Regulatory Guide 5.58

Considerations for Establishing Traceability of Special Nuclear Material Accounting Measurements

ML13350A228
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Issue date:	11/30/1978
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RG-5.058
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C." Clt RIC.

U.S. NUCLEAR REGULATORY COMMISSION

November 1978

0

• REGULATORY

GUIDE

,"

OFFICE OF STANDARDS DEVELOPMENT

REGULATORY GUIDE 5.58 CONSIDERATIONS FOR ESTABLISHING TRACEABILITY OF SPECIAL

NUCLEAR MATERIAL ACCOUNTING MEASUREMENTS

A. INTRODUCTION

assigned value 3 is known relative to national stand- ards or nationally accepted measurement systems.

Part 70, -Domestic Licensing of Special Nuclear Material," of Title 10 of the Code of Federal Regu- This guide presents conditions and procedural ap- lations requires that for approval to possess and use proaches acceptable to the NRC staff for establishing more than one effective kilogram of special nuclear and maintaining traceability of SNM cpntrol and material (SNM)' the licensee must provide proper accounting measurements. No speci ethods will physical security and an adequate material control be presented herein since the methio o- to be used and accounting system. Section 70.51, "Material Bal- for any given measurement musThe tai-'

d to the ance, Inventory, and Records Requirements,- re- needs and peculiarities of t proc's mate quires licensees to calculate material unaccounted for rial, reference standarW in

.enon, and cir- (MUF) and the limit of error of the MUF value cumstance

s. Rationat

"a p

analytical fac- (LEMUF) following each physical inventory and to tors will be pr te copsp ration as to their compare the LEMUF with prescribed standards. Sec- applicability to

.ea. *.,It at hand.

tion 70.58, "Fundamental Nuclear Material Con- trols," requires licensees to maintain a program for CUSSION

the continuing determination of systematic and ran- o W

i]

,

ld dom measurement errors and for maintaining control O

of such errors within prescribed limit

s. Section

,

"asurements for control and accounting are

70.57, "Measurement Control Program for Spe'%

ed on a great variety of material types and Nuclear Materials Control and Accounting,C

o c

entrattons, with a diversity of measurement pro- vides criteria for establishing and maiu.ai*, an j cedures, by a large number of licensees at all the acceptable measurement and control sys *'IX"*

various industrial, research and development, and Implicit in the criteria stated in §

57I the academic facilities involved. A way of linking all requirement of traceability of all SNM

and these measurements and their uncertainties to the reqountingrementof traceablityo N

nall San- NMS is necessary to achieve valid overall accounta- accounting measurements tTo this end all measurement systems must be ment System (NMS) b t'kns of reference stand- b

il e with end, all measurement ards. Traceability me .

' Ibility to relate indi- compatible with the NMS, and all measurement vidual measure,,s.. s to ational standards or results must be traceable to the appropriate national nationally acc ted m s

,' ent systems through an (primary) reference standards or Primary Certified unbrokeniRai f con arisons, and reference stand- Reference Materials (PCRMs). To obtain this neces- rdm-*

device, or inssary compatibility for any given SNM measurement task, secondary (intermediate, working) reference

__

_

standards or Secondary Certified Reference Materials

'For definitlns, see paragraphs 70.4(m) and (t) of 10 CFR

(SCRMs) appropriate for each SNM type and meas- Part 70.

urement system are nearly always require

d. Table I

'The listed regulations do not apply to special nuclear defines the various types of reference materials.

materials involved in the operation of a nuclear reactor, in waste disposal operations. or as scaled source

s. See paragraphs

3The term "value"

includes instrumental response and other

70.51(e). 70.57(b), and 70.58(a) of 10 CFR Pan 70.

pertinent factors.

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20O6, Attention:

ODrector.

Division of particularly useful In evaluating the need for an early revision.

Technical Information and Document Control.

