siting

9. Antitrust and Financial Review

5. Materials and Plant Protection 10. General Copies of issued guides may be purchased at the current Government Printing Office price. A subscription service for future guides in spe- cific divisions is available through the Government Printing Office.

Information on the subscription service and current GPO prices may be obtained by writing the U.S. Nuclear Regulatory Commission, Washington, D.C. 20555, Attention: Publications Sales Manager.

A decision should be made to reduce each potentially significant source of error through (1) appropriate instrument design considerations, (2) operational controls, or (3) supple- mentary measurements made to establish bias corrections (see also Reference 1). Instrument procurement specifica- tions and operational instructions should be developed and followed to reflect each error-reduction decision.

To minimize operator-related errors and to promote uni- farm measurement practices, NDA instruments used for fixed- station operations should be automated to control (1) data acquisition and analysis, (2) diagnostic testing of instrument performance stability and calibration validity, and (3) calcu- lation of associated error estimates. It is recognized that, for some less complicated NDA measurements, consistency of operation may be achieved through the implementation of carefully written and tested standard operating procedures.

Instruments should be tested to ensure that they meet procurement specifications prior to calibration.

3. OPERATORS

Adequate operator qualification requirements are crucial to proper calibration and effective measurement control of an NDA instrument. The qualification require- ments should include a general knowledge of the assay technique being used and an understanding of the typical behavior and the limitations of the instrument and the technique. A knowledge of the external factors to which the measurement technique is sensitive (factors such as matrix composition, background, material forms, and container type) is also necessary. Only then can proper standards be chosen for calibration and measurement control data be interpreted effectively.

If the operators have only a general knowledge of external factors, the NDA measurement program must be overseen by a director with a detailed knowledge of all related factors. Only qualified operators should be permit- ted to make SNM assays.

4. STABILITY TESTING

A preventive maintenance program should be devised and implemented to ensure the long-term stability and reliability of each instrument.

As part of an ongoing program of measurement control, more working standards 3 should be fabricated to period-

3Working standards are used to check the performance of an NDA instrument. They should be nominally representative of the items to be assayed. They should be fabricated and handled to ensure their internal integrity so that deviations in the measured response of the assay system can be attributed to the instrument.

As stated in ANSI Ni5.20-1975, working standards built to meet these requirements are not acceptable as calibration standards.

Calibration standards are defined in ANSI N15.20-1975 as "physically and chemically similar to the items to be assayed, for which the mass of the nuclide(s) of interest and all properties to which the measurement technique is sensitive are known." Calibration standards can be used as working standards, but working standards cannot be used as calibration standards. When calibration standards meet thle requirements for working standards, licensees may elect to maintain only calibration standards. However, calibration standards may deteriorate through extensive use or may be prohibitively expensive for stability monitoring purposes.

ically test the performance stability of the instrument.

Each working standard should contain a different amount of the species of SNM to be assayed. Current licensing review criteria require the use of four working standards.

On a rotating basis, one or two of these standards are used to check the system each day.

It should be noted that, in general, a working standard need not be fabricated from the same type of material being assayed. Even a material from a different radioactive species may be acceptable if carefully chosen and pre- pared. The essential requirements for a working standard are that (1) the radiation characteristics of the working stan- dard are sufficiently stable to ensure that fluctuations in instrument response during measurement control can con- fidently be attributed to aberrations in instrument param- eters rather than to variations in source characteristics and

(2) the working standard induces a response in the NDA

instrument that is characteristic of the expected response to real assay material. The most convenient means of achieving this "representative response" characteristic is to use mate- rial similar to the material that will be assayed.

A study should be made to determine the frequency with which the working standards are to be measured. If there is some instability, a working standard should be measured before and after each assay of an unknown item, and the calibration should be normalized to reflect the average of the before-assay and after-assay tests. In general, excessive instabilities should not be tolerated;

they should be remedied by frequent recalibration. If instabilities persist, an alternative technique, an alternative instrument, or another measurement environment should be sought. In any case, a working standard should be measured a minimum of twice per shift, once at the beginning of the shift and again at some random time during the shift.

