ASTM_D_6122_-_22.pdf

Designation:D612222Standard Practice forValidation of the Performance of Multivariate Online,At-Line,Field and Laboratory Infrared Spectrophotometer,andRaman Spectrometer Based Analyzer Systems1This standard is issued under the fixed designation D6122;the number immediately following the 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.INTRODUCTIONOperation of a laboratory or process stream analyzer system typically involves five sequentialactivities.(1)CorrelationPrior to the initiation of the procedures described in this practice,amultivariate model is derived which relates the spectrum produced by the analyzer to the Primary TestMethod Result(PTMR).(1a)If the analyzer and Primary Test Method(PTM)measure the samematerial,then the multivariate model directly relates the spectra to PTMR collected on the samesamples.Alternatively(1b)if the analyzer measures the spectra of a material that is subjected totreatment prior to being measured by the PTM,then the multivariate model relates the spectra ofthe untreated sample to the PTMR for the same sample after treatment.(2)Analyzer QualificationWhen an analyzer is initially installed,or after major maintenance has been performed,diagnostictesting is performed to demonstrate that the analyzer meets the manufacturers specifications andhistorical performance standards.These diagnostic tests may require that the analyzer be adjusted soas to provide predetermined output levels for certain reference materials(3)Local ValidationAlocal validation is performed using an independent but limited set of materials that were not part ofthe correlation activity.This local validation is intended to demonstrate that the agreement between thePredicted Primary Method Test Results(PPTMRs)and the PTMRs are consistent with expectationsbased on the multivariate model.(4)General ValidationAfter an adequate number of PPTMRs andPTMRs have been accrued on materials that were not part of the correlation activity and whichadequately span the multivariate model compositional space,a comprehensive statistical assessmentcan be performed to demonstrate that the PPTMRs agree with the PTMRs to within user-specifiedrequirements.(5)Continual ValidationSubsequent to a successful local or general validation,quality assurance control chart monitoring of the differences between PPTMR and PTMR is conductedduring normal operation of the process analyzer system to demonstrate that the agreement between thePPTMRs and the PTMRs established during the General Validation is maintained.This practice dealswith the third,fourth,and fifth of these activities.“Correlation where analyzer measures a material which is subjected to treatment before beingmeasured by the PTM”as outlined in this practice can be applied to biofuels where the biofuelmaterial is added at a terminal or other facility and not included in the process stream material sampledby the analyzer at the basestock manufacturing facility.The“treatment”shall be a constant percentageaddition of the biofuels material to the basestock material.The correlation is deemed valid only forthe specific percentage addition and type of biofuel material used in its development.1.Scope*1.1 This practice covers requirements for the validation ofmeasurements made by laboratory,field,or process(online orat-line)infrared(near-or mid-infrared analyzers,or both),andRaman analyzers,used in the calculation of physical,chemical,or quality parameters(that is,properties)of liquid petroleumproducts and fuels.The properties are calculated from spectro-scopic data using multivariate modeling methods.The require-ments include verification of adequate instrument performance,verification of the applicability of the calibration model to thespectrum of the sample under test,and verification that theuncertainties associated with the degree of agreement between*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 principles 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.1the results calculated from the infrared or Raman measure-ments and the results produced by the PTM used for thedevelopment of the calibration model meets user-specifiedrequirements.Initially,a limited number of validation samplesrepresentative of current production are used to do a localvalidation.When there is an adequate number of validationsamples with sufficient variation in both property level andsample composition to span the model calibration spac