Traceability is a property of the overall measure- ment, including all Certified Reference Materials (CRMs), instruments, procedures, measurement con- ditions, techniques, and calculations employed. Each component of a measurement contributes to the un- certainty of the measurement result relative to the NMS. The NMS itself comprises a number of com- ponents, including Standard Reference Materials (SRMs) or PCRMs, national laboratories, calibration facilities, and standard-writing groups. If the NMS is viewed as an entity capable of making measurements without error, traceability can be defined as the abil- ity to relate any measurement made by a local station (e.g., licensee) to the "correct" value as measured by the NMS. If it were possible for the NMS to make measurements on the same item or material as the local station, this relationship, and hence traceability, could be directly obtained. Since the NMS is largely an intangible reference system, not a functioning entity, such direct comparisons are not ordinarily possible, and alternative means for achieving traceability must be employed. This neces- sary linkage of measurement results and their uncer- tainties to the NMS can be achieved by:

a. Periodic measurements by the licensee of SRMs or PCRMs whose assigned values and uncertainties have been certified by the National Bureau of Stand- ards (NBS). These measurements may include inter- national reference materials whose assigned values have been approved and accepted by the NBS. This option applies only if the materials to be measured have a substantially identical effect upon the meas- urement process as do the reference materials (RMs)

or if the difference is relatively small and easily correctable by means of the known effects *of all interfering parameters. Also, of course, the meas- urement of the RMs must be performed in a manner identical to that employed for the SNM measurements (see Section B.3.1 of this guide).

Table 1 TYPES OF REFERENCE MATERIALS

Definition RM Type and Abbreviation Examples Reference Material (RM)

Certified Reference Material (CRM)

Primary Certified Reference Material (PCRM)

Secondary Certified Reference Material (SCRM)

Working Reference Material (WRM)

A general term that is recom- mended as a substitute for that which previously has been re- ferred to as a standard or standard material.

A general term for any PCRM or SCRM or these materials as a group.

A stable material characterized, certified, and distributed by a national or international standards body.

An RM characterized against PCRMs, usually by several lab- oratories.

Unlike PCRMs, SCRMs can be typical, somewhat less stable materials.

An RM derived from CRMs or characterized against CRMs, used to monitor measurement methods, to calibrate and test methods and equipment, and to train and test personnel.

Any or all of the materials listed below.

Any PCRM or SCRM or these materials as a group. See ex- amples below.

Standard Reference Materials of the National Bureau of Standards (NBS SRMs) and Standard Mate- rials of the International Atomic Energy Agency (IAEA) bearing the IAEA classification, S.

Reference Materials available from New Brunswick Laboratory (NBL) or from IAEA. Those from the latter bear the IAEA

classification, R.

Process stream materials and any RM prepared according to this and related reports.

5.58-2

b. Periodic measurements of well-characterized process materials or synthesized artifacts that have been shown to be substantially stable and either (a)

homogeneous or (b) having small variability of known limits. The uncertainties (relative to the NMS)

associated with the values assigned to such process materials or artifacts are obtained by direct or indirect comparisons with PCRMs or NBS SRMs.

c. Periodic submission of samples for comparative measurement by a recognized facility having estab- lished traceability in the measurement involved, employing one or both of the above procedures, and involving only samples not subject to change in their measured values during storage or transit.

("Round-robin" sample exchanges between facilities can be useful in confirming or denying compatibility of results, but such exchanges do not of themselves constitute the establishment or maintenance of traceability.)

Valid assignment of an uncertainty value to any measurement result demands a thorough knowledge of all the observed or assigned uncertainties in the measurement system, including an understanding of the nature of the sources of these uncertainties, not just a statistical measure of their existence. It is not sufficient, for example. to derive a root-mean-square value for a succession of observed or assigned un- certainties (CRM, instrumental, and procedural) for which standard deviation values have been calculated by statistical methods for random events. To do so involves assumptions as to the randomness of these variances that may not be at all valid. The variances may, in faci. be due to a combination of systematic errors that appear to be randomly distributed over the long run but that are not at all random in their occurrence for a given analyst employing a given combination of standards, tools, and instrumental components. Thus, it is necessary to derive the un- certainty value of a measurement from methods that also involve a summation of the nonrandom (sys- tematic) uncertainties, not from the mathematics of random events alone. The valid determination of the uncertainty of a measurement relative to the N MS.

and thus of the degree of traceability, is not a rigorous procedure hut is the result of sound judg- mtent based on thorough knowledge aul understand- ing of all factors involved.