As a general principle, working standards should be run with a frequency directly proportional to the frequency of measurements (i.e.,

increase as the measurement frequency increases and decrease as the measurement frequency decreases). Also, the quantity of SNM in the standards measurements should closely follow the quanti- ties of SNM being measured (ie., the frequency of high- SNM-content working standards measurements increases as the frequency of assays of like items increases). These procedures provide a useful estimate of the bias when determined at the end of the inventory period. In addition, working standards should be run frequently enough for each measurement system so that no one system could contribute excessively to the inventory difference (ID) by being out of control for an extended period. A minimum of 16 control measurements should be made per material balance period. Assuming two systems having equal material flows in SNM quantity and number of items, the system with the greater uncertainty per measurement should run more working standards to reduce its potential impact on the ID.

Each response to a working standard should be compared to the previous calibration data as well as to the mean value

5.53-2

of previous measurements of that working standard (under the same calibration) that were accumulated during the preceding material balance period. The difference should be plotted on a control chart. Control chart limits should be established at 0.05 and 0.001 levels of significance. When- ever control data exceed the 0.05 control limits, the test should be repeated. Whenever the control data exceed the

0.001 control limits, normal assay operations should cease.

Normal operations should not resume until the out-of- control performance has been remedied and the instrument has been recalibrated.

The control chart of the working standard responses should be examined at frequent intervals to detect indica- tions of drift, which should be compensated. The frequency for such examinations should be determined by the operat- ing characteristics of each instrument. The minimum frequency for examining the control chart of a regularly used instrument for indications of drift should be once per week.

5. CALIBRATION

Calibration of NDA instruments should be accomplished by measuring the response to calibration standards as described in ANSI N15.20-1975.

The nuclear material content of these standards should be characterized through established assay procedures (e.g., chemical assays) that are calibrated relative to national standards or nationally accepted measurement systems. The calibration standards should represent the unknown items in all physical and chemical characteristics that affect the response of the instrument. Calibration data should be obtained by averag- ing the responses from repeated measurements of the calibration standards and should be corrected to remove observed nonrandom variations.

Recalibration of an instrument is required following repair or replacement of parts if measurement of one or more working standards shows the instrument response to have changed. In addition, the calibration should be checked following a power outage or any unusual mechanical or electrical shock to the system. Recalibration data are also required if the characteristics of the items to be assayed change to the extent that previous calibration standards no longer adequately represent the unknown items.

Criteria for segregating and packaging different forms of SNM should be developed and implemented. Each material category should be established to enhance assay perform- ance, consistent with safety requirements and subsequent processing needs. Guidance for material categorization is provided in Regulatory Guides 5.11, "Nondestructive Assay of Special Nuclear Material Contained in Scrap and Waste," 2 and 5.34, "Nondestructive Assay for Plutonium in Scrap Material by Spontaneous Fission Detection." 4 For all categories of materials to be assayed, with the exception of small-content miscellaneous categories (e.g.,

4A proposed revision to this guide has been issued for comment as Task SG 046-4.

furnace liner bricks, contaminated tools, or machine parts),

the calibration relationship should be determined by a suitable method such as a least-squares fit to an appropriate function as described in ANSI N15.20-1975. The graphical calibration method is acceptable only for miscellaneous categories of material that contain a total of no more than

0.1 effective kilograms of SNM in each category during a material balance period. The combined contribution from all assays calibrated through the graphical method should be less than 10 percent of the total plant standard error (estimator) of inventory difference (SEID).

6. CALIBRATION STANDARDS

Calibration standards should be obtained to serve as the basis for the initial calibration of each instrument for each separate measurement technique or category of material.

The number of standards in each set should be greater than the number of free parameters in the calibration function for that set. It is recognized that, in some special cases, one set of calibration standards may suffice for more than one measurement technique or material category with proper analysis of the raw calibration data. Furthermore, if the NDA instrument is intended for use over a very narrow range of SNM loadings, a more restricted range of SNM

content in the calibration standards (confined to bracket the expected assay range) would prove adequate. The calibration standards should be completely characterized, including the mass and isotopic composition of the species of SNM to be assayed and all physical or chemical variables to which the response of the instrument is sensitive.

