ASTM C1297-2018 Standard Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle Materials.pdf

1、Designation: C1297 03 (Reapproved 2011)C1297 18Standard Guide forQualification of Laboratory Analysts for the Analysis ofNuclear Fuel Cycle Materials1This standard is issued under the fixed designation C1297; the number immediately following the designation indicates the year oforiginal adoption or,

2、 in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This guide covers the qualification of analysts to perform chemical analysis or

3、physical measurements of nuclear fuel cyclematerials. The guidance is general in that it is applicable to all analytical methods, but must be applied method by method. Also,the guidance is general in that it may be applied to initial qualification or requalification.1.2 The guidance is provided in t

4、he following sections:SectionQualification Considerations 4Qualification Considerations 5Demonstration Process 5Demonstration Process 6Statistical Tests 6Statistical Tests 71.3 This standard does not apply to maintaining qualification during routine use of a method. Maintaining qualification isinclu

5、ded in Guide C1210.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regul

6、atory limitations prior to use.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organi

7、zation Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2C859 Terminology Relating to Nuclear MaterialsC1009 Guide for Establishing and Maintaining a Quality Assurance Program for Analytical Laboratories Within the NuclearIndustryC1068 Guide for Qualification of

8、Measurement Methods by a Laboratory Within the Nuclear IndustryC1128 Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle MaterialsC1156 Guide for Establishing Calibration for a Measurement Method Used to Analyze Nuclear Fuel Cycle MaterialsC1210 Guide for E

9、stablishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Withinthe Nuclear IndustryC1215 Guide for Preparing and Interpreting Precision and Bias Statements in Test Method Standards Used in the NuclearIndustry2.2 ISO Standard:Standards:3ISO Guide 30 Terms and Def

10、initions Used in Connection with Reference MaterialsReference materials Selected terms anddefinitionsISO Guide 33 Reference materials Good practice in using reference materials1 This guide is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycleand is the direct responsibility of Subcom

11、mittee C26.08 on Quality Assurance,Statistical Applications, and Reference Materials.Current edition approved June 1, 2011July 1, 2018. Published June 2011July 2018. Originally approved in 1995. Last previous edition approved in 20032011 asC1297 - 03.C1297 03 (2011). DOI: 10.1520/C1297-03R11.10.1520

12、/C1297-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American National Standards Instit

13、ute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequate

14、ly depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,

15、 PA 19428-2959. United States13. Terminology3.1 For definitions of terms used in this test method but not defined herein, refer to Terminology C859.3.2 Definitions of Terms Specific to This Standard:3.2.1 qualification, ndemonstration by a laboratory analyst of acceptable knowledge, skills and exper

16、ience for a specificanalytical method to generate data with the stated bias and precision as determined using guidance in Guide C1068.4. Significance and Use4.1 This is one of a series of guides designed to provide guidance for implementing activities that meet the requirements of asound laboratory

17、quality assurance program. The first of these, Guide C1009, is an umbrella guide that provides general criteriafor ensuring the quality of analytical laboratory data. Other guides provide expanded criteria in various areas affecting quality,producing a comprehensive set of criteria for controlling d

18、ata quality. The approach to ensuring the quality of analyticalmeasurements described in these guides is depicted in Fig. 1.4.2 The training and qualification of analysts is one of the elements of laboratory quality assurance presented in Guide C1009,which provides some general criteria regarding qu

19、alification. This guide expands on those criteria to provide more comprehensiveguidance for qualifying analysts. As indicated in Guide C1009, the qualification process can vary in approach; this guide providesone such approach.4.3 This guide describes an approach to analyst qualification that is des

20、igned to be used in conjunction with a rigorous programfor the qualification and control of the analytical measurement system. This requires an existing data base which defines thecharacteristics (precision and bias) of the system in routine use. The initial development of this data base is describe

21、d in GuideC1068. The process described here is intended only to qualify analysts when such a data base exists and the method is in control.4.4 The qualification activities described in this guide assume that the analyst is already proficient in general laboratoryoperations. The training or other act

22、ivities that developed this proficiency are not covered in this guide.4.5 This guide describes a basic approach and principles for the qualification of laboratory analysts. Users are cautioned toensure that the qualification program implemented meets the needs and requirements of their laboratory.5.

23、 Qualification Considerations5.1 When a qualification program is being established, consideration should be given to analyst selection criteria, the trainingprogram, and practical demonstration. knowledge requirements, practical demonstration requirements, and the training program formeeting those r

24、equirements. The criteria that govern when qualification is achieved should be documented along with methods fordetermining the knowledge and skill of the analyst.5.1.1 Analyst selection should be based on established criteria that are related to the complexity of the method that analysts areexpecte

25、d to perform. Criteria should include the minimum education required, any prerequisite training, and the overall experiencerequired. The selection criteria should be defined and documented.FIG. 1 Quality Assurance of Analytical Laboratory DataC1297 1825.1.2 The method-specific analyst training progr

26、am should be an established program with a prescribed training procedure.Some mechanism such as an oral or written test should be used to allow an analyst to demonstrate knowledge and understandingof the chemical, physical, instrumental, and mathematical concepts used to execute the method. It is ad

27、visable to monitor progressduring training to ensure that the analyst has a reasonable chance of passing the qualification test.5.1.3 The practical demonstration of the analysts ability to generate results with the analytical method should be compared toestablished criteria. The comparison criteria