Obviously, the sources of systematic error can be reduced if the Working Reference Materials (WRMs)

are included at least once in every series of related measurements by a given analyst and combination of tools, instruments, and conditions. The calibration and correlation factors so obtained cannot be applied uncritically to successive measurements. It also fol- lows that the applicability of any given RM to a series of measurements of process material should be examined critically both periodically and with every change or hint of change in the measurement charac- teristics of the process material.

It is doubtful that the WRMs can ever be exact representations of the material under measurement in any given instance, even for highly controlled proc- ess materials, such as formed fuel pieces or uniform powdered oxide, shown to be substantially uniform in both composition and measurement-affecting physical characteristics (e.g., density or shape for nonde- structive assay (NDA) measurements). However, in most cases RMs that yield measurement uncertainties within the selected limits for the material in question can be achieved. Obviously, the errors resulting from mismatch of the RM with the measure-d material will be largest in heterogeneous matter such as waste materials, but in these cases the SNM concentrations normally will be low and the allowable limits of uncertainty correspondingly less stringent.

The important truth being stressed here is that everyn measurement ntist be considered, in all as- pects, as an individual determination subject to error from a variety of sources, none of which mayuv be safely ignored. The all-too-natural tendency to treat successive measurements as routine must be rigor- ously avoided. Physical RMs, in particular, tend to be mistakenly accepted as true and unvarying: but they may well be subject to changes in effective value (measured response), as well as unrepresenta- tive of the samples. unless wisely, selected and carefully handled.

The characteristics required of CRMs include:

a. Sufficiently small and known uncertainties in the assigned values. (Normally, the uncertainties of the CRMs will contribute only a small fraction of the total uncertainty of the measurement.)

b. Predictability in the response produced in the measurement process. (Ideally, the measurement process will respond to the reference materials in the same way as to the item or material to be measured.

If there is a difference in measurement response to the measured parameter arising from other measurement-affecting factors, these effects must be known and quantifiable.)

c. Adequate stability with respect to all measurement-affecting characteristics of the stand- ard. (This is necessary to avoid systematic errors due to changes in such properties as density. concentra- tion, shape, and distribution.)

d. Availability in quantities adequate for the in- tended applications.

It cannot be assumed that RMs will always remain wholly stable as seen by the measurement system employed, that working RMs will forever remain representative of the measured materiel for which they were prepared or selected, or that the measured material itself will remain unchanged in its measure-

0

5.58-3

ment characteristics. Therefore, it is essential that these RMs, as well as the measurement instrumenta- tion and procedures, be subject to a program of continuing confirmation of traceability. Many of the factors involved in such a program are discussed in Reference I.L

2. Mass and Volume Measurements The national systems of mass and volume meas-

• urements are so well established that RMs meeting the above criteria arc readily available. Where neces- sary, the licensee can use the RMs to calibrate WRMs that more closely match the characteristics of the measured material in terms of mass, shape, and density in the case of mass measurements or are more easily adapted to the calibration of volume- measurement equipment.

Specific procedures for the use of mass and volume RMs for the calibration of measurement processes and equipment arc given in the corresponding ANSI

standards (Refs. 2 and 3). Factors likely to affect uncertainty levels in inventory measurements of mass and volume are discussed in other regulatory guides (Refs. 4, 5, and 6).