In general, the mass of SNM contained in the standards should extend over the range of loadings encountered in routine assays. This is especially true for NDA instruments whose responses are not linear functions of SNM content (e.g., some neutron-based NDA instruments). However, if the assay response (after application of appropriate correc- tions) is known to be highly linear and to have zero offset (i.e., zero response for zero SNM content), it may be more advantageous to avoid using standards with low loading, where calibration precision would suffer because of low count rates. In such a case, calibration in the upper half of the range of expected SNM loadings, combined with the constraint of zero response for zero loading, can produce a higher precision calibration than a least-squares fitting of measured responses to the standard over the full range of expected loadings, including values at low concentrations of SNM. If such a calibration procedure is used, careful initial establishment of the zero offset and instrument linearity followed by occasional verification of both assumptions is strongly recommended.

Such verification could be accomplished by an occasional extended measurement of a low-loading standard.

Unless isotopic composition is being measured, the isotopic composition of the material used in all calibration standards should be similar to the isotopic composition of the material being assayed. This is especially important for

5 The term "effective kilogram" is defined in paragraph 70.4(t)

of 10 CFR Part 70.

5.53-3

assays employing passive neutron coincidence counting or calorimetry. When the isotopic composition changes so that the response per gram of SNM differs by 10 percent or more from the value of the calibration standards, the material should be identified as a new material category.

The NDA system should be recalibrated for that category using new calibration standards made up using the new isotopic composition. When the change in response per gram is less than 10 percent, a bias correction should be determined and applied to the assay data.

The uncertainty in the bias correction should be deter- mined and accounted for in estimating the total assay uncertainty. Appropriate error propagation procedures are described in Regulatory Guide 5.18, "Limit of Error Concepts and Principles of Calculation in Nuclear Materials Control."

When the response is sensitive to ingrowth or decay of a daughter product, the procedures described in the preced- ing paragraphs are appropriate and should be applied.

Once fabricated, the calibration standards should be handled with extreme care to attempt to ensure that the distribution of contents remains fixed. It should be noted that solution standards lose their integrity over time because of evaporation and diffusion (Ref. 2) and radiolysis (Ref. 3).

Calibration standards prepared by the mixing of different powders or densities tend to stratify or segregate. The containers should be tumbled periodically to reblend the constituents. Calibration standards should be used only when developing the initial calibration or when recalibrat- ing the instrument following a repair or power outage.

Working standards should be used to test the continued stability of the instrument (see footnote 3).

The degree of effort that should be expended in fabricat- ing the calibration standards depends on the method used to estimate the assay uncertainty, as described in the next section.

7. METHODS FOR ESTIMATING UNCERTAINTY

Instrument errors associated with NDA should be estimated periodically by means of replicate assays as described in ANSI N15.20-1975.

Three methods are acceptable to estimate the uncertain- ties associated with calibrations and bias corrections for NDA. The first two procedures, graphical estimation and analytical estimation through the calibration relationship, are detailed in ANSI N15.20-1975. The third procedure, comparative evaluation, is not described in the standard.

7.1 Graphical Estimation Use of the graphical error estimation technique should result in a conservative error estimate that is acceptable for miscellaneous unusual assay categories, as described in Regulatory Position 5 of this guide.

7.2 Analytical Estimation Through the Calibration Relationship When the calibration standards can be shown to represent adequately the unknown items, the bias associated with the NDA of an inventory of items can be estimated through the calibration relationship as demonstrated in ANSI N15.20-

1975Property "ANSI code" (as page type) with input value "ANSI N15.20-</br></br>1975" contains invalid characters or is incomplete and therefore can cause unexpected results during a query or annotation process.. The calibration standards should be fabricated from different batches of material The uncertainty associated with the content of SNM elements and response-related isotopes contained in each calibration standard should be based on an extensive characterization as described in ANSI N15.20-1975. The uncertainty associated with the, contained mass of the response-related isotopes should be included in the calibration as described in the standard.

Further, the element uncertainty should be factored into the estimated total assay uncertainty.

Using this procedure, it is necessary to periodically ensure that the calibration standards adequately represent the unknown items. This can be accomplished by isolating and characterizing the extraneous interference factors that affect the response of the instrument. Typically, this separation and characterization is most easily accomplished when the items are either finished fuel items or uniform containers of feed or intermediate product material.

To ensure that the calibration standards continue to adequately represent unknown items, key parameters6 that affect the observed response (i.e., item-to-item variations)

should be monitored through separate tests. Measurements of the key parameters should be compiled and analyzed at least twice a month to catch any large instrument drift. For more timely measurement control, a superior approach would be to perform such analyses on a continuing basis and repeat measurements of unknowns where standards exceed control limits. This latter approach minimizes the backfitting of measurement data and provides a timely basis for measurement control.

