1、Designation: C 1210 06Standard Guide forEstablishing a Measurement System Quality ControlProgram for Analytical Chemistry Laboratories Within theNuclear Industry1This standard is issued under the fixed designation C 1210; the number immediately following the designation indicates the year oforiginal
2、 adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This standard provides guidance for establishing andmaintaining a
3、measurement system quality control program.Guidance is provided for general program considerations,preparation of quality control samples, analysis of qualitycontrol samples, quality control data analysis, analyst qualifi-cation, measurement system calibration, measurement methodqualification, and m
4、easurement system maintenance.1.2 This guidance is provided in the following sections:SectionGeneral Quality Control Program Considerations 4Quality Control Samples 5Analysis of Quality Control Samples 6Quality Control Data Analysis 7Analyst Qualification 8Measurement System Calibration 9Measurement
5、 Method Qualification 10Measurement System Maintenance 112. Referenced Documents2.1 ASTM Standards:2C 1009 Guide for Establishing a Quality Assurance Pro-gram for Analytical Chemistry Laboratories Within theNuclear IndustryC 1068 Guide for Qualification of Measurement Methodsby a Laboratory Within t
6、he Nuclear IndustryC 1128 Guide for Preparation of Working Reference Mate-rials for Use in the Analysis of Nuclear Fuel CycleMaterialsC 1156 Guide for Establishing Calibration for a Measure-ment Method Used to Analyze Nuclear Fuel Cycle Mate-rialsC 1297 Guide for Laboratory Analysts for the Analysis
7、 ofNuclear Fuel Cycle Materials2.2 ANSI Standards:3ANSI/ASQ B1 Guide for Quality Control ChartsANSI/ASQ B2 Control Chart Method of Analyzing DataANSI/ASQ B3 Control Chart Method of Controlling Qual-ity During Production3. Significance and Use3.1 A laboratory quality assurance program is an essential
8、program for laboratories within the nuclear industry. GuideC 1009 provides guidance for establishing a quality assuranceprogram for an analytical laboratory within the nuclear indus-try. The basic elements of a laboratory quality assuranceprogram are organization, quality assurance program, training
9、and qualification, procedures, laboratory records, control ofrecords, control of procurement, control of measuring equip-ment and materials, control of measurements, and deficienciesand corrective actions. This guide deals with the control ofmeasurements aspect of the laboratory quality assurance pr
10、o-gram. Fig. 1 shows the relationship of measurement controlwith other essential aspects of a laboratory quality assuranceprogram.3.2 The fundamental purposes of a measurement controlprogram are to provide the with use assurance (real-timecontrol) that a measurement system is performing satisfactori
11、lyand to provide the data necessary to quantify measurementsystem performance. The with use assurance is usually pro-vided through the satisfactory analysis of quality controlsamples (reference value either known or unknown to theanalyst). The data necessary to quantify measurement systemperformance
12、 is usually provided through the analysis of qualitycontrol samples or the duplicate analysis of process samples, orboth. In addition to the analyses of quality control samples, thelaboratory quality control program should address (1) thepreparation and verification of standards and reagents, (2) da
13、taanalysis procedures and documentation, (3) calibration andcalibration procedures, (4) measurement method qualification,(5) analyst qualification, and (6) other general program con-siderations. Other elements of laboratory quality assurance also1This guide is under the jurisdiction of ASTM Committe
14、e C26 on Nuclear FuelCycle and is the direct responsibility of Subcommittee C26.08 on QualityAssuranceApplications.Current edition approved Jan. 1, 2006. Published February 2006. Originallyapproved in 1991. Last previous edition approved in 1996 as C 1210 96e1.2For referenced ASTM standards, visit t
15、he ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual 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
16、 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.impact the laboratory quality control program. These elementsor requirements include (1) chemical analysis procedures andprocedure control, (2) records storage and retrieval requ
17、ire-ments, (3) internal audit requirements, (4) organizational con-siderations, and (5) training/qualification requirements. To theextent possible, this standard will deal primarily with qualitycontrol requirements rather than overall quality assurancerequirements.3.3 Although the Standard Guide use
18、s suggestive ratherthan prescriptive language (for example, “should” as opposedto “shall”), the elements being addressed should not beinterpreted as optional. An effective and comprehensive labo-ratory quality control program should, at minimum, completelyand adequately consider and include all elem
