1、Designation: C1068 03 (Reapproved 2011)C1068 15Standard Guide forQualification of Measurement Methods by a LaboratoryWithin the Nuclear Industry1This standard is issued under the fixed designation C1068; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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 provides guidance for selecting, validating, and qualifying measurement me
3、thods when qualification is requiredfor a specific program. The recommended practices presented in this guide provide a major part of a quality assurance programfor the laboratory data (see Fig. 1). Qualification helps to assure that the data produced will meet established requirements.1.2 The activ
4、ities intended to assure the quality of analytical laboratory measurement data are diagrammed in Fig. 1. Discussionand guidance related to some of these activities appear in the following sections:SectionSelection of Measurement Methods 5Validation of Measurement Methods 6Qualification of Measuremen
5、t Methods 7Control 8Personnel Qualification 91.3 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 and health practices and determine the applicability of regulat
6、orylimitations prior to use.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 NuclearIndustryC1128 Guide for Preparation of Working Reference Materia
7、ls 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 Establishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Withinthe Nuclear Indust
8、ryC1297 Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle MaterialsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Technique
9、sE2655 Guide for Reporting Uncertainty of Test Results and Use of the Term Measurement Uncertainty in ASTM Test Methods2.2 ISO Standards:3ISO/IEC 17025 General Requirements for the Competence of Testing and Calibration Laboratories2.3 Other Standards:ASME NQA-1 Quality Assurance Requirements for Nuc
10、lear Facility Applications4IEEE/ASTM SI 10 American National Standard for Metric Practice51 This guide is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.08 on Quality Assurance,Statistical Applications, and Reference Materials.
11、Current edition approved June 1, 2011June 1, 2015. Published June 2011June 2015. Originally approved in 1986. Last previous edition approved in 20032011 asC1068 03.C1068 03 (2011). DOI: 10.1520/C1068-03R11.10.1520/C1068-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or conta
12、ctASTM 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 Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.4 Availab
13、le from American Society of Mechanical Engineers (ASME), ASME International Headquarters, Two Park Ave., New York, NY 10016-5990, http:/www.asme.org.5 Available from Institute of Electrical and Electronics Engineers, Inc. (IEEE), 445 Hoes Ln., Piscataway, NJ 08854-4141, http:/www.ieee.org.This docum
14、ent 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 adequately depict all changes accurately, ASTM recommends that users consult prior editions as a
15、ppropriate. 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, PA 19428-2959. United States1JCGM-100 Evaluation of Measurement Data Guide to the Expre
16、ssion of Uncertainty in Measurement (GUM)JCGM-200 International Vocabulary of Metrology Basic and General Concepts and Associated Terms (VIM)3. Terminology3.1 Except as otherwise defined herein, definitions of terms are as given in Terminology C859.3.2 Definitions of Terms Specific to This Standard:
17、3.2.1 fitness for purpose, ndegree to which data produced by a measurement process enables a user to make technically andadministratively correct decisions for a stated purpose (1).73.2.2 qualificationa formal process to provide a desired level of confidence that measurement methods used will produc
18、e datasuitable for their intended use. The methods must meet established criteria prior to use and must be used under conditionsestablished for qualifications.3.2.3 representative sample, na sample resulting from a sampling plan that can be expected to adequately reflect the propertiesof interest of
19、 the parent population (1).3.2.4 validation, ninvestigation to determine the applicability of a measurement method to a particular use.4. Significance and Use4.1 Because of concerns for safety and the protection of nuclear materials from theft, stringent specifications are placed onchemical processe
20、s and the chemical and physical properties of nuclear materials. Strict requirements for the control andaccountability of nuclear materials are imposed on the users of those materials. Therefore, when analyses are made by a laboratoryto support a project such as the fabrication of nuclear fuel mater
21、ials, various performance requirements may be imposed on thelaboratory. One such requirement is often the use of qualified methods. Their use gives greater assurance that the data producedwill be satisfactory for the intended use of those data.Aqualified method will help assure that the data produce
22、d will be comparableto data produced by the same qualified method in other laboratories.4.2 This guide provides guidance for qualifying measurement methods and for maintaining qualification. Even though allpractices would be used for most qualification programs, there may be situations in which only
23、 a selected portion would berequired. Care should be taken, however, that the effectiveness of qualification is not reduced when applying these practicesselectively. The recommended practices in this guide are generic; based on these practices, specific actions should be developedto establish a qual
24、ification program.5. Selection of Measurement Methods5.1 General:7 The boldface numbers in parentheses refer to a list of references at the end of this standard.FIG. 1 Quality Assurance of Analytical Laboratory DataC1068 1525.1.1 Before qualifying a method for a specific application, there should be
25、 assurance that the method has been properly selectedfor that application. The guidance given in this section can be used to assess the adequacy of the methods application. Theguidance can also be used to select a new method when a new measurement capability is required within a laboratory.5.1.2 Mea
26、surement methods generally can be classified as one of three types as follows:5.1.2.1 Those published as national or international consensus standards,5.1.2.2 Those established as acceptable for a specific application based on long-term and wide usage, and5.1.2.3 Those having limited use, for exampl
27、e, those used only by a few laboratories or those that are relatively new.5.1.3 For some applications, there is a choice available of two or more acceptable methods. In those cases, one method is usuallyrecognized as the reference method, particularly if it is a published standard or if it is capabl