28、should be defined and documented.NOTE 1The qualification of analysts, like many other laboratory processes, has the potential for undetected errors. There are two types of errors thatoccur. One is to fail an individual who should have been determined to be qualified. The other error is to pass an in

29、dividual who should not have beendetermined to be qualified. The potential for these errors to occur and the potential consequences to the laboratory should be carefully considered whendetermining the laboratorys qualification methodology. A statistical approach includes choosing the significance le

30、vel at which the determination ofqualification will be made. This produces a quantitative value of the two possible risks. This is described further in Appendix X1.6. Demonstration Process6.1 The suggested approach to practical demonstration for analyst qualification that is described in the remaind

31、er of this guideinvolves a comparison of the performance of the analyst with the performance of all qualified analysts on a particular analyticalmethod. The performance is measured by the analysis of reference materials (see ISO Guide 30) and comparison of the results tothe data base for the analyti

32、cal method. This approach requires a data base that describes method performance. The comparisondescribed in this guide is statistical in nature and therefore statisticians should be involved early on in the process of definingqualification. Other types of comparisons may serve to qualify equally we

33、ll; however, such comparisons are not addressed in thisguide. If used, they should be defined and documented.6.2 The data base for a given analytical method is generated by all qualified analysts who run reference material samples onan established schedule or frequency. The data base is used to esta

34、blish the bias and precision of the method as routinely used inthe laboratory. The data base is established through a measurement control program as presented in Guide C1210. For a newmethod, a data base should be established according to Guide C1068 and the analyst should be qualified against that

35、data base.6.3 If changes in a method occur or changes in the execution of a method occur that render the existing data base representationof the method questionable, the qualification of analysts should be suspended until the data base is verified or a new data base isgenerated. When a new data base

36、 is generated, the old data base should be archived (retained for future reference) as a part of thedocumentation of the laboratory quality assurance program.6.4 Apredetermined number of reference material samples should be selected for the analyst after training has been completed.The analyst shoul

37、d analyze the samples over several days, and not in a single session, to simulate more realistically the conditionsunder which the data base was established.6.5 Since the samples may be at different concentration levels, the analysts demonstration results are normalized usingestablished parameters f

38、rom the existing data base for each control standard. The normalized data are used to test for conformityto the data base. Statistical tests for the statistical distribution (normality) as well as precision and bias are suggested in Section67. These terms are described in Guide C1215.6.6 If the resu

39、lts of all three tests are satisfactory, the analyst is qualified on that method. If the analyst does not qualify,retraining should be required before being allowed to retest for qualification. The analyst should be given a different set ofreference material samples each time retesting is allowed to

40、 maintain the independence of successive tries.That will allow the samestatistical tests to be used on each set of results. See Fig. 2 for a schematic of the qualification process.7. Statistical Tests7.1 There are a number of statistical procedures appropriate for performing the statistical tests on

41、 the analysts demonstrationdata set to determine qualification. The procedures detailed in Appendix X2 are suggested since they have proven to be useful.Further information about these procedures is provided by Snedecor and Cochran4 and by NUREG/CR-4604.57.2 The analystss data set is first tested fo

42、r statistical normality. If normality is rejected, the data set is rejected and the analystis determined to have failed the qualification test. If the data set is accepted as normally distributed, bias and precision tests maybe performed.7.3 If these statistical tests indicate that the analysts data

43、 set exhibits bias and precision estimates that are within those of theestablished data base, the analyst is determined to be qualified. If the precision or bias estimates, or both, are not acceptable, thedata set is rejected and the analysts is determined to have failed the qualification test.7.4 E

44、xamples of statistical tests are presented in Appendix X2.8. Keywords8.1 analyst qualification; measurement(s); quality assurance; reference materials4 Snedecor, G.W., and Cochran, W.G., Statistical Methods, 8th Ed., Iowa State University Press, Ames, Iowa, 1989.5 NUREG/CR-4604, Statistical Methods

45、for Nuclear Material Management, U.S. Nuclear Regulatory Commission, Washington, DC, 1988.C1297 183APPENDIXES(Nonmandatory Information)X1. STATISTICAL CONSIDERATIONSX1.1 The significance level, , for a statistical test is set depending on the desired risk of rejecting a qualified analyst. The smalle

46、rthe significance level, the smaller the chance that a qualified analyst will be rejected (Type I error). For example, if the significancelevel is 0.10, then there is a one in ten chance that a qualified analyst will fail the test. However, by using a small , the chanceof accepting an unqualified an

47、alyst is large (Type II error). Thus there is a trade-off between accepting an unqualified analyst andrejecting a qualified one. Both types of errors can be controlled at desirable low levels by requiring a sufficiently large number ofdemonstration tests.4,5 Practical limitations usually restrict th

48、e available number of demonstration tests so that only the risk ofrejecting a qualified analyst may be adequately controlled by an appropriately small level of significance.X1.2 For multiple statistical tests, another factor that should be considered when selecting the significance level of each tes

49、t is theoverall significance level. For example, the overall significance level for three independent tests would be = 1 (1 )4.Therefore, if the significance level of each test was 0.05, the overall significance level would be 0.143. In other words, the chanceof a qualified analyst failing any one or more of three independent statistical tests when each test has a significance level of 0.05would be 14.3 %.FIG. 2 Steps in the Analyst Qualification ProcessC1297 184X2. SUGGESTED STATISTICAL TESTSX2.1 TEST 1Test for Normality:X2.1.1 Problem StatementTest w