1、Designation: C1297 03 (Reapproved 2011)Standard 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, in the
2、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 per-form chemical analysis or physica
3、l measurements of nuclearfuel cycle materials. The guidance is general in that it isapplicable to all analytical methods, but must be appliedmethod by method.Also, the guidance is general in that it maybe applied to initial qualification or requalification.1.2 The guidance is provided in the followi
4、ng sections:SectionQualification Considerations 4Demonstration Process 5Statistical Tests 61.3 This standard does not apply to maintaining qualifica-tion during routine use of a method. Maintaining qualificationis included in Guide C1210.1.4 This standard does not purport to address all of thesafety
5、 concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C1009 Guide for Establishing a Qua
6、lityAssurance Programfor Analytical Chemistry Laboratories Within the NuclearIndustryC1068 Guide for Qualification of Measurement Methods bya Laboratory Within the Nuclear IndustryC1128 Guide for Preparation of Working Reference Mate-rials for Use in Analysis of Nuclear Fuel Cycle MaterialsC1156 Gui
7、de for Establishing Calibration for a Measure-ment Method Used to Analyze Nuclear Fuel Cycle Mate-rialsC1210 Guide for Establishing a Measurement System Qual-ity Control Program forAnalytical Chemistry LaboratoriesWithin the Nuclear IndustryC1215 Guide for Preparing and Interpreting Precision andBia
8、s Statements in Test Method Standards Used in theNuclear Industry2.2 ISO Standard:ISO Guide 30 Terms and Definitions Used in Connectionwith Reference Materials33. Significance and Use3.1 This is one of a series of guides designed to provideguidance for implementing activities that meet the require-m
9、ents of a sound laboratory quality assurance program. Thefirst of these, Guide C1009, is an umbrella guide that providesgeneral criteria for ensuring the quality of analytical laboratorydata. Other guides provide expanded criteria in various areasaffecting quality, producing a comprehensive set of c
10、riteria forcontrolling data quality. The approach to ensuring the qualityof analytical measurements described in these guides is de-picted in Fig. 1.3.2 The training and qualification of analysts is one of theelements of laboratory quality assurance presented in GuideC1009, which provides some gener
11、al criteria regarding quali-fication. This guide expands on those criteria to provide morecomprehensive guidance for qualifying analysts. As indicatedin Guide C1009, the qualification process can vary in ap-proach; this guide provides one such approach.3.3 This guide describes an approach to analyst
12、 qualificationthat is designed to be used in conjunction with a rigorousprogram for the qualification and control of the analyticalmeasurement system. This requires an existing data base whichdefines the characteristics (precision and bias) of the system inroutine use. The initial development of thi
13、s data base isdescribed in Guide C1068. The process described here isintended only to qualify analysts when such a data base existsand the method is in control.3.4 The qualification activities described in this guide as-sume that the analyst is already proficient in general laboratoryoperations. The
14、 training or other activities that developed thisproficiency are not covered in this guide.1This guide is under the jurisdiction of ASTM Committee C26 on Nuclear FuelCycle and is the direct responsibility of Subcommittee C26.08 on Quality Assur-ance, Statistical Applications, and Reference Materials
15、.Current edition approved June 1, 2011. Published June 2011. Originallyapproved in 1995. Last previous edition approved in 2003 as C1297 - 03. DOI:10.1520/C1297-03R11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
16、Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700,
17、West Conshohocken, PA 19428-2959, United States.3.5 This guide describes a basic approach and principles forthe qualification of laboratory analysts. Users are cautioned toensure that the qualification program implemented meets theneeds and requirements of their laboratory.4. Qualification Considera
18、tions4.1 When a qualification program is being established,consideration should be given to analyst selection criteria, thetraining program, and practical demonstration. The criteria thatgovern when qualification is achieved should be documentedalong with methods for determining the knowledge and sk
19、ill ofthe analyst.4.1.1 Analyst selection should be based on establishedcriteria that are related to the complexity of the method thatanalysts are expected to perform. Criteria should include theminimum education required, any prerequisite training, and theoverall experience required. The selection
