ASTM D6299-2017a red 3750 Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance《采用统计质量保.pdf

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1、Designation: D6299 17D6299 17a 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. Scope*1.1 This practice covers info

3、rmation for the design and operation of a program to monitor and control ongoing stability andprecision and bias performance of selected analytical measurement systems using a collection of generally accepted statisticalquality control (SQC) procedures and tools.NOTE 1A complete list of criteria for

4、 selecting measurement systems to which this practice should be applied and for determining the frequency atwhich it should be applied is beyond the scope of this practice. However, some factors to be considered include (1) frequency of use of the analyticalmeasurement system, (2) criticality of the

5、 parameter being measured, (3) system stability and precision performance based on historical data, (4) businesseconomics, and (5) regulatory, contractual, or test method requirements.1.2 This practice is applicable to stable analytical measurement systems that produce results on a continuous numeri

6、cal 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 practice is applicable to monitoring the differences between two analytical measurement systems that purport tomeasure the same property provided that b

7、oth systems have been assessed in accordance with the statistical methodology inPractice D6708 and the appropriate bias applied.NOTE 2For validation 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 va

8、lidated process stream analyzers.1.6 This practice assumes that the normal (Gaussian) model is adequate for the description and prediction of measurementsystem behavior when it is in a state of statistical control.NOTE 4For non-Gaussian processes, transformations of test results may permit proper ap

9、plication of these tools. Consult a statistician for furtherguidance and information.1.7 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guid

10、es and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D3764 Practice for Validation of the Performance of Process Stream Analyzer SystemsD5191 Test Method for Vapor Pressure of Petroleum Products (Mini Meth

11、od)D6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purportto Measure the Same Property of a MaterialD6792 Practice for Quality Management Systems in Petroleum Products, Liquid Fuels, and Lubricants Testing LaboratoriesD7372 Guide for Anal

12、ysis 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 Observations1 This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants

13、 and is the direct responsibility of SubcommitteeD02.94 on Coordinating Subcommittee on Quality Assurance and Statistics.Current edition approved Jan. 1, 2017Nov. 15, 2017. Published January 2017November 2017. Originally approved in 1998. Last previous edition approved in 20162017as D6299 16.D6299 1

14、7. DOI: 10.1520/D6299-17.10.1520/D6299-17A.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.This document is n

15、ot 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 appropria

16、te. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E

17、456 Terminology Relating to Quality and StatisticsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 accepted reference value, na value that serves as an agreed-upon reference for comparison and that is derived as (1)

18、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 Institute of Standards and Technology (NIST), or (3) a consensus value,based on collaborative experimental wor

19、k 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 assignable cause, na factor that contributes to variation and that is feasible to detect and identify. E4563.1.4

20、 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 limits, nlimits on a control chart that are used as criteria for signaling the need for action or for judging wh

21、ethera 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 uniform for samplingpurposes. E4563.1.7 precision, nthe closeness of agreement between test results obtained unde

22、r 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 operator with the same equipment within short intervals of time, using test specimens taken atrandom from a single

23、 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 from the same sample of material.3.2 Definitions of Terms Specific to This Standard:3.2.1 analytical measur

24、ement 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 used to determine a quantitativevalue of a specific property for an unknown sample in accordance with a tes

25、t 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 multiple instruments being used for the same test method provided there is nostatistically observable bias and

26、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 to the person performing the analysis.3.2.3 check standard, nin QC testing, a material having an accepted ref

27、erence 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 to a nationally recognizedbody or a material that has an accepted reference value established through interla

28、boratory 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 serve as a check standard. Users should be aware that for measurement systems that show matrixdependencies,

29、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 of generally numerous factors, individually ofrelatively small importance, that contributes to variation, a

30、nd 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 and expected value to the person performing the analysis.D6299 17a23.2.6 in-statistical-control, adja proces

31、s, analytical measurement system, or function that exhibits variations that can only beattributable to common cause.3.2.7 out-of-statistical-control, adja process, analytical measurement system, or function that exhibits variations in additionto those that can be attributable to common cause and the