3. Chemical Assay and Isotopic Measurements Methods for chemical analysis and isotopic meas- urement often are subject to systematic errors caused by the presence of interfering impurities, gross dif- ferences in t(ie concentrations of the measured com- ponent(s) or of measurement-affecting matrix mate- rials, and other compositional factors. Traceability in these measurements can be obtained only if such effects are recognized and either are eliminated by adjustment of the RM (or sample) composition or, in some cases, are compensated for by secondary meas- urements of the measurement-affecting variable com- ponent(s) and corresponding correction of the meas- ured SNM value. The latter procedure involves addi- tional sources of uncertainty and therefore should be employed only if it has a substantial economic or time advantage, if the interferences or biasing effects are small and limited in range, if the corrected method is reliable, and if the correction itself is verifiable and is regularly verified.

3.1 National Standards - Uses and Limitations NBS SRMs generally are not recommended for use directly as WRMs, not only because of cost and required quantities but also because of differences in composition (or isotopic ratios) compared to the process materials to be measured. NBS SRMs are more often used to prepare synthesized intermediate RMs of composition and form matching the process

'Regulatory guides under development on measurement con- trol progrdms for SNM accounting and on considerations for determining the systematic error and the random error of SNM

accounting measurements will also discuss the factors involved in a program of continuing confirmation of traceability.

material or to evaluate (and give traceability to)

non-NBS but substantially identical material from which matching WRMs are then prepared. This is necessary because of both the wide diversity of proc- ess materials encountered and the very small number and variety of SNM SRMs available. These inter- mediate RMs may be used directly as WRMs, if appropriate, or may be reserved for less frequent use in the calibration of suitable synthetic or process- material WRMs of like characteristics, as well as for verifying instrumental response factors and other as- pects of the measurement system. However, each level of subsidiary RMs adds another level of uncer- tainty to the overall uncertainty of the SNM meas- urement.

SRMs can also be used to "spike" process sam- ples or WRMs to determine or verify the measurabil- ity of incremental changes at the working SNM level.

However, because of possible "threshold" or "zero error" effects and/or nonlinearity or irregularity of measurement response with concentration, this pro- cess does not of itself establish traceability.

3.2 Working Reference Materials WRMs that closely match the effective compo- sition of process material, or a series of such WRMs that encompass the full range of variation therein, serve as the traceability link in most chemical analy- sis and isotopic measurements. The WRMs derive traceability through calibration relative to either SRMs or, more often, synthesized intermediate CRMs containing either SRMs or other material evaluated relative to the SRM (see Section B:3.1 of this guide).

The characteristics required of a WRM are that it be chemically similar to the material to be measured (including interfering substances), that it be suffi- ciently stable to have a useful lifetime, and that it have sufficiently low uncertainty in its assigned value to meet the requirements of the measurement methods and of the accountability limits of error.

WRMs can be prepared (a) from process mate- rials characteristic of the material to be measured or (b) by synthesis using known quantities of pure SNM. The former method offers the advantage that the WRM will include all the properties that can affect the measurement such as impurities, SNM

concentration level, and chemical and physical form;

it suffers from the disadvantage that the assigned value is determined by analyses subject to uncertain- ties that must be ascertained. The latter method in- volves preparations using standard reference material (not usually economical unless small amounts are used) or SCRMs (see Section B.3.1) with the appro- priate combination of other materials to simulate the material to be measured. The advantages of the latter method include more accurate knowledge of the SNM

I

5.58-4

content and better control of other variables such as the amount of impurities and the matrix composition.

The chief disadvantage is that the synthesized RM

may not possess all the subtle measurement-affecting characteristics of the process material. Moreover, the preparation of synthesized WRMs may be substan- tially more costly than the analysis of WRMs pre- pared fronh process material. Detailed procedures for preparing plutonium and uranium WRMs are de- scribed in NRC reports (Refs. 7 and 8).

The primary concern in the use of a WRM to establish traceability in SNM measurements is the validity of the assigned value and its uncertain.y.

Considerable care is necessary to ensure that the WRMs are prepared with a minimal increase in the uncertainty of the assigned value above that of the SRM upon which the WRM value is based. If the assigned value of a WRM is to be determined by analysis, the use of more than one method of analysis is necessary to enhance confidence in the validity of the assigned value. The methods should respond dif- ferently to impurities and to other compositional variations. If the WRM has been synthesized from standard reference material or from intermediate ref- erence material, the composition and SNM content can be verified by subsequent analyses.

