ASTM_D_7371_-_14.pdf

Designation:D737114Standard Test Method forDetermination of Biodiesel(Fatty Acid Methyl Esters)Content in Diesel Fuel Oil Using Mid Infrared Spectroscopy(FTIR-ATR-PLS Method)1This standard is issued under the fixed designation D7371;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.Scope*1.1 This test method covers the determination of the contentof fatty acid methyl esters(FAME)biodiesel in diesel fuel oils.It is applicable to concentrations from 1.00 to 20 volume%(see Note 1).This procedure is applicable only to FAME.Biodiesel in the form of fatty acid ethyl esters(FAEE)willcause a negative bias.NOTE1Using the proper ATR sample accessory,the range maybeexpanded from 1 to 100 volume%,however precision data is not availableabove 20 volume%.1.2 The values stated in SI units of measurement are to beregarded as the standard.The values given in parentheses arefor information only.1.3 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 limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D975 Specification for Diesel Fuel OilsD976 Test Method for Calculated Cetane Index of DistillateFuelsD1298 Test Method for Density,Relative Density,or APIGravity of Crude Petroleum and Liquid Petroleum Prod-ucts by Hydrometer MethodD4052 Test Method for Density,Relative Density,and APIGravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD4737 Test Method for Calculated Cetane Index by FourVariable EquationD5854 Practice for Mixing and Handling of Liquid Samplesof Petroleum and Petroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6751 Specification for Biodiesel Fuel Blend Stock(B100)for Middle Distillate FuelsD7467 Specification for Diesel Fuel Oil,Biodiesel Blend(B6 to B20)E168 Practices for General Techniques of Infrared Quanti-tative Analysis(Withdrawn 2015)3E1655 Practices for Infrared Multivariate QuantitativeAnalysisE2056 Practice for Qualifying Spectrometers and Spectro-photometers for Use in Multivariate Analyses,CalibratedUsing Surrogate Mixtures3.Terminology3.1 Definitions:3.1.1 biodiesel,na fuel comprised of mono-alkyl esters oflong chain fatty acids derived from vegetable oils or animalfats,designated B100.D67513.1.2 biodiesel blend,BXX,na blend of biodiesel fuelwith petroleum-based diesel fuel.D74673.1.2.1 DiscussionIn the abbreviation BXX,the XX rep-resents the volume percentage of biodiesel fuel in the blend.D67513.1.3 diesel fuel,npetroleum-based middle distillate fuel.3.1.4 multivariate calibration,nprocess for creating amodel that relates component concentrations or properties tothe absorbances of a set of known reference samples at morethan one wavelength or frequency.E16551This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.04.0F on Absorption Spectroscopic Methods.Current edition approved Oct.1,2014.Published October 2014.Originallyapproved in 2007.Last previous edition approved in 2012 as D7371 12.DOI:10.1520/D7371-14.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.*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 States1 3.1.4.1 DiscussionThe resultant multivariate calibrationmodel is applied to the analysis of spectra of unknown samplesto provide an estimate of the component concentration orproperty values for the unknown sample.3.1.4.2 DiscussionThe multivariate calibration algorithmemployed in this test method is partial least square(PLS)asdefined in Practices E1655.3.2 Abbreviations:ATR=attenuated total reflectanceBxx=see 3.1.2FAEE=fatty acid ethyl estersFAME=fatty acid methyl estersFTIR=Fourier transform infraredmid-IR=mid infraredPLS=partial least squareULSD=ultra low sulfur diesel4.Summary of Test Method4.1 A sample of diesel fuel,biodiesel,or biodiesel blend isintroduced into a liquid attenuated total reflectance(ATR)sample cell.A beam of infrar