ASTM_E_2056_-_04_2010.pdf

Designation:E205604(Reapproved 2010)Standard Practice forQualifying Spectrometers and Spectrophotometers for Usein Multivariate Analyses,Calibrated Using SurrogateMixtures1This standard is issued under the fixed designation E2056;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.1.Scope1.1 This practice relates to the multivariate calibration ofspectrometers and spectrophotometers used in determining thephysical and chemical characteristics of materials.A detaileddescription of general multivariate analysis is given in PracticeE1655.This standard refers only to those instances wheresurrogate mixtures can be used to establish a suitable calibra-tion matrix.This practice specifies calibration and qualificationdata set requirements for interlaboratory studies(ILSs),that is,round robins,of standard test methods employing surrogatecalibration techniques that do not conform exactly to PracticesE1655.NOTE1For some multivariate spectroscopic analyses,interferencesand matrix effects are sufficiently small that it is possible to calibrate usingmixtures that contain substantially fewer chemical components than thesamples that will ultimately be analyzed.While these surrogate methodsgenerally make use of the multivariate mathematics described in PracticesE1655,they do not conform to procedures described therein,specificallywith respect to the handling of outliers.1.2 This practice specifies how the ILS data is treated toestablish spectrometer/spectrophotometer performance qualifi-cation requirements to be incorporated into standard testmethods.NOTE2Spectrometer/spectrophotometer qualification procedures areintended to allow the user to determine if the performance of a specificspectrometer/spectrophotometer is adequate to conduct the analysis so asto obtain results consistent with the published test method precision.1.2.1 The spectroscopies used in the surrogate test methodswould include but not be limited to mid-and near-infrared,ultraviolet/visible,fluorescence and Raman spectroscopies.1.2.2 The surrogate calibrations covered in this practice are:multilinear regression(MLR),principal components regression(PCR)or partial least squares(PLS)mathematics.Thesecalibration procedures are described in detail in PracticesE1655.1.3 For surrogate test methods,this practice recommendslimitations that should be placed on calibration options that areallowed in the test method.Specifically,this practice recom-mends that the test method developer demonstrate that allcalibrations that are allowed in the test method producestatistically indistinguishable results.1.4 For surrogate test methods that reference spectrometer/spectrophotometer performance practices,such as PracticesE275,E925,E932,E958,E1421,E1683,or E1944;TestMethods E387,E388,or E579;or Guide E1866,this practicerecommends that instrument performance data be collected aspart of the ILS to establish the relationship betweenspectrometer/spectrophotometer performance and test methodprecision.2.Referenced Documents2.1 ASTM Standards:2D6277 Test Method for Determination of Benzene in Spark-Ignition Engine Fuels Using Mid Infrared SpectroscopyD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsE131 Terminology Relating to Molecular SpectroscopyE275 Practice for Describing and Measuring Performance ofUltraviolet and Visible SpectrophotometersE387 Test Method for Estimating Stray Radiant Power Ratioof Dispersive Spectrophotometers by the Opaque FilterMethodE388 Test Method for Wavelength Accuracy and SpectralBandwidth of Fluorescence SpectrometersE579 Test Method for Limit of Detection of Fluorescence ofQuinine Sulfate in SolutionE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE925 Practice for Monitoring the Calibration of Ultraviolet-Visible Spectrophotometers whose Spectral Bandwidth1This practice is under the jurisdiction of ASTM Committee E13 on MolecularSpectroscopy and Separation Science and is the direct responsibility of Subcom-mittee E13.11 on Multivariate Analysis.Current edition approved March 1,2010.Published May 2010.Originallyapproved in 1999.Last previous edition approved in 2004 as E2056 04.DOI:10.1520/E2056-04R10.2For 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 Summary page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 does not Exceed 2 nmE932 Practice for Describing and Measuring Performance ofDispersive Infrared SpectrometersE958 Practice for Measuring Practical Spectral Bandwidt