19、ents listed inSection 1 and in the corresponding referenced sections of thisguide.4. General Quality Control Program Considerations4.1 The quality control activities described in this guide areintended for a quality control function which is internal to ananalytical chemistry laboratory. The quality
20、 control programshould have an administrator or manager working in concertwith laboratory managers to produce cost effective measure-ments of demonstrated quality. The program manager shouldhave the authority based on quality control sample perfor-mance to disqualify analysts or measurement systems,
21、 or torequest or require additional quality control sample analyses. Itis desirable for the quality control program to have periodicinternal assessments. These assessments should involve labo-ratory managers, the quality control manager, and laboratorycustomers. The quality control program should be
22、 audited forprocedure compliance at periodic intervals by the qualityassurance organization.4.2 The analytical laboratories quality control programshould be described in laboratory procedures and all measure-ment system quality control activities should be documented.The retention period for the doc
23、umentation should be describedin laboratory procedures and consistent with other laboratorystorage requirements and any applicable contractual or regula-tory requirements.4.3 External quality control program assessment should beconducted by an outside organization or agency at a frequencydictated by
24、 company or facility policy, contract, or otherapplicable regulations or requirements. When possible, labo-ratory and quality control management should involve labora-tory measurement systems in external exchange programs,such as: interlaboratory exchange programs, sample exchangeprograms, sample or
25、 standard round robins, and referee analy-ses programs. The programs provide some degree of externalverification or validation of the measurement system qualitycontrol program that is desirable.5. Quality Control Samples5.1 Quality control samples (knowns, unknowns, blinds,blanks, etc.) are used to
26、verify and monitor measurementsystem performance. Quality control samples should be pre-pared or purchased over the measurement range of interest andhave an impurity content and matrix composition that approxi-mates the process samples, unless the measurement method hasbeen shown to be free from sam
27、ple matrix effects. Qualitycontrol sample preparation procedures, specific requirements(purity of source materials and solvents; storage requirement;shelf life; etc.), and the preparation should be documented.Quality control samples may be prepared from the following:Certified Reference Materials (C
28、RMs), Working ReferenceMaterials (WRMs), other reference materials, pure elements orcompounds with vendor supplied assay, reagent grade (orbetter) chemicals with assay, and process materials. Guidanceon the preparation of WRMs for use in the analysis of nuclearfuel cycle materials is provided in Gui
29、de C 1128.5.2 When quality control samples are prepared, the prepa-ration procedure and data (mass, volume, etc.) should bedocumented. Further, appropriate measurements should beperformed to verify the prepared value.5.3 The quality control samples should be characterized toestablish their reference
30、 values when prepared from materialswith uncertain assays, or from process material, or when asmaller uncertainties are required on the samples than can beobtained from the source materials. A record of the preparationprocedure and data should be maintained. The characterizationmethod or procedure,
31、complete with calibration data and thecharacterization analysis results, should be referenced or in-cluded in the preparation data.5.4 All quality control samples should be labeled with (1)the concentration, activity, abundance, etc. of the species ofinterest, (2) solvent if other than water, (3) ma
32、trix, (4) dateprepared, (5) identification of preparer, and (6) storage require-ments or limitations. Alternately, QC samples should be codedin such a manner as to uniquely identify this same information.5.5 All incoming chemicals and RMs should be labeled witha shelf life, acceptance date, or expir
33、ation date, if applicable.FIG. 1 Quality Assurance of Analytical Laboratory DataC12100626. Analysis of Quality Control Samples6.1 The analysis of data from quality control samplesprovides a demonstration of measurement system performanceand provides the information necessary to quantify that perfor-
34、mance over the portion of the system covered by the qualitycontrol samples. The reference value of the quality controlsamples may be either known or unknown to the analyst.6.1.1 The analysis of known quality control samples canprovide a satisfactory bench demonstration of whether asystem is in- or o
