1、Designation: D3764 13Standard Practice forValidation of the Performance of Process Stream AnalyzerSystems1This standard is issued under the fixed designation D3764; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONOperation of a process stream analyzer system typically involves four sequential activities.(1) Analyzer Calibration When an
3、 analyzer is initially installed, or after major maintenance hasbeen performed, diagnostic testing is performed to demonstrate that the analyzer meets themanufacturers specifications and historical performance standards.These diagnostic tests may requirethat the analyzer be adjusted so as to provide
4、 predetermined output levels for certain referencematerials. (2) CorrelationOnce the diagnostic testing is completed, process stream samples areanalyzed using the analyzer system. For application where the process analyzer system results arerequired to agree with results produced from an independent
5、 (primary) test method (PTM), amathematical function is derived that relates the analyzer results to the primary test method results(PTMR). The application of this mathematical function to an analyzer result produces a predictedprimary test method result (PPTMR). (3) Probationary ValidationAfter the
6、 correlation relation-ship between the analyzer results and primary test method results has been established, a probationaryvalidation is performed using an independent but limited set of materials that were not part of thecorrelation activity. This probationary validation is intended to demonstrate
7、 that the PPTMRs agreewith the PTMRs to within user-specified requirements for the analyzer system application. (4)General and Continual ValidationAfter an adequate amount of PPTMRs and PTMRs have beenaccrued on materials that were not part of the correlation activity, a comprehensive statisticalass
8、essment is performed to demonstrate that the PPTMRs agree with the PTMRs to within thetolerances established from the correlation activities. Subsequent to a successful general validation,quality assurance control chart monitoring of the differences between PPTMR and PTMR is conductedduring normal o
9、peration of the process analyzer system to demonstrate that the agreement between thePPTMRs and PTMRs established in the General Validation is maintained. This practice deals with thethird and fourth of these activities.1. Scope*1.1 This practice describes procedures and methodologiesbased on the st
10、atistical principles of Practice D6708 to validatewhether the degree of agreement between the results producedby a total analyzer system (or its subsystem), versus the resultsproduced by an independent test method that purports tomeasure the same property, meets user-specified requirements.This is a
11、 performance-based validation, to be conducted usinga set of materials that are not used a priori in the developmentof any correlation between the two measurement systems underinvestigation. A result from the independent test method isherein referred to as a Primary Test Method Result (PTMR).1.2 Thi
12、s practice assumes any correlation necessary tomitigate systemic biases between the analyzer system and PTMhave been applied to the analyzer results. See Guide D7235 forprocedures for establishing such correlations.1.3 This practice requires that both the primary methodagainst which the analyzer is
13、compared to, and the analyzersystem under investigation, are in statistical control. Practicesdescribed in Practice D6299 should be used to ensure thiscondition is met.1.4 This practice applies if the process stream analyzersystem and the primary test method are based on the samemeasurement principl
14、e(s), or, if the process stream analyzersystem uses a direct and well-understood measurement prin-ciple that is similar to the measurement principle of the primary1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Su
15、bcommittee D02.25 onPerformance Assessment and Validation of Process Stream Analyzer Systems.Current edition approved May 1, 2013. Published June 2013. Originallyapproved in 1980. Last previous edition approved in 2009 as D3764 09. DOI:10.1520/D3764-13.*A Summary of Changes section appears at the en
16、d of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1test method. This practice also applies if the process streamanalyzer system uses a different measurement technology fromthe primary test method, provided that the cali
17、bration protocolfor the direct output of the analyzer does not require use of thePTMRs (see Case 1 in Note 1).1.5 This practice does not apply if the process streamanalyzer system utilizes an indirect or mathematically modeledmeasurement principle such as chemometric or multivariateanalysis techniqu