When the mean value of a parameter shifts from its previously established value, the impact of the shift on the response of the assay instrument should be measured through an appropriate experiment or calculation (Ref. 4).

An appropriate bias correction should be determined and applied to all items that were assayed after the best estimate of when the parameter changed. The uncertainty in that bias estimate should be combined with the uncertainty in the assay values as predicted through the calibration function to estimate the total assay uncertainty.

The uncertainty due to a bias correction may significantly increase the standard error of the assay. In severe cases,. the effect may increase the SEID above the level acceptable for the total plant. In such cases, new calibration standards should be obtained and the assay system should be recali- brated.

6 See Section 5.4 of ANSI N15.20-1975.

See Regulatory Posi- tion 6 of this guide for provisions to include the effects of changing isotopic compositions.

5.53-4

As a further check on the continued validity of the cali- bration standards, a program to periodically introduce new calibration standards should be implemented. The rate of replacement of standards with fresh material depends on the intrinsic durability and stability of the standard in question. Some solution standards lose their calibrated concentration values in a matter of days or weeks. On the other hand, standard fuel rods are much more durable and may last indefinitely with careful handling. In any case, calibration standards should be replaced with new standards at a rate sufficiently above their failure rate to ensure continued high quality in the instrument calibration.

7.3 Comparative Evaluation The procedure described in this section is not included in ANSI N15.20-1975 but is appropriate for determining the validity of the calibration of NDA instruments.

When two measurement methods are used for each of a series of items and one of the methods is considerably more accurate than the other, corresponding measurements can be usefully compared. The comparison can be used to establish an estimate of bias between the measurement methods. The comparison can also be used to estimate the total uncertainty associated with the less accurate measure-

  • ment method.

To determine the uncertainty associated with the NDA

of an inventory of items using this method, unknown items should be randomly selected for comparative measurements.

The SNM content of the items selected should span the range of contents normally encountered, subject to the qualification pointed out in Regulatory Position 6. Random error should be estimated through replicate analyses. To estimate the remaining contributions to the total assay uncertainty, each item should be repeatedly assayed to reduce the random assay error to less than 10 percent of the estimated or previously established total uncertainty.

Then, to determine the SNM content of each item selected for comparative evaluation, one of the following procedures should be employed:

1. Each item should be completely dissolved, independ- ently, and the resulting solution should be analyzed by high-accuracy elemental and isotopic assay procedures, which in turn are calibrated relative to national standards or nationally accepted measurement systems. It should be recognized that dissolution residues may be present in such a procedure. These residues should also be assayed for a complete analysis. Items composed of an aggregate of similar units, e.g., fuel rods containing discrete pellets, should be opened and the contained units should be weighed, pulverized, blended, and sampled for assay through appro- priate high-accuracy elemental and isotopic assay proce- dures. The emptied container should be examined for indications of residual accumulations and cleaned, leached, or assayed nondestructively to determine the residual SNM

content.

2. For plutonium-bearing items only, each item can be assayed through calorimetric procedures (see Reference 5).

Large items should be subdivided into smaller containers.

Each small container should be assayed calorimetrically.

Samples should be taken from at least three of the smaller containers. The samples should be measured by micro- calorimetry and then assayed through highly accurate elemental and isotopic procedures that, in turn, are calibrated relative to national standards or nationally accepted measure- ment systems (Ref. 6). The isotopic measurement data should be examined for evidence of nonhomogeneous isotopic content. Isotopically nonhomogeneous materials should be blended and reanalyzed. On the basis of the average grams of plutonium per watt of the samples meas- ured by microcalorimetry, the total amount of plutonium in each of the smaller containers should be determined. The total plutonium content of the items selected for compar- ison is then estimated as the combined contents of the smaller containers.