35、ut-of-control without the need for a computerbased quality control program. In general, the data resultingfrom the analysis of known quality control samples is notrecommended for quantifying measurement system perfor-mance.6.1.2 In general, the analysis of unknown quality controlsamples provides the
36、 data necessary to quantify measurementsystem performance. The data resulting from the analysis ofunknown quality control samples may also be used to providethe with use assurance of method performance, but some formof computer based system would be required in order toprovide the real-time, at-benc
37、h determination of system per-formance. The use of unknown quality control samples forboth functions can significantly increase the amount of dataavailable to model measurement systems.6.2 The frequency of analysis of quality control samplesshould be determined and described in laboratory procedures
38、.The frequency should be a function of the stability of themeasurement system.6.3 Quality control samples should be subjected to the sameanalysis conditions as the actual samples. The condition shouldbe the same over the entire analysis sequence from samplealiquoting and preparation to data reductio
39、n.6.3.1 When quality control samples are not subjected to aportion of the sample analysis sequence, sufficient documen-tation should exist to demonstrate that the portion of the systemthat is not covered does not contribute significantly to themeasurement system bias and precision. The liability tha
40、texists for not covering the entire sequence should be under-stood and documented.6.3.2 Even though sample aliquoting by mass or by volumemay be included in the analysis of quality control samples, thisfunction is so fundamental and common to nearly all measure-ment systems that laboratories should
41、maintain calibration andquality control programs on balances and, if applicable, onvolume aliquoting and measuring devices. Balance and volumealiquoting devices should be treated as measurement systemsor methods and should have calibration and quality controlprograms that satisfy the information con
42、tained in this guide.6.4 The analysis of quality control samples should bedocumented. The documentation should include, but not nec-essarily be limited to, date and time of analysis, measurementsystem identification, analyst identification, quality controlsample reference value or code, analysis res
43、ults, analysis rawdata, and whether the analysis passed or failed system perfor-mance criteria.6.5 The data resulting from the analyses of quality controlsamples should be evaluated against established measurementmethod control limits immediately (real-time, at-the-bench, byplotting on some form of
44、control chart or by computerassessment) and a determination made as to whether themeasurement system is in- or out-of-control.6.6 Corrective actions for an out-of-control measurementsystem should be defined and documented. The quality controlprogram should define responsibilities for taking correcti
45、veactions and should establish reporting requirements to techni-cal and operation management.6.6.1 If the measurement system is out-of-control, correc-tive actions should be initiated and measurement systemcontrol should be reestablished before using the measurementsystem to produce results.6.6.2 Co
46、rrective actions vary with circumstances and sys-tems and may include but not be limited to (1) running anumber of quality control samples; (2) a simple assignment ofcause and correction of conditions coupled with the successfulanalyses of quality control samples; (3) assignment of causethat is not
47、readily correctable, that therefore necessitates thegeneration of a new quality control data base; and (4)acomplete and detailed evaluation of measurement systemperformance and suitability to its intended purpose. In allcases, the conditions for reestablishing control need to bedefined and control s
48、hould be reestablished prior to using themeasurement system. In general, a single remeasurement of aquality control sample is not adequate to reestablish control.6.6.3 When a measurement system is out-of-control, anevaluation should be made as to the validity of the resultsgenerated since the measur
49、ement system was last verified to bein control and the samples should be reanalyzed if possible.7. Quality Control Data Analysis7.1 Data from the measurements of quality control samplesshould be statistically evaluated to assign control limits tomeasurement systems and to quantify system performancethrough bias and precision statements. ASTM STP 7A4andvarious references provide guidance on presentation of dataand control chart analysis (see Refs (1-4)5and ANSI/ASQCB1, B2, and B3).7.1.1 The frequency of measurement system data analysisor the conditions which require data analysis shoul