18、es where PTMRs are required for the chemo-metric or multivariate model development. Users should referto Practice D6122 for detailed validation procedures for thesetypes of analyzer systems (see Case 2 in Note 1).NOTE 1For example, for the measurement of benzene in sparkignition fuels, comparison of
19、 a Mid-Infrared process analyzer systembased on Test Method D6277 to a Test Method D3606 gas chromatogra-phy primary test method would be considered Case 1, and this practicewould apply. For each sample, the Mid-Infrared spectrum is convertedinto a single analyzer result using methodology (Test Meth
20、od D6277) thatis independent of the primary test method (Test Method D3606). However,when the same analyzer uses a multivariate model to correlate themeasured Mid-Infrared spectrum to Test Method D3606 reference valuesusing the methodology of Practice E1655, it is considered Case 2 andPractice D6122
21、 applies. In this case 2 example, the direct output of theanalyzer is the spectrum, and the conversion of this multivariate output toan analyzer result require use of Practice D6122, hence it is notindependent of the primary test method.1.6 Performance Validation is conducted by calculating thepreci
22、sion and bias of the differences between results from theanalyzer system (or subsystem) after the application of anynecessary correlation, (such results are herein referred to asPredicted Primary Test Method Results (PPTMRs), versus thePTMRs for the same sample set. Results used in the calculationar
23、e for samples that are not used in the development of thecorrelation. The calculated precision and bias are statisticallycompared to user-specified requirements for the analyzersystem application.1.6.1 For analyzers used in product release or productquality certification applications, the precision
24、and bias re-quirement for the degree of agreement are typically based onthe site or published precision of the Primary Test Method.NOTE 2In most applications of this type, the PTM is the specification-cited test method.1.6.2 This practice does not describe procedures for estab-lishing precision and
25、bias requirements for analyzer systemapplications. Such requirements must be based on the critical-ity of the results to the intended business application and oncontractual and regulatory requirements. The user must estab-lish precision and bias requirements prior to initiating thevalidation procedu
26、res described herein.1.7 Two procedures for validation are described: the linesample procedure and the validation reference material (VRM)injection procedure.1.8 Only the analyzer system or subsystem downstream ofthe VRM injection point or the line sample extraction point isbeing validated by this p
27、ractice.1.9 The line sample procedure is limited to applicationswhere material can be safely withdrawn from the samplingpoint of the analyzer unit without significantly altering theproperty of interest.1.10 Validation information obtained in the application ofthis practice is applicable only to the
28、type and property rangeof the materials used to perform the validation.1.11 Two types of validation are described: GeneralValidation, and Level Specific Validation. These are typicallyconducted at installation or after major maintenance once thesystem mechanical fitness-for-use has been established.
29、1.11.1 General Validation is based on the statistical prin-ciples and methodology of Practice D6708. In most cases,General Validation is preferred, but may not always be possibleif the variation in validation materials is insufficient. GeneralValidation will validate analyzer operation over a wider
30、oper-ating range than Level Specific Validation.1.11.2 When the variation in available validation materialsis insufficient to satisfy the requirements of Practice D6708,aLevel Specific Validation is done to validate analyzer operationover a limited range.1.11.3 The validation outcome are considered
31、valid onlywithin the range covered by the validation material Data fromseveral different Validations (general or level-specific) canpotentially be combined for use in a General Validation.1.12 Procedures for the continual validation of systemperformance are described. These procedures are typicallya
32、pplied at a frequency commensurate with the criticality of theapplication.1.13 This practice does not address procedures for diagnos-ing causes of validation failure.1.14 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of
33、the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1265 Practice for Sampling Liquefied Petroleum (LP)Gases, Manual MethodD3606 Test Method for Determinati
34、on of Benzene andToluene in Finished Motor and Aviation Gasoline by GasChromatographyD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD5842 Practice for Sampling and Handling of Fuels forVolatility Measuremen