For the first full material balance period during the initial implementation of this guide, two items from each category of assay items should be randomly selected each week for a check of the validity of the instrument cali- bration. Following this initial implementation period, licensees may reduce the verification measurement frequency to two items per month per category. When fewer than 100

new items of a given category are created per week, at least two of the item-comparison verification measurements should be made per material balance period per category through the procedures described above. In such cases, to provide an adequate data base to update the uncertainty estimates for NDA, licensees may pool the verification data provided the measurements are in statistical control, i.e.,

when repeated samples from the portion of the measure- ment system under test behave as random samples from a stable probability distribution. Under such conditions, data sets may be combined provided the parameters based on the current set of data and the previous set of data are not significantly different on the basis of acceptable statistical tests.

As an alternative to this selection criterion, licensees may elect the latter frequency for a specific category when it can be demonstrated that the contribution to the SEID

from that category is less than 100 grams in any mate- rial balance period.

At the close of the reporting period, differences between assay values and verification values should be recorded and tested for outliers. Methods for detecting outliers are described in ANSI/ASTM E 178-80, "Practice for Dealing with Outlying Observations."'7 See also Regulatory Guide 5.36,

"Recommended Practice for Dealing with Outlying Observa- tions," for further details.

7 Copies may be obtained from the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pennsylvania 19103.

5.53-5

A straight line with a nonzero intercept should be fitted to the nondestructive assay vs. verification measurement data as described in ANSI N15.20-1975. The slope and intercept should be jointly tested for one and zero, respec- tively, using the "F" ratio at the 5 percent significance level (Ref. 7). If this result is significant, separate tests on the slope equal to one and the intercept equal to zero should be made to determine the presence of either proportional or constant bias or both. When bias is indicated, the assay results during the preceeding operating period should be corrected. The variance associated with the bias corrections should be estimated by the standard error of estimate of the verification line. This variance must be included in the estimate of the variance of an assay result as described in ANSI N15.20-1975.

Whenever a bias exceeding 50 percent of its estimated uncertainty is indicated, its cause should be investigated.

This investigation should include a review of the assump- tions factored into the NDA system's calibration. In partic- ular, instrument stability and the stability of parameters that may influence the response of the assay system should be investigated. The investigation should also address the comparative measurement method, including sampling, sample handling, analytical procedures, interference com- pensation, and calibration validity. Results from the investi- gation, if they show the NDA system to have been incorrectly calibrated, should be employed to recalibrate the instrument for the forthcoming material balance period. Conversely, when the source of bias can be attributed to errors in the comparative measurements, bias corrections should not be made to the items assayed by NDA. Results from such investigations should be documented, and the documents should be maintained in accordance with Regulatory Position 8 of this guide.

8. RECORDS RETENTION

All records generated in connection with the activities discussed in this guide, including control charts, should be retained for a period of 5 years, as specified in para- graph 70.5 1(e)(4)(iii) of 10 CFR Part 70.

5.53-6

REFERENCES

1. T. E. Shea, "Reduction, Control, and Estimation of Nondestructive Assay Errors," Nuclear Materials Manage- ment, Vol. III, No. 3, 1974.

2. G. J. Curtis, J. E. Rein, and S. S. Yamamura, "Compara- tive Study of Different Methods of Packaging Liquid Reagents," Analytical Chemistry, Vol. 45, No. 6, p. 996,

1973.

3. J. R. Weiss and E. E. Pietri, "Calculation of Hydrogen Generation from Pu-Induced Alpha Radiolysis of Nitric, Sulfuric, and Perchloric Acids," Radiation Effects, Vol.

19, p. 191, 1973.

4. R. A. Forster, D. B. Smith, and H. 0. Menlove, "Error Analysis of a Cf-252 Fuel-Rod-Assay System," Los Alamos Scientific Laboratory, LA-5317, 1974.

S. U.S.

Nuclear Regulatory Commission, "Calorimetric Assay for Plutonium," NUREG-0228, 1977.

6. F. S. Stephens et al., "Methods for the Accountability of Plutonium Dioxide," U.S. Nuclear Regulatory Com- mission, WASH-1335, 1975.

7. F. A. Graybill, An Introduction to Linear Statistical Models, McGraw-Hill, New York, Vol. 1, p. 128, 1961.

5.53-7

BIBLIOGRAPHY

Alvar, K., H. Lukens, and N. Lurie, "Standard Containers for SNM Storage, Transfer, and Measurement," U.S. Nu- clear Regulatory Commission, NUREG/CR-1847, 1980.

This report details the variations of container properties (especially wall thicknesses) and their effects on NDA measurements. A candidate list of standard containers, each sufficiently uniform to cause less than 0.2 percent variation in assay results, is given, along with comments on the value and impact of container standardization.