The composition of a WRM can change with time, e.g., changes in oxidation state, crystalline form, hydration, or adsorption. These changes and their effects on measurement are minimized by ap- propriate packaging and proper storage conditions.

Additional assurance is attained by distributing pre- measured amounts of the material into individual packets at the time of preparation, and these packets can be appropriately sized so that the entire packet is used for a single calibration or test. Even among such subsamples there may be variability in SNM content, and this variability must he taken into account in determining the uncertainty of the assigned value.

3.3 Standard Laboratories and Sample Inter- change Traceability of chemical assay and isotopic anal- ysis values also may be obtainable through compara- tive analyses of identical samples under parallel con- ditions. A comparative-measurement program may take either or both of two forms:

a. Periodic submission of process samples for analysis by a recognized facility having demonstrated traceability in the desired measurement.

b. Interfacility interchange and measurement of well-characterized and representative materials with values assigned by a facility having demonstrated traceability in the measurement.

Round-robin programs in which representative samples are analyzed by a number of laboratories do not establish traceability but can only indicate inter- laboratory agreement or differences, unless tracea- bility of one or more of the samples in a set has been established as above.

4. Nondestructive Assay Nondestructive assay (NDA) measurement methods are those that leave the measured material unchanged (e.g., gamma emission methods) or with no significant change (e.g., neutron activation) rela- tive to its corresponding unmeasured state (Ref. i).

NDA offers the advantages that the same RM or the same sample can be measured repeatedly and yields valuable data on sysiem uncertainties not otherwise obtained, that the nmeasurcinent made does not con- sume process material

,Ad that measurements can be made more frequently or in greater number, usually at a lesser unit cost than destructive chemical methods. These advantages often yield better process and inventory control and enhanced statistical signifi- cance in the measurement data. However, like chemical analytical methods, NDA methods have many sources of interferences that may affect their accuracy and reliability.

In nearly all NDA methods.' the integrity and traceability of the measurements depend on the va- lidity of the RMs by which the NDA system is calibrated. Calibrations generally are based on WRMs that are or are intended to be well- characterized and representative of the process mate- rial or items to be measured. While the matching of RMs to process itoms, and consequent valid tracea- bility, is not difficult to achieve for homogeneous materials of substantially constant composition (e.g..

alloys) having fixed size and shape (e.g.. machined pieces), such ideal conditions are not obtained for most SNM measurements. Many of the materials and items encountered are nonhomogeneous, noncon- forming in distribution, size, or shape, and highly variable in type of material and composition. In order to ensure traceability of the measurement results to the NMS, variations in the physical characteristics and composition of process items and in their effects upon the response of the NDA measurement system must be evaluated and carefully considered in the selection or design of WRMs and measurement pro- cedures (Refs. 9 and 10).

WRMs usually (a) are prepared from process ma- terials that have been characterized by measurement methods whose uncertainties have been ascertained relative to the NMS (i.e., are traceable) or (b) are artifacts synthesized from well-characterized mate- rials to replicate the process material." However, calibration of the NDA method by means of such

-Absolute calorimetry of SNM of known chemical and isotopic composition is an exception.

'The advantages stated for similarly derived WRMs (see Section 8.3.2) also apply here.

5.58-5

RMs does not automatically establish continuing traceability of all process item measurement results obtained by that method. The effects of small varia- tions in the materials being assayed may lead to biased results even when the WRM and the material under assay were obtained from nominally the same process material. It therefore may be necessary either (a) to establishtraceability of process item measure- ment results by comparing the NDA measurement

.results with those obtained by means of a reliable alternative measurement system of known traceabil- ity, e.g.. by total dissolution and chemical analysis (see Section B.4.1) or (b) to establish adequate sample characterization to permit the selection of a similarly characterized WRM for method calibration (see Section B.4.2).