20、criteria should bedefined and documented.4.1.2 The method-specific analyst training program shouldbe an established program with a prescribed training proce-dure. Some mechanism such as an oral or written test should beused to allow an analyst to demonstrate knowledge andunderstanding of the chemica
21、l, physical, instrumental, andmathematical concepts used to execute the method. It isadvisable to monitor progress during training to ensure that theanalyst has a reasonable chance of passing the qualificationtest.4.1.3 The practical demonstration of the analysts ability togenerate results with the
22、analytical method should be comparedto established criteria. The comparison criteria should bedefined and documented.NOTE 1The qualification of analysts, like many other laboratoryprocesses, has the potential for undetected errors. There are two types oferrors that occur. One is to fail an individua
23、l who should have beendetermined to be qualified. The other error is to pass an individual whoshould not have been determined to be qualified. The potential for theseerrors to occur and the potential consequences to the laboratory should becarefully considered when determining the laboratorys qualif
24、icationmethodology. A statistical approach includes choosing the significancelevel at which the determination of qualification will be made. Thisproduces a quantitative value of the two possible risks. This is describedfurther in Appendix X1.5. Demonstration Process5.1 The suggested approach to prac
25、tical demonstration foranalyst qualification that is described in the remainder of thisguide involves a comparison of the performance of the analystwith the performance of all qualified analysts on a particularanalytical method. The performance is measured by the analy-sis of reference materials (se
26、e ISO Guide 30) and comparisonof the results to the data base for the analytical method. Thisapproach requires a data base that describes method perfor-mance. The comparison described in this guide is statistical innature and therefore statisticians should be involved early on inthe process of defin
27、ing qualification. Other types of compari-sons may serve to qualify equally well; however, such com-parisons are not addressed in this guide. If used, they should bedefined and documented.5.2 The data base for a given analytical method is generatedby all qualified analysts who run reference material
28、 samples onan established schedule or frequency. The data base is used toestablish the bias and precision of the method as routinely usedin the laboratory. The data base is established through ameasurement control program as presented in Guide C1210.For a new method, a data base should be establishe
29、d accordingto Guide C1068 and the analyst should be qualified against thatdata base.5.3 If changes in a method occur or changes in the executionof a method occur that render the existing data base represen-tation of the method questionable, the qualification of analystsshould be suspended until the
30、data base is verified or a newdata base is generated. When a new data base is generated, theold data base should be archived (retained for future reference)as a part of the documentation of the laboratory qualityassurance program.5.4 A predetermined number of reference material samplesshould be sele
31、cted for the analyst after training has beencompleted. The analyst should analyze the samples overseveral days, and not in a single session, to simulate morerealistically the conditions under which the data base wasestablished.5.5 Since the samples may be at different concentrationlevels, the analys
32、ts demonstration results are normalized usingestablished parameters from the existing data base for eachcontrol standard. The normalized data are used to test forconformity to the data base. Statistical tests for the statisticaldistribution (normality) as well as precision and bias aresuggested in S
33、ection 6. These terms are described in GuideC1215.5.6 If the results of all three tests are satisfactory, the analystis qualified on that method. If the analyst does not qualify,retraining should be required before being allowed to retest forqualification. The analyst should be given a different set
34、 ofreference material samples each time retesting is allowed toFIG. 1 Quality Assurance of Analytical Laboratory DataC1297 03 (2011)2maintain the independence of successive tries. That will allowthe same statistical tests to be used on each set of results. SeeFig. 2 for a schematic of the qualificat
