ASTM D6299-2017b 9375 Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance.pdf

1、Designation: D6299 17b 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 designat

2、ion 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 information

3、for the design andoperation of a program to monitor and control ongoing stabilityand precision and bias performance of selected analyticalmeasurement systems using a collection of generally acceptedstatistical quality control (SQC) procedures and tools.NOTE 1A complete list of criteria for selecting

4、 measurement systemsto which this practice should be applied and for determining the frequencyat which it should be applied is beyond the scope of this practice.However, some factors to be considered include (1) frequency of use ofthe analytical measurement system, (2) criticality of the parameter b

5、eingmeasured, (3) system stability and precision performance based onhistorical data, (4) business economics, and (5) regulatory, contractual, ortest method requirements.1.2 This practice is applicable to stable analytical measure-ment systems that produce results on a continuous numericalscale.1.3

6、This practice is applicable to laboratory test methods.1.4 This practice is applicable to validated process streamanalyzers.1.5 This practice is applicable to monitoring the differencesbetween two analytical measurement systems that purport tomeasure the same property provided that both systems have

7、been assessed in accordance with the statistical methodology inPractice D6708 and the appropriate bias applied.NOTE 2For validation of univariate process stream analyzers, see alsoPractice D3764.NOTE 3One or both of the analytical systems in 1.5 can be laboratorytest methods or validated process str

8、eam analyzers.1.6 This practice assumes that the normal (Gaussian) modelis 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 resultsmay permit proper application of these to

9、ols. Consult a statistician forfurther guidance and information.1.7 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendat

10、ions issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D3764 Practice for Validation of the Performance of ProcessStream Analyzer SystemsD5191 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini Method)D6708 Practice

11、for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a MaterialD6792 Practice for Quality Management Systems in Petro-leum Products, Liquid Fuels, and Lubricants TestingLaboratoriesD7372 Guide for Analysis and Interpreta

12、tion of ProficiencyTest Program ResultsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE178 Practice for Dealing With Outlying ObservationsE456 Terminology Relating to Quality and StatisticsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a

13、Test Method3. Terminology3.1 Definitions:3.1.1 accepted reference value, na value that serves as anagreed-upon reference for comparison and that is derived as (1)a theoretical or established value, based on scientific principles,(2) an assigned value, based on experimental work of some1This practice

14、 is under the jurisdiction of ASTM Committee D02 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.94 on Coordinating Subcommittee on Quality Assurance and Statistics.Current edition approved Dec. 15, 2017. Published March 2018. Originallyapprov

15、ed in 1998. Last previous edition approved in 2017 as D6299 17a. DOI:10.1520/D6299-17B.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summar

16、y page onthe ASTM website.*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 StatesThis international standard was developed in accordance with internationally recognized principl

17、es on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1national or international organization, such as the U.S. Na-tional Institute o

18、f Standards and Technology (NIST), or (3)aconsensus value, based on collaborative experimental workunder the auspices of a scientific or engineering group. E177,E4563.1.2 accuracy, nthe closeness of agreement between anobserved value and an accepted reference value. E177, E4563.1.3 assignable cause,

19、 na factor that contributes to varia-tion and that is feasible to detect and identify. E4563.1.4 bias, na systematic error that contributes to thedifference between a population mean of the measurements ortest results and an accepted reference or true value. E177, E4563.1.5 control limits, nlimits o

20、n a control chart that areused as criteria for signaling the need for action or for judgingwhether a set of data does or does not indicate a state ofstatistical control. E4563.1.6 lot, na definite quantity of a product or materialaccumulated under conditions that are considered uniform forsampling p

21、urposes. E4563.1.7 precision, nthe closeness of agreement between testresults obtained under prescribed conditions. E4563.1.8 repeatability conditions, nconditions where mutu-ally independent test results are obtained with the same testmethod in the same laboratory by the same operator with thesame

22、equipment within short intervals of time, using testspecimens taken at random from a single sample of material.3.1.9 reproducibility conditions, nconditions under whichtest results are obtained in different laboratories with the sametest method, using test specimens taken at random from thesame samp

23、le of material.3.2 Definitions of Terms Specific to This Standard:3.2.1 analytical measurement system, na collection of oneor more components or subsystems, such as samplers, testequipment, instrumentation, display devices, data handlers,printouts or output transmitters, that is used to determine aq

24、uantitative value of a specific property for an unknownsample in accordance with a test method.3.2.1.1 DiscussionA standard test method (for example,ASTM, ISO) is an example of an analytical measurementsystem.3.2.1.2 DiscussionAn analytical measurement systemmay comprise multiple instruments being u

25、sed for the sametest method provided there is no statistically observable biasand precision differences between the multiple instruments.3.2.2 blind submission, nsubmission of a check standardor quality control (QC) sample for analysis without revealingthe expected value to the person performing the

26、 analysis.3.2.3 check standard, nin QC testing, a material having anaccepted reference value used to determine the accuracy of ameasurement system.3.2.3.1 DiscussionA check standard is preferably a mate-rial that is either a certified reference material with traceabilityto a nationally recognized bo

27、dy or a material that has anaccepted reference value established through interlaboratorytesting. For some measurement systems, a pure, single com-ponent material having known value or a simple gravimetric orvolumetric mixture of pure components having calculablevalue may serve as a check standard. U