4.1 Traceability Assay by a Second Method Any NDA method would be of little practical use if every measurement also required a confirma- tory analysis. However, in cases in which there are a number of items or. material samples of established similar characteristics, it is practical to establish traceability for a series of measurements by means of traceable second-method evaluations of an appro- priate proportion of randomly selected samples. If the correlation between the two methods is then found to be consistent, tracedbility is established for all NDA

measurements on that lot of SNM and on other highly similar material.

For nominally uniform process or production material of which multiple subsamples can be ob- tained from a gross sample. the uniformity can be deduced from the distribution of the NDA measure- ment data. For thus characterized material, traceabil- ity can be established for all subsamples that ap- proximate the mean7 from the separate traceable second-method analysis of a few of the subsamples.

Other like subsamples can then be selected as trace- able WRMs whose assigned values are related to the separately analyzed subsamples through their re- spective NDA measurement results.

For subsample populations exhibiting a range of NDA values, especially where a destructive second-method analysis is used, the "twinning"

method of sample selection may be employed. In this method, pairs of subsamples are matched by their NDA measurement values, and the matches are con- firmed by NDA reruns. One member of each pair is evaluated by the traceable second-method analysis- the other member of that pair is then assigned the

.value determined for its twin and may serve thereaf- ter as a traceable WRM for the measurement of that process material by that NDA method.

ISubsamples whose measured values markedly deviate from the mean (i.e.. "flyers") are not used for second-method

• analysis or for WRMs.

4.2 Characterization by a Second Method If the process items or materials being measured are subject to non-SNM variations that affect the SNM measurement, it may be possible to employ one or more additional methods of analysis to measure these variations and thus to characterize process ma- terials in terms of such analysis results. If the sec- ondary analyses also are by an NDA method, they may often be performed routinely with the SNM

measurements. In many cases, the results of sec- ondary analyses may be used to derive simple cor- rections to the SNM measurement results. Correction also may be obtained and traceability preserved by the judicious modification of RMs so as to incorpo- rate the same variable factors, i.e., so that they can produce the same relative effects in the SNM and non-SNM measurements as do the process vari- able(s).

Alternatively, it may be advantageous to prepare WRMs that span the normal range of variability of the measurement-affecting non-SNM parameter(s)

(and also the SNM-concept range, if appropriate).

These standards can then be characterized on the basis of their non-SNM measurement results or of some function(s) of SNM and non-SNM measurement results and can be assigned a corresponding

"characteristic figure. ' If this procedure can be car- ried out with adequate sensitivity and specificity rel- ative to the interfering factors, and within acceptable limits of uncertainty, the process material can be routinely characterized in like manner and the appro- priate WRM selected on the basis of such characteri- zation.

5. Continuing Traceability Assurance Initial or occasional demonstration that a laboratory has made measurements compatible with the NMS is not sufficient to support a claim of traceability.

Measurement processes are by their nature dynamic.

They are vulnerable to small changes in the skill and care with which they are performed. Deterioration in the reliability of their measurement results can be caused by (a) changes in personnel performance, (b)

deterioration in or the development of defects in RMs, instrumentation, or other devices, or (c) varia- tion in the environmental conditions under which the measurements are performed. The techniques dis- cussed in preceding sections ensure traceability only if they are used *within a continuing program of measurement control.

C. REGULATORY POSITION

The measurement control. program used by the licensee should include provisions to ensure that in- dividual measurement results are traceable to the national measurement system (NMS). RMs used to establish traceability of measurement results to the NMS should have assigned values whose uncertain- ties are known relative to the NMS. To meet this condition, the licensee should maintain a continuing

0

5.58-6

program for calibrating each measurement process.

using RMs that meet the criteria in the following paragraphs.

1. Reference Materials

1.1 The National Bureau of Standards Devices, instruments, and materials calibrated or approved by the NBS are acceptable RMs' for calil brating either methods or WRMs. However, it is very important that the licensee be able to demonstrate that the RMs are stable under the conditions for which they are used, that their validity has not been com- promised, and that they meet the accuracy require- ments of the intended applications.