35、tD6122 Practice for Validation of the Performance of Multi-variate Online, At-Line, and Laboratory Infrared Spectro-photometer Based Analyzer SystemsD6277 Test Method for Determination of Benzene in Spark-Ignition Engine Fuels Using Mid Infrared SpectroscopyD6299 Practice for Applying Statistical Qu
36、ality Assurance2For 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 Summary page onthe ASTM website.D3764 132and Control Charting Techniques to Ev
37、aluate AnalyticalMeasurement System PerformanceD6708 Practice for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a MaterialD7235 Guide for Establishing a Linear Correlation Relation-ship Between Analyzer and Primary Te
38、st Method ResultsUsing Relevant ASTM Standard PracticesD7278 Guide for Prediction ofAnalyzer Sample System LagTimesD7453 Practice for Sampling of Petroleum Products forAnalysis by Process Stream Analyzers and for ProcessStream Analyzer System ValidationD7808 Practice for Determining the Site Precisi
39、on of aProcess Stream Analyzer on Process Stream MaterialE456 Terminology Relating to Quality and StatisticsE1655 Practices for Infrared Multivariate QuantitativeAnalysisF307 Practice for Sampling Pressurized Gas for Gas Analy-sis3. Terminology3.1 Definitions:3.1.1 accepted reference value (ARV), n
40、a value thatserves as an agreed-upon reference for comparison, and whichis derived as: (1) a theoretical or established value, based onscientific principles, (2) an assigned or certified value, based onexperimental work of some national or internationalorganization, or (3) a consensus or certified v
41、alue, based oncollaborative experimental work under the auspices of ascientific or engineering group. E4563.1.2 between-method reproducibility (RXY), na quantita-tive expression of the random error associated with thedifference between two results obtained by different operatorsusing different appar
42、atus and applying the two methods X andY, respectively, each obtaining a single result on an identicaltest sample, when the methods have been assessed and anappropriate bias-correction has been applied in accordancewith this practice; it is defined as the 95 % confidence limit forthe difference betw
43、een two such single and independentresults. D67083.1.2.1 DiscussionWithin the context of this practice, RXYis interpreted to be the 95 % confidence limit for the predictiondeviation between any single Primary Test Method Result(PTMR) and the Predicted Primary Test Method Result(PPTMR) produced by th
44、e analyzer system that is deemedacceptable on the assumption that both the analyzer system andprimary test method are in statistical control, and that thecorrelation relationship applied to the analyzer results toproduce the PPTMR is fit-for-purpose.3.1.3 precision, nthe closeness of agreement betwe
45、enindependent test results obtained under stipulated conditions.E4563.1.4 repeatability conditions, nconditions where inde-pendent test results are obtained with the same method onidentical test items in the same laboratory by the same operatorusing the same equipment within short intervals of time.
46、 E4563.1.5 reproducibility conditions, nconditions where testresults are obtained with the same method on identical testitems in different laboratories with different operators usingdifferent equipment. E4563.1.6 site precision conditions, nconditions under whichtest results are obtained by one or m
47、ore operators in a singlesite location practicing the same test method on a singlemeasurement system using test specimens taken at randomfrom the same sample of material, over an extended period oftime spanning at least a 15 day interval. D62993.1.6.1 DiscussionA measurement system may comprisemulti
48、ple instruments being used for the same test method.3.1.7 site precision, n2.77 times the standard deviation ofresults obtained under site precision conditions. D62993.2 Definitions of Terms Specific to This Standard:3.2.1 Analyzer System Items:3.2.1.1 analyzer output, na signal (pneumatic, electric
49、al,or digital), proportional to the property being measured that issuitable for readout or control instrumentation external to theanalyzer system.3.2.1.2 analyzer system result, nthe measured propertyreading, in the accepted property measurement units, that isdisplayed by the analyzer unit readout instrumentation ortransmitted to end user of the analyzer system.3.2.1.3 analyzer unit, nthe instrumental equipment neces-sary to automatically measure the physical or chemical prop-erty of a process or product stream sample using either anintermittent or a continuous t
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