1、Designation: D 3764 09Standard Practice forValidation of the Performance of Process Stream AnalyzerSystems1This standard is issued under the fixed designation D 3764; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、 revision. 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 CalibrationWhen a
3、n 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 provid
4、e 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 independen
5、t (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 th
6、e 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 demonstrat
7、e that the PPTMRs agreewith the PTMRs to within user-specified requirements for the analyzer system application. (4) Gen-eral and Continual ValidationAfter an adequate amount of PPTMRs and PTMRs have beenaccrued on materials that were not part of the correlation activity, a comprehensive statistical
8、assessment 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 norma
9、l operation 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. Scope1.1 This practice describes procedures and methodologiesbased on the
10、statistical principles of Practice D 6708 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 i
11、s a 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
12、This practice assumes any correlation necessary tomitigate systemic biases between the analyzer system and PTMhave been applied to the analyzer results.1.3 This practice requires that both the primary methodagainst which the analyzer is compared to, and the analyzersystem under investigation, are in
13、 statistical control. Practicesdescribed in Practice D 6299 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 principle(s), or, if the process stream analyzersystem uses a direct a
14、nd well-understood measurement prin-ciple that is similar to the measurement principle of the primarytest method. This practice also applies if the process stream1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Sub
15、committee D02.25 onPerformance Assessment and Validation of Process Stream Analyzer Systems.Current edition approved June 1, 2009. Published July 2009. Originally approvedin 1980. Last previous edition approved in 2006 as D 3764061.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, W
16、est Conshohocken, PA 19428-2959, United States.analyzer system uses a different measurement technology fromthe primary test method, provided that the calibration 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
17、the process streamanalyzer system utilizes an indirect or mathematically modeledmeasurement principle such as chemometric or multivariateanalysis techniques where PTMRs are required for the chemo-metric or multivariate model development. Users should referto Practice D 6122 for detailed validation p
18、rocedures for thesetypes of analyzer systems (see Case 2 in Note 1).NOTE 1For example, for the measurement of benzene in sparkignition fuels, comparison of a Mid-Infrared process analyzer systembased on Test Method D 6277 to a Test Method D 3606 gas chromatog-raphy primary test method would be consi
19、dered Case 1, and this practicewould apply. For each sample, the Mid-Infrared spectrum is convertedinto a single analyzer result using methodology (Test Method D 6277) thatis independent of the primary test method (Test Method D 3606).However, when the same analyzer uses a multivariate model to corr
20、elatethe measured Mid-Infrared spectrum to Test Method D 3606 referencevalues using the methodology of Practice E 1655, it is considered Case 2and Practice D 6122 applies. In this case 2 example, the direct output ofthe analyzer is the spectrum, and the conversion of this multivariate outputto an an
21、alyzer result require use of Practice D 6122, hence it is notindependent of the primary test method.1.6 Performance Validation is conducted by calculating theprecision and bias of the differences between results from theanalyzer system (or subsystem) after the application of anynecessary correlation
22、, (such results are herein referred to asPredicted Primary Test Method Results (PPTMRs), versus thePTMRs for the same sample set. Results used in the calculationare for samples that are not used in the development of thecorrelation. The calculated precision and bias are statisticallycompared to user
23、-specified requirements for the analyzersystem application.1.6.1 For analyzers used in product release or productquality certification applications, the precision and bias re-quirement for the degree of agreement are typically based onthe site or published precision of the Primary Test Method.NOTE 2
24、In 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 bias requirements for analyzer systemapplications. Such requirements must be based on the critical-ity of the results to the intended bus
25、iness application and oncontractual and regulatory requirements. The user must estab-lish precision and bias requirements prior to initiating thevalidation procedures described herein.1.7 Two procedures for validation are described: the linesample procedure and the validation reference material (VRM
26、)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 practice.1.9 The line sample procedure is limited to applicationswhere material can be safely withdrawn from the samplingpoint of the anal
27、yzer unit without significantly altering theproperty of interest.1.10 Validation information obtained in the application ofthis practice is applicable only to the type and property rangeof the materials used to perform the validation.1.11 Two types of validation are described: General Valida-tion, a