Brouns, R. J., F. P. Roberts, and U. L. Upson, "Considera- tions for Sampling Nuclear Materials for SNM Accounting Measurements,"

U.S. Nuclear Regulatory Commission, NUREG/CR-0087, 1978.

This report presents principles and guidelines for sampling nuclear materials to measure chemical and isotopic content of the material. Develop- ment of sampling plans and procedures that maintain random and systematic errors of sampling within acceptable limits for SNM

accounting purposes are emphasized.

Cooper, B. E., Statistics for Experimentalists, Pergamon Press, New York, 1969.

This book provides a complete discussion of statistical procedures and describes a variety of statistical tests of experimental data. Examples are provided.

Reilly, T. D., and M. L. Evans, "Measurement Reliability for Nuclear Material Assay," Nuclear Materials Manage- ment, Vol. VI, No. 2, 1977.

This paper provides an overview of experience in nuclear material assay by analytical chemistry, calorimetry, and nondestructive assay. Ranges of accuracy and precision obtained in the assay of nuclear material are given.

Sher, R., and S. Untermeyer, The Detection of Fissionable Materials by Nondestructive Means, American Nuclear Society Monograph, 1980.

This book contains a helpful overview of a wide variety of nondestructive assay techniques for special nuclear material. In addition, it contains a rather extensive discussion of error estimation and measurement control techniques, as well as a presentation on measurement statistics.

5.53-8

VALUE/IMPACT STATEMENT

1. PROPOSED ACTION

1.3.4 Public

1.1 Description No impact on the public can be foreseen.

Licensees authorized to possess at any one time more than one effective kilogram of special nuclear material (SNM) are required in paragraph 70.5 8(f) of 10 CFR Part 70

to establish, maintain, and follow a program for the main- tenance of acceptable measurement quality in terms of measurement bias and for the evaluation and control of the quality of the measurement system.

This guide describes methods and procedures acceptable to the NRC staff for meeting the provisions of para- graph 70.58(f) of 10 CFR Part 70 for nondestructive assay (NDA) systems.

The proposed action would revise the guide, which is still basically sound.

1.2 Need The regulatory guide endorses ANSI N15.20-1975,

"Guide to Calibrating Nondestructive Assay Systems."

This standard was reaffirmed without modification in 1980

and the regulatory guide should be revised to indicate this.

Further, revisions are needed in some sections to make the guide clearer and more consistent with current thinking.

This proposed action is needed to bring Regulatory Guide 5.53 up to date.

1.3 Value/Impact

1.3.1 NRC

The regulatory positions will be brought up to date.

1.3.2 Other Government Agencies Not applicable.

1.3.3 Industry Since industry is already applying the methods and procedures discussed in the guide, updating these should have no adverse impact.

1.4 Decision The guide should be revised to reflect the affirmation of ANSI N15.20-1975 in 1980 and to make it more consistent with current usage.

2. TECHNICAL APPROACH

Not applicable.

3. PROCEDURAL APPROACH

Of the procedural alternatives considered, revision of the existing regulatory guide was selected as the most advanta- geous and cost effective.

4. STATUTORY CONSIDERATIONS

4.1 NRC Authority Authority for the proposed action is derived from the Atomic Energy Act of 1954, as amended, and the Energy Reorganization Act of 1974, as amended, and implemented through the Commission's regulations, in particular § 70.51 of 10 CFR Part 70.

4.2 Need for NEPA Assessment The proposed action is not a major action that may significantly affect the quality of the human environment and does not require an environmental impact statement.

5. RELATIONSHIP TO OTHER EXISTING OR

PROPOSED REGULATIONS OR POLICIES

The proposed action is one of a series of revisions of existing regulatory guides on nondestructive assay techniques.

6. SUMMARY AND CONCLUSIONS

A revised guide should be prepared to bring Regulatory Guide 5.53 up to date.

5.53-9

UNITED STATES

NUCLEAR REGULATORY COMMISSION

WASHINGTON, D.C. 20555 FIRST CLASS MAIL

POSTAGE & FEES PAID

USNRC

WASH

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PERMIT No _E

OFFICIAL BUSINESS

PENALTY FOR PRIVATE USE. $300