1.2 Secondary Certified Reference and Work- ing Reference Materials Lower-order SCRMs or WRMs that have been produced by the licensee or by a commercial supplier are acceptable provided their uncertainties relative to PCRMs are known.

A statement of uncertainty should be assigned to each RM based on an evaluation of the uncertainties of the calibration process. The statement should con- tain both the standard deviation and the estimated bounds of the systematic errors associated with the assigned value.

1.2. / RAfs for Chemical arnd Isotopic Analyses.

WRMs used for calibrating chemical assay and isotopic measurements may be prepared from stand- ard reference materials (SRMs) supplied by NBS or from other well-characterized materials available to the industry. Such WRMs should be prepared under conditions that ensure high reliability and should be packaged and stored in a way that eliminates any potential for degradation of the WRM.

The assigned values of WRMs prepared from process materials should be determined by analysis, using two different methods whenever possible. A

sufficient number of analyses should be done by both methods to allow a reliable estimate of the compo- nents of random variation that affect the measure- ment. If two methods are not available, as may be the case for isotopic analysis, it is recommended that a verification analysis be obtained from another lab- oratory.

If WRMs are prepared from NBS SRMs or other PCRMs, they should be analyzed to verify that the makeup value is correct. i.e., that no mistakes have been made in their preparation. For this verification, at least five samples should be analyzed, using the most reliable method available. Should the analytical results differ significantly from the makeup value.

"International RMs and reference material such as IAEA RN~s are included, if accepted by NBS.

the WRM should not be used. Typical statistical and analytical procedures acceptable to the NRC staff for preparing WRMs are found in References 7 and 8.

Storage and packaging of WRMs should follow procedures designed to minimize any changes likely to affect the validity of the assigned values. When- ever practical, the WRM should be divided into small measured quantities at the time of preparation, and the quantities should be of appropriate size so that each entir, unit is used for a single calibration or calibra- tion test.

1.2.2 Nondestructive Assay. RMs for NDA should be prepared from well-characterized materials whose SNM contents have been measured by methods that have been calibrated with CRMs or from synthetic materials of known SNM content. The NDA RMs should closely resemble in all key characteristics the process items to be measured by the system. Since destructive measurements ordinarily cannot be made on NDA RMs in order to verify makeup, as required for WRMs for chemical assay and isotopic analyses, RMs should be prepared in sets of at least three.

using procedures that guard against errors common to all members of the set. The consistency of the NDA

system response to all the RMs in the set provides a basis for judging the validity of the set of RMs. If one or more of the RMs in the set differs significantly from the expected response. no RMs from that set should be used. Statistical tests for this comparison can be found in References 7 and 8.

The design and fabrication of the RMs should take into account the measurement process parame- ters affecting the response of the system (Ref. 1).

including:

a. SNM content, b. Isotopic content, c. Matrix material, d. Density, e. Container material and dimensions, f. Self-absorption effects, and g. Absorption and moderation effects.

Studies should be carried out in sufficient detail to identify the process item characteristics and the variations of the characteristics that can cause sys- tematic error. The results of the studies should be used to establish reasonable bounds for the systematic errors.

NDA systems whose uncertainties relative to the NMS cannot be satisfactorily established directly through the calibration process should be tested by comparative analysis. This test should be done by periodically analyzing randomly selected process items with the NDA system in question and by another method with known uncertainty. The verifi- cation analysis can be done on samples obtained after reduction of the entire item to a homogeneous form.

In some cases, verification analysis by small-sample

5.58-7

NDA- or by other NDA methods may be acceptable if the uncertainties of the verification method are known relative to the NMS.

2. Measurement Assurance Table 2 RECERTIFICATION OR REPLACEMENT

INTERVALS FOR CRMs The traceability of each measurement process to the NMS should be maintained by a continuing program of measurement assurance. This program should include planned periodic verifications of the assigned values of all RMs used for calibrations.

