ASTM D6299-2013 red 1250 Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance《采用统计质量保证.pdf

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1、Designation: D6299 102D6299 13 An American National StandardStandard Practice forApplying Statistical Quality Assurance and Control ChartingTechniques to Evaluate Analytical Measurement SystemPerformance1This standard is issued under the fixed designation D6299; the number immediately following the

2、designation indicates the year oforiginal adoption or, 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 NOTECorrected definition references

3、and figure numbering editorially in March 2011.2 NOTECorrected Table A1.8 footnote editorially in March 2012.1. Scope Scope*1.1 This practice covers information for the design and operation of a program to monitor and control ongoing stability andprecision and bias performance of selected analytical

4、 measurement systems using a collection of generally accepted statisticalquality control (SQC) procedures and tools.NOTE 1A complete list of criteria for selecting measurement systems to which this practice should be applied and for determining the frequency atwhich it should be applied is beyond th

5、e scope of this practice. However, some factors to be considered include (1) frequency of use of the analyticalmeasurement system, (2) criticality of the parameter being measured, (3) system stability and precision performance based on historical data, (4) businesseconomics, and (5) regulatory, cont

6、ractual, or test method requirements.1.2 This practice is applicable to stable analytical measurement systems that produce results on a continuous numerical scale.1.3 This practice is applicable to laboratory test methods.1.4 This practice is applicable to validated process stream analyzers.1.5 This

7、 practice is applicable to monitoring the differences between two analytical measurement systems that purport tomeasure the same property provided that both systems have been assessed in accordance with the statistical methodology inPractice D6708 and the appropriate bias applied.NOTE 2For validatio

8、n of univariate process stream analyzers, see also Practice D3764.NOTE 3One or both of the analytical systems in 1.5 can be laboratory test methods or validated process stream analyzers.1.6 This practice assumes that the normal (Gaussian) model is adequate for the description and prediction of measu

9、rementsystem behavior when it is in a state of statistical control.NOTE 4For non-Gaussian processes, transformations of test results may permit proper application of these tools. Consult a statistician for furtherguidance and information.2. Referenced Documents2.1 ASTM Standards:2D3764 Practice for

10、Validation of the Performance of Process Stream Analyzer SystemsD5191 Test Method for Vapor Pressure of Petroleum Products (Mini Method)D6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purportto Measure the Same Property of a MaterialD6792

11、 Practice for Quality System in Petroleum Products and Lubricants Testing LaboratoriesD7372 Guide for Analysis and Interpretation of Proficiency Test Program ResultsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE178 Practice for Dealing With Outlying ObservationsE456 Term

12、inology Relating to Quality and Statistics1 This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.94 on Coordinating Subcommittee on Quality Assurance and Statistics.Current editi

13、on approved March 1, 2010Oct. 1, 2013. Published June 2010October 2013. Originally approved in 1998. Last previous edition approved in 20092010 asD6299D6299 10209 DOI: 10.1520/D6299-10.10.1520/D6299-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Servi

14、ce at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.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

15、 version. Becauseit may not be technically possible to adequately 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.*A Summary of Changes

16、 section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 accepted

17、reference value, na value that serves as an agreed-upon reference for comparison and that is derived as (1) atheoretical or established value, based on scientific principles, (2) an assigned value, based on experimental work of some nationalor international organization, such as the U.S. National In

18、stitute of Standards and Technology (NIST), or (3) a consensus value,based on collaborative experimental work under the auspices of a scientific or engineering group. E177, E4563.1.2 accuracy, nthe closeness of agreement between an observed value and an accepted reference value. E177, E4563.1.3 assi

19、gnable cause, na factor that contributes to variation and that is feasible to detect and identify. E4563.1.4 bias, na systematic error that contributes to the difference between a population mean of the measurements or test resultsand an accepted reference or true value. E177, E4563.1.5 control limi

20、ts, nlimits on a control chart that are used as criteria for signaling the need for action or for judging whethera set of data does or does not indicate a state of statistical control. E4563.1.6 lot, na definite quantity of a product or material accumulated under conditions that are considered unifo

21、rm for samplingpurposes. E4563.1.7 precision, nthe closeness of agreement between test results obtained under prescribed conditions. E4563.1.8 repeatability conditions, nconditions where mutually independent test results are obtained with the same test method inthe same laboratory by the same operat

22、or with the same equipment within short intervals of time, using test specimens taken atrandom from a single sample of material.3.1.9 reproducibility conditions, nconditions under which test results are obtained in different laboratories with the same testmethod, using test specimens taken at random

23、 from the same sample of material.3.2 Definitions of Terms Specific to This Standard:3.2.1 analytical measurement system, na collection of one or more components or subsystems, such as samplers, testequipment, instrumentation, display devices, data handlers, printouts or output transmitters, that is

24、 used to determine a quantitativevalue of a specific property for an unknown sample in accordance with a test method.3.2.1.1 DiscussionA standard test method (for example, ASTM, ISO) is an example of an analytical measurement system.3.2.1.2 DiscussionAn analytical measurement system may comprise mul

25、tiple instruments being used for the same test method provided there is nostatistically observable bias and precision differences between the multiple instruments.3.2.2 blind submission, nsubmission of a check standard or quality control (QC) sample for analysis without revealing theexpected value t

26、o the person performing the analysis.3.2.3 check standard, nin QC testing, a material having an accepted reference value used to determine the accuracy of ameasurement system.3.2.3.1 DiscussionA check standard is preferably a material that is either a certified reference material with traceability t

27、o a nationally recognizedbody or a material that has an accepted reference value established through interlaboratory testing. For some measurement systems,a pure, single component material having known value or a simple gravimetric or volumetric mixture of pure components havingcalculable value may