32、 magnitude of these additional variations exceed specified limits.3.2.8 proficiency testing, ndetermination of a laboratorys testing capability by participation in an interlaboratory crosscheckprogram.3.2.8.1 DiscussionASTM Committee D02 conducts proficiency testing among hundreds of laboratories, u

33、sing a wide variety of petroleum productsand lubricants.3.2.9 quality control (QC) sample, nfor use in quality assurance programs to determine and monitor the precision and stabilityof a measurement system, a stable and homogeneous material having physical or chemical properties, or both, similar to

34、 those oftypical samples tested by the analytical measurement system. The material is properly stored to ensure sample integrity, and isavailable in sufficient quantity for repeated, long term testing.3.2.10 site expected value (SEV), nfor a QC sample this is an estimate of the theoretical limiting

35、value towards which theaverage of results collected from a single in-statistical-control measurement system under site precision conditions tends as thenumber of results approaches infinity.3.2.10.1 DiscussionThe SEV is associated with a single measurement system; for control charts that are plotted

36、 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 chart specific to a batchof QC material are constructed.3.2.11 site precision (R), nthe value below which the absolute difference between two individual test

37、 results obtained undersite precision conditions may be expected to occur with a probability of approximately 0.95 (95 %). It is defined as 2.77 times R,the standard deviation of results obtained under site precision conditions.3.2.12 site precision conditions, nconditions under which test results a

38、re obtained by one or more operators in a single sitelocation practicing the same test method on a single measurement system which may comprise multiple instruments, using testspecimens taken at random from the same sample of material, over an extended period of time spanning at least a 15 day inter

39、val.3.2.12.1 DiscussionSite precision conditions should include all sources of variation that are typically encountered during normal, long term operationof the measurement system. Thus, all operators who are involved in the routine use of the measurement system should contributeresults to the site

40、precision determination. If multiple results are obtained within a 24-h period, then only results separated by atleast 4 h should be used in site precision calculations in order to reflect the longer term variation in the system.3.2.13 site precision standard deviation, nthe standard deviation of re

41、sults obtained under site precision conditions.3.2.14 validation audit sample, na QC sample or check standard used to verify precision and bias estimated from routinequality assurance testing.3.3 Symbols:3.3.1 ARVaccepted reference value.3.3.2 EWMAexponentially weighted moving average.3.3.3 Iindivid

42、ual 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 expected value.3.3.9 Rsite precision standard deviation.3.3.10 VAvalidation audit.3.3.11 2chi squared.D6299 17a33.3.12 lambda.4. Summary of Practice4.1 QC

43、samples and check standards are regularly analyzed by the measurement system. Control charts and other statisticaltechniques are presented to screen, plot, and interpret test results in accordance with industry-accepted practices to ascertain thein-statistical-control status of the measurement syste

44、m.4.2 Statistical estimates of the measurement system precision and bias are calculated and periodically updated using accrueddata.4.3 In addition, as part of a separate validation audit procedure, QC samples and check standards may be submitted blind ordouble-blind and randomly to the measurement s

45、ystem for routine testing to verify that the calculated precision and bias arerepresentative of routine measurement system performance when there is no prior knowledge of the expected value or samplestatus.5. Significance and Use5.1 This practice can be used to continuously demonstrate the proficien

46、cy of analytical measurement systems that are used forestablishing and ensuring the quality of petroleum and petroleum products.5.2 Data accrued, using the techniques included in this practice, provide the ability to monitor analytical measurement systemprecision and bias.5.3 These data are useful f

47、or updating test methods as well as for indicating areas of potential measurement systemimprovement.6. Reference Materials6.1 QC samples are used to establish and monitor the precision of the analytical measurement system.6.1.1 Select a stable and homogeneous material having physical or chemical pro

48、perties, or both, similar to those of typicalsamples tested by the analytical measurement system.NOTE 5When the QC sample is to be utilized for monitoring a process stream analyzer performance, it is often helpful to supplement the processanalyzer system with a subsystem to automate the extraction,

49、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 sample 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 container and isolate it.6.1.4 Thoroughly mix the material to ensure homogeneit