28、e of producing the least bias and bestprecision.5.1.4 The selection of a method should be based on the criteria in 5.2. In situations where a reference method and one or moreacceptable methods are available, there should be no technical restrictions placed on which method is used.5.2 Recommended Pra
29、ctices for Method Selection:5.2.1 Technical BasisThe method should be based on sound technology. This means that proven laboratory and instrumentaltechniques are used in ways recognized and accepted by the community of users.5.2.2 InterferencesThe method should not be adversely affected by component
30、s in the matrix of the material to be analyzed.Knowledge about the methods limitations and about the composition of the material should be used to determine if the analysiswill be affected by interferences. Other potential interferences such as environmental or electrical/electronic conditions shoul
31、d beconsidered in the selection process.5.2.3 RangeThe method should be capable of responding adequately across the range of concentration levels that will beencountered for the constituent to be measured. This requirement is most often of concern for methods used to measure impuritiesin materials s
32、ince impurity concentrations may fluctuate to a greater extent than other constituents. It is important that themeasurement technique used discriminates adequately between concentration levels encountered. The lowest concentration levelthat can be measured reliably should be clearly established (det
33、ection limit).5.2.4 Reliability of MethodThe method must be capable of producing data that will meet the bias and precision requirementsestablished for the required analysis under the expected conditions of use. The requirements are usually established by the userof the data and they should be based
34、 on the concentration levels of the constituents to be measured and on specification limits setfor the constituents.5.2.5 Fitness for Purpose of Safeguards and Nuclear Safety ApplicationsMethods intended for use in safeguards and nuclearsafety applications shall meet the additional requirements spec
35、ified in Annex A1.6. Validation of Measurement Methods6.1 There are occasions when it is desirable to investigate the applicability of a method to a particular use. This may be the casewhen the method has had limited use or it is being considered for a new or unique application. To provide some conf
36、idence thata qualification effort would be successful, it may be desirable to validate the application of the method. Validation is not amandatory step in the selection and qualification process, but it can prevent wasted effort from attempts to qualify inadequatemethods.6.2 Validation of a method i
37、s usually done by an analyst under controlled conditions. Basically, validation involves investigatingany or all of the selection criteria in 5.2. The intent is to define method capability and to determine if the method can be properlyapplied as intended. If modification of the method is required fo
38、r it to be applicable, validation will provide the technicalinformation needed for modification. Validation also provides the experience and information to write a detailed procedure ifnecessary. The result of the validation process will be either the rejection of a proposed method or confidence tha
39、t it is acceptablefor use as intended.7. Qualification of Measurement Methods7.1 General:7.1.1 Although a method is selected based on the criteria in 5.2 of this guide, there is no assurance that a laboratory can actuallyobtain the performance expected from the method. In addition, there may not be
40、sufficient assurance that the method is in factadequate for its intended use. To provide those assurances, demonstration is included in the qualification process.7.1.2 Qualification requires having a laboratory demonstrate that a method can produce acceptable data under specifiedconditions of qualif
41、ication. Demonstration must be done under actual operating conditions and not under ideal test conditions. Aspecified material is analyzed to produce a specified amount of data. These data are evaluated by the person or organization thatis responsible for approving qualification. The procedure estab
42、lished for demonstration should include provisions for handlingfailures in the demonstration and for repeating the demonstration should the method not be used for a specified period of time.Demonstration could also include producing other evidence such as appropriate literature references that the m
43、ethod is in factapplicable to the material to be analyzed.7.2 Recommended Practices:C1068 1537.2.1 ProceduresThe use of a method to make a laboratory measurement involves taking discrete actions in a specific order.Any change in an action or in the order may produce unsatisfactory data. To minimize
44、potential problems, written, stepwiseprocedures should be provided within the methods. It is important that procedures are well-written, complete, and correct. Theyshould receive technical and editorial reviews, and should be approved by appropriate management. Approval by the user of thedata to be
45、produced also may be required. Procedures prepared in accordance with Guide C1009 will meet these criteria.7.2.2 Method Performance RequirementsTo provide acceptable data, the method must be capable of meeting performancerequirements for bias, precision, and range. Before a laboratory demonstrates i
46、ts capability, these requirements should be clearlyestablished (this should be done even before a method is selected for use; see 5.2). Specifications established for a process ormaterial are the primary source of information on which the performance requirements are based. The performance requireme
47、ntsshould be used to establish conditions required for qualification. Such conditions may require a statistically designed experimentto allow for other sources of variability such as the number of analysts or instruments, or both, as well as the concentration rangeof interest.7.2.3 Test MaterialsThe
48、 material or materials that will be used for demonstration should be specified. The test materialsshould be as similar as possible to the material that will be analyzed. When possible, the composition or properties of test materialsshould be defined by measurements traceable to certified reference m
49、aterials. See Guide C1128.7.2.3.1 Major ConstituentsWhen the method is to be used to determine a major constituent (for example, uranium in uraniumoxide), a single test material may be specified. The concentration of the constituent in this test material should approximate thespecification value established for the constituent in the material to be analyzed. The concentration value of the test material shouldnot be given to the laboratory; only those responsible for evaluating the data and approving qualification should know the value(see 7.2.4.4). The ca
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