28、nd Level Specific Validation. These are typically con-ducted at installation or after major maintenance once thesystem mechanical fitness-for-use has been established.1.11.1 General Validation is based on the statistical prin-ciples and methodology of Practice D 6708. In most cases,General Validatio
29、n is preferred, but may not always be possibleif the variation in validation materials is insufficient. GeneralValidation will validate analyzer operation over a wider oper-ating range than Level Specific Validation.1.11.2 When the variation in available validation materialsis insufficient to satisf
30、y the requirements of Practice D 6708,aLevel Specific Validation is done to validate analyzer operationover a limited range.1.11.3 The validation outcome are considered valid onlywithin the range covered by the validation material Data fromseveral different Validations (general or level-specific) ca
31、npotentially be combined for use in a General Validation.1.12 Procedures for the continual validation of systemperformance are described. These procedures are typicallyapplied at a frequency commensurate with the criticality of theapplication.1.13 This practice does not address procedures for diagno
32、s-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 the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limi
33、tations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1265 Practice for Sampling Liquefied Petroleum (LP)Gases, Manual MethodD 3606 Test Method for Determination of Benzene andToluene in Finished Motor and Aviation Gasoline by GasChromatographyD 4057 Practice for Manual Sampling of Petro
34、leum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 5842 Practice for Sampling and Handling of Fuels forVolatility MeasurementD 6122 Practice for Validation of the Performance of Mul-tivariate Process Infrared SpectrophotometersD 6277 Test Method for
35、Determination of Benzene inSpark-Ignition Engine Fuels Using Mid Infrared Spectros-copyD 6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance2For referenced ASTM standards, visit the ASTM website, www.astm.org, o
36、rcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.D3764092D 6708 Practice for Statistical Assessment and Improve-ment of Expected Agreement Between Two Test Methodsthat Purport to Me
37、asure the Same Property of a MaterialE 456 Terminology Relating to Quality and StatisticsE 1655 Practices for Infrared Multivariate QuantitativeAnalysisF 307 Practice for Sampling Pressurized Gas for GasAnaly-sis2.2 ASTM Adjuncts:Software Program CompTM, adjunct to Practice D 670833. Terminology3.1
38、Definitions:3.1.1 accepted reference value (ARV), na 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 internati
39、onal organiza-tion, or (3) a consensus or certified value, based on collabora-tive experimental work under the auspices of a scientific orengineering group. E 4563.1.2 cross-method reproducibility (RXY), na quantitativeexpression of the random error associated with the differencebetween two results
40、obtained by different operators usingdifferent apparatus and applying the two methods X and Y,respectively, each obtaining a single result on an identical testsample, when the methods have been assessed and an appro-priate bias-correction has been applied in accordance with thispractice; it is defin
41、ed as the 95 % confidence limit for thedifference between two such single and independent results.D 67083.1.2.1 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 Pre
42、dicted Primary Test Method Result(PPTMR) produced by the 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-pur
43、pose.3.1.3 precision, nthe closeness of agreement betweenindependent test results obtained under stipulated conditions.E 4563.1.4 repeatability conditions, nconditions where inde-pendent test results are obtained with the same method onidentical test items in the same laboratory by the same operator
44、using the same equipment within short intervals of time.E 4563.1.5 reproducibility conditions, nconditions where testresults are obtained with the same method on identical testitems in different laboratories with different operators usingdifferent equipment. E 4563.1.6 site precision conditions, nco
45、nditions under whichtest results are obtained by one or more 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. D 62
46、993.1.6.1 DiscussionA measurement system may comprisemultiple 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. D 62993.2 Definitions of Terms Specific to This Standard:3.2.1 Analyzer System It
47、ems:3.2.1.1 analyzer output, na signal (pneumatic, electrical,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 measure
48、ment 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 nec-essary to automatically measure the physical or chemicalproperty of a process or product stream sample using either aninte
49、rmittent or a continuous technique.3.2.1.4 analyzer unit repeatability, n2.77 times the stan-dard deviation of results obtained from repetitive analysis ofthe same material directly injected into the analyzer unit underrepeatability conditions.3.2.1.5 continuous analyzer unit, nan analyzer that mea-sures the property value of a process or product stream on acontinuous basis and dynamically displays the instantaneouslyupdated analyzer output.3.2.1.6 intermittent analyzer unit, na cyclic type analyzerthat performs a measurement sequence on samples from aprocess o
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