2.1 VerifIcition of Calibrations A formal program fixing the frequency at which calibrations and calibration checks are performed should be established. The required frequencies are strongly dependent on system sability and should be determined for each case by using historical perform- ance experience. Current performance of the meas- urement system based on measurement control pro- gram data may signal the need for more frequent verifications. Also, the effects of cL'angcs in process parameters such as composition of material or mate- rial flows should De evaluated when they occur to determine the need for new calibrations.

WRMs that are subject to deterioration should be recertified or replaced on a predetermined schedule.

The frequency of recertification or replacement should be based on performance history. If the integrity of an RM is in doubt, it must be discarded or recalibrated.

2.2 Recertification or Replacement of CRMs Objects, instruments, or materials calibrated by NBS or other authoritative laboratories and used as CRMs by the licensee should be monitored by intercomparisons with other CRMs to establish their continued validity. In any case, the values should be redetermined periodically according to Table 2.

Test Objects and Devices Mass Length Volumetric Provers Thermometers and Thermocouples Calorimetric Standards Certified Reference Materials Plutonium Metal (after unpacking)

U 30s (after unpacking)

Maximum Periods

5 yr

5 yr

5 yr

3 yr

2 yr

3 mo I yr

2.3 Interlaboratory Exchange Programs The licensee should participate in interlaboratory exchange programs when such programs are relevant to the types of measurements performed in his laboratory. The data obtained through this participa- tion and other comparative measurement data (such as shipper-receiver differences and'inventory verifi- cation analyses) should be used to substantiate the uncertainty statements of his measurements.

When significant deviations in the rcsults of the comparative measurements occur, indicating lack of consistency in measurements, the licensee should conduct an investigation. The investigation should identify the cause of the inconsistency and, if the cause is within his organization, the licensee should initiate corrective actions to remove the inconsis- tency. The investigation may involve a reevaluation of the measurement process and the CRMs to locate sources of bias or systematic error or a reevaluation of the measurement errors to determine if the stated uncertainties are correct.

3. Records The licensee should retain all records relevant to the uncertainty of each measurement process for 5 years. The records should include documents or certificates of CRMs, the measurement and statistical data used for assigning values to WRMs, and the calibration procedures used in preparing the WRMs.

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REFERENCES

1. Regulatory Guide 5.11, "Nondestructive Assay of Special Nuclear Material Contained in Scrap and Waste" (1973).

2. ANSI Standard N15.18, "Mass Calibration Techniques for Nuclear Material Control,"

American National Standards Institute, 1430

Broadway, New York, New York (1975).

3. ANSI Standard N15.19, "Volume Calibration Techniques for Nuclear Material Control,"

American National Standards Institute, 1430

Broadway, New York, New York (1975).

4. Regulatory Guide 5.25, "Design Considerations for Minimizing Residual Holdup of Special Nu- clear Material in Equipment for Wet Process Operations" (1974).

5. Regulatory Guide 5.42, "Design Considerations for Minimizing Residual Holdup of Special Nu- clear Material in Equipment for Dry Process Operations" (1975).

6. Regulatory Guide 5.48, "Design Consid- erations-Systems for Measuring the Mass of Liquids" (1975).

7. G. C. Swanson, S. F. Marsh, J. E. Rein, G. L.

Tietjen, R. K. Zeigler, and G. R. Waterbury,

"Preparation of Working Calibration and Test Materials-Plutonium Nitrate Solution," NRC

report NUREG-01 18 (1977).

8. S. S. Yamamura, F. W. Spraktes, J. M. Baldwin R. L. Hand, R. P. Lash, and J. P. Clark,

"Preparation of Working Calibration and Test Materials: Uranyl Nitrate Solution," NRC report NUREG-0253 (1977).

9. ANSI Standard N15.20, "Guide to Calibrating Nondestructive Assay Systems," American Na- tional Standards Institute, 1430 Broadway, New York, New York (1975).

10. Regulatory Guide 5.53, "Qualification, Calibra- tion, and Error Estimation Methods for Nondes- tructive Assay" (1975).

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