28、sers should be awarethat for measurement systems that show matrix dependencies,accuracy determined from pure compounds or simple mixturesmay not be representative of that achieved on actual samples.3.2.4 common (chance, random) cause, nfor quality as-surance programs, one of generally numerous facto

29、rs, individu-ally of relatively small importance, that contributes tovariation, and that is not feasible to detect and identify.3.2.5 double blind submission, nsubmission of a checkstandard or QC sample for analysis without revealing the checkstandard or QC sample status and expected value to the pe

30、rsonperforming the analysis.3.2.6 in-statistical-control, adja process, analytical mea-surement system, or function that exhibits variations that canonly be attributable to common cause.3.2.7 out-of-statistical-control, adja process, analyticalmeasurement system, or function that exhibits variations

31、 inaddition to those that can be attributable to common cause andthe magnitude of these additional variations exceed specifiedlimits.3.2.8 proficiency testing, ndetermination of a laboratorystesting capability by participation in an interlaboratory cross-check program.3.2.8.1 DiscussionASTM Committe

32、e D02 conducts pro-ficiency testing among hundreds of laboratories, using a widevariety of petroleum products and lubricants.3.2.9 quality control (QC) sample, nfor use in qualityassurance programs to determine and monitor the precision andstability of a measurement system, a stable and homogeneousm

33、aterial having physical or chemical properties, or both,similar to those of typical samples tested by the analyticalmeasurement system. The material is properly stored to ensuresample integrity, and is available in sufficient quantity forrepeated, long term testing.3.2.10 site expected value (SEV),

34、nfor a QC sample this isan estimate of the theoretical limiting value towards which theaverage of results collected from a single in-statistical-controlmeasurement system under site precision conditions tends asthe number of results approaches infinity.3.2.10.1 DiscussionThe SEV is associated with a

35、 singlemeasurement system; for control charts that are plotted inactual measured units, the SEV is required, since it is used asa reference value from which upper and lower control limits forthe control chart specific to a batch of QC material areconstructed.3.2.11 site precision (R), nthe value bel

36、ow which theabsolute difference between two individual test results obtainedunder site precision conditions may be expected to occur witha probability of approximately 0.95 (95 %). It is defined as 2.77times R, the standard deviation of results obtained under siteprecision conditions.3.2.12 site pre

37、cision conditions, nconditions under whichtest results are obtained by one or more operators in a singlesite location practicing the same test method on a singleD6299 17b2measurement system which may comprise multipleinstruments, using test specimens taken at random from thesame sample of material,

38、over an extended period of timespanning at least a 15 day interval.3.2.12.1 DiscussionSite precision conditions should in-clude all sources of variation that are typically encounteredduring normal, long term operation of the measurement sys-tem. Thus, all operators who are involved in the routine us

39、e ofthe measurement system should contribute results to the siteprecision determination. In situations of high usage of a testmethod where multiple QC results are obtained within a 24 hperiod, then only results separated by at least 4 h to 8 h,depending on the absence of auto-correlation in the data

40、, thenature of the test method/instrument, site requirements, orregulations, should be used in site precision calculations toreflect the longer term variation in the system.3.2.13 site precision standard deviation, nthe standarddeviation of results obtained under site precision conditions.3.2.14 val

41、idation audit sample, na QC sample or checkstandard used to verify precision and bias estimated fromroutine quality 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

42、 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.3.3.12 lambda.4. Summary of Practice4.1 QC samples and check standards are regularly analyzedby the measurement

43、 system. Control charts and other statisticaltechniques are presented to screen, plot, and interpret testresults in accordance with industry-accepted practices to as-certain the in-statistical-control status of the measurementsystem.4.2 Statistical estimates of the measurement system preci-sion and

44、bias are calculated and periodically updated usingaccrued data.4.3 In addition, as part of a separate validation auditprocedure, QC samples and check standards may be submittedblind or double-blind and randomly to the measurement systemfor routine testing to verify that the calculated precision andb

45、ias are representative of routine measurement system perfor-mance when there is no prior knowledge of the expected valueor sample status.5. Significance and Use5.1 This practice can be used to continuously demonstratethe proficiency of analytical measurement systems that areused for establishing and

46、 ensuring the quality of petroleum andpetroleum products.5.2 Data accrued, using the techniques included in thispractice, provide the ability to monitor analytical measurementsystem precision and bias.5.3 These data are useful for updating test methods as wellas for indicating areas of potential mea

47、surement system im-provement.6. Reference Materials6.1 QC samples are used to establish and monitor theprecision of the analytical measurement system.6.1.1 Select a stable and homogeneous material havingphysical or chemical properties, or both, similar to those oftypical samples tested by the analyt

48、ical measurement system.NOTE 5When the QC sample is to be utilized for monitoring a processstream 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

49、 Estimate the quantity of the material needed for eachspecific 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 analyzersystems) and (2) provide determination of QC statistics for auseful and desirable period of time.6.1.3 Collect the material into a single container and isolateit.6.1.4 Thoroughly mix the material to ensure homogeneity.6.1.5 Conduct any testing necessary to ensure that the QCsample meets the character