35、ion process.6. Statistical Tests6.1 There are a number of statistical procedures appropriatefor performing the statistical tests on the analysts demonstra-tion data set to determine qualification. The procedures de-tailed in Appendix X2 are suggested since they have proven tobe useful. Further infor
36、mation about these procedures isprovided by Snedecor and Cochran4and by NUREG/CR-4604.56.2 The analystss data set is first tested for statisticalnormality. If normality is rejected, the data set is rejected andthe analyst is determined to have failed the qualification test. Ifthe data set is accepte
37、d as normally distributed, bias andprecision tests may be performed.6.3 If these statistical tests indicate that the analysts data setexhibits bias and precision estimates that are within those ofthe established data base, the analyst is determined to bequalified. If the precision or bias estimates,
38、 or both, are notacceptable, the data set is rejected and the analysts is deter-mined to have failed the qualification test.6.4 Examples of statistical tests are presented in AppendixX2.7. Keywords7.1 analyst qualification; measurement(s); quality assur-ance; reference materials4Snedecor, G.W., and
39、Cochran, W.G., Statistical Methods, 8th Ed., Iowa StateUniversity Press, Ames, Iowa, 1989.5NUREG/CR-4604, Statistical Methods for Nuclear Material Management,U.S. Nuclear Regulatory Commission, Washington, DC, 1988.FIG. 2 Steps in the Analyst Qualification ProcessC1297 03 (2011)3APPENDIXES(Nonmandat
40、ory Information)X1. STATISTICAL CONSIDERATIONSX1.1 The significance level, a, for a statistical test is setdepending on the desired risk of rejecting a qualified analyst.The smaller the significance level, the smaller the chance thata qualified analyst will be rejected (Type I error). For example,if
41、 the significance level is 0.10, then there is a one in ten chancethat a qualified analyst will fail the test. However, by using asmall a, the chance of accepting an unqualified analyst is large(Type II error). Thus there is a trade-off between accepting anunqualified analyst and rejecting a qualifi
42、ed one. Both types oferrors can be controlled at desirable low levels by requiring asufficiently large number of demonstration tests.4,5Practicallimitations usually restrict the available number of demonstra-tion tests so that only the risk of rejecting a qualified analystmay be adequately controlle
43、d by an appropriately small levelof significance.X1.2 For multiple statistical tests, another factor thatshould be considered when selecting the significance level ofeach test is the overall significance level. For example, theoverall significance level for three independent tests would bea8 =1(1a)4
44、. Therefore, if the significance level of eachtest was 0.05, the overall significance level would be 0.143. Inother words, the chance of a qualified analyst failing any one ormore of three independent statistical tests when each test has asignificance level of 0.05 would be 14.3 %.X2. SUGGESTED STAT
45、ISTICAL TESTSX2.1 TEST 1Test for Normality:X2.1.1 Problem StatementTest whether the demonstra-tion data set is normally distributed.NOTE X2.1This test assumes that the data base itself is normallydistributed.Let,Yi5xi2 isi(X2.1)Y5(i 5 1nYin(X2.2)s25(i 5 1nYi2 Y!2n 2 1(X2.3)where:xi= theith demonstra
46、tion result,i= the known mean associated with theith referencematerial sample in the data base, andsi= the known standard deviation associated with theithreference material sample in the data base, and n is thenumber of demonstration results.X2.1.2 Test statistic:W 5b2n 2 1!s2(X2.4)where:b 5(i 5 1ka
47、iYn21112 Yi! (X2.5)Yiare sorted in ascending order,k = n/2, rounded down, andaiare the Shapiro-Wilks coefficients.4 ,5X2.1.3 Acceptance RegionUse Shapiro-Wilks tables todetermine the acceptance region for a desired level of signifi-cance.4,5X2.2 TEST 2Testing the Variance (Precision):X2.2.1 Problem
48、StatementTest whether the standardizeddemonstration results have a variance different from thevariance of a standard normal distribution.Ho: s25 1 (X2.6)Ha: s2fi 1 (X2.6)X2.2.2 Test Statistic:X25n21!s2s2(X2.7)where:s2=1.X2.2.3 Acceptance RegionUse chi-square tables to deter-mine the acceptance regio
49、n for a desired level of significanceand n1 degrees of freedom.4,5X2.3 TEST 3Testing the Mean (Bias):X2.3.1 Problem StatementTest whether the standardizeddemonstration results have a mean different from the mean ofthe standard normal distribution.Ho: 5 0 Ha: fi 0 (X2.8)X2.3.2 Test Statistic:C1297 03 (2011)4Z 5Y2s/=n(X2.9)where: = 0 and s =1.X2.3.3 Acceptance RegionUse standard normal tables todetermine the acceptance region for a desired level of signifi-cance.4,5X2.3.4 The following examples provide data and test resultsfor actual qualification