28、serve as a check standard. Users should be aware that for measurement systems that show matrixdependencies, accuracy determined from pure compounds or simple mixtures may not be representative of that achieved on actualsamples.3.2.4 common (chance, random) cause, nfor quality assurance programs, one

29、 of generally numerous factors, individually ofrelatively small importance, that contributes to variation, and that is not feasible to detect and identify.3.2.5 double blind submission, nsubmission of a check standard or QC sample for analysis without revealing the checkstandard or QC sample status

30、and expected value to the person performing the analysis.3.2.6 in-statistical-control, adja process, analytical measurement system, or function that exhibits variations that can only beattributable to common cause.D6299 1323.2.7 proficiency testing, ndetermination of a laboratorys testing capability

31、 by participation in an interlaboratory crosscheckprogram.3.2.7.1 DiscussionASTM Committee D02 conducts proficiency testing among hundreds of laboratories, using a wide variety of petroleum productsand lubricants.3.2.8 quality control (QC) sample, nfor use in quality assurance programs to determine

32、and monitor the precision and stabilityof a measurement system, a stable and homogeneous material having physical or chemical properties, or both, similar to those oftypical samples tested by the analytical measurement system. The material is properly stored to ensure sample integrity, and isavailab

33、le in sufficient quantity for repeated, long term testing.3.2.9 site expected value (SEV), nfor a QC sample this is an estimate of the theoretical limiting value towards which theaverage of results collected from a single in-statistical-control measurement system under site precision conditions tend

34、s as thenumber of results approaches infinity.3.2.9.1 DiscussionThe SEV is associated with a single measurement system; for control charts that are plotted in actual measured units, the SEV isrequired, since it is used as a reference value from which upper and lower control limits for the control ch

35、art specific to a batchof QC material are constructed.3.2.10 site precision (R), nthe value below which the absolute difference between two individual test results obtained undersite precision conditions may be expected to occur with a probability of approximately 0.95 (95 %). It is defined as 2.77

36、times thestandard deviation of results obtained under site precision conditions.3.2.11 site precision conditions, nconditions under which test results are obtained by one or more operators in a single sitelocation practicing the same test method on a single measurement system which may comprise mult

37、iple instruments, using testspecimens taken at random from the same sample of material, over an extended period of time spanning at least a 15 day interval.3.2.11.1 DiscussionSite precision conditions should include all sources of variation that are typically encountered during normal, long term ope

38、rationof the measurement system. Thus, all operators who are involved in the routine use of the measurement system should contributeresults to the site precision determination. If multiple results are obtained within a 24h period, then it is recommended that thenumber of results used in site precisi

39、on calculations be increased to capture the longer term variation in the system.3.2.12 site precision standard deviation, nthe standard deviation of results obtained under site precision conditions.3.2.13 validation audit sample, na QC sample or check standard used to verify precision and bias estim

40、ated from routinequality assurance testing.3.3 Symbols:3.3.1 ARVaccepted reference value.3.3.2 EWMAexponentially weighted moving average.3.3.3 Iindividual observation (as in I-chart).3.3.4 MRmoving range.3.3.5 MRaverage of moving range.3.3.6 QCquality control.3.3.7 Rsite precision.3.3.8 SEVsite expe

41、cted value.3.3.9 Rsite precision standard deviation.3.3.10 VAvalidation audit.3.3.11 2chi squared.3.3.12 lambda.4. Summary of Practice4.1 QC samples and check standards are regularly analyzed by the measurement system. Control charts and other statisticaltechniques are presented to screen, plot, and

42、 interpret test results in accordance with industry-accepted practices to ascertain thein-statistical-control status of the measurement system.D6299 1334.2 Statistical estimates of the measurement system precision and bias are calculated and periodically updated using accrueddata.4.3 In addition, as

43、 part of a separate validation audit procedure, QC samples and check standards may be submitted blind ordouble-blind and randomly to the measurement system for routine testing to verify that the calculated precision and bias arerepresentative of routine measurement system performance when there is n

44、o prior knowledge of the expected value or samplestatus.5. Significance and Use5.1 This practice can be used to continuously demonstrate the proficiency of analytical measurement systems that are used forestablishing and ensuring the quality of petroleum and petroleum products.5.2 Data accrued, usin

45、g the techniques included in this practice, provide the ability to monitor analytical measurement systemprecision and bias.5.3 These data are useful for updating test methods as well as for indicating areas of potential measurement systemimprovement.6. Reference Materials6.1 QC samples are used to e

46、stablish and monitor the precision of the analytical measurement system.6.1.1 Select a stable and homogeneous material having physical or chemical properties, or both, similar to those of typicalsamples tested by the analytical measurement system.NOTE 5When the QC sample is to be utilized for monito

47、ring a process stream analyzer performance, it is often helpful to supplement the processanalyzer system with a subsystem to automate the extraction, mixing, storage, and delivery functions associated with the QC sample.6.1.2 Estimate the quantity of the material needed for each specific lot of QC s

48、ample to (1) accommodate the number ofanalytical measurement systems for which it is to be used (laboratory test apparatuses as well as process stream analyzer systems)and (2) provide determination of QC statistics for a useful and desirable period of time.6.1.3 Collect the material into a single co

49、ntainer and isolate it.6.1.4 Thoroughly mix the material to ensure homogeneity.6.1.5 Conduct any testing necessary to ensure that the QC sample meets the characteristics for its intended use.6.1.6 Package or store QC samples, or both, as appropriate for the specific analytical measurement system to ensure that allanalyses of samples from a given lot are performed on essentially identical material. If necessary, split the bulk material collectedin 6.1.3 into separate and smaller containers to help ensure integrity over