ASTM_D_7039_-_15a.pdf

Designation:D703915aStandard Test Method forSulfur in Gasoline,Diesel Fuel,Jet Fuel,Kerosine,Biodiesel,Biodiesel Blends,and Gasoline-Ethanol Blendsby Monochromatic Wavelength Dispersive X-rayFluorescence Spectrometry1This standard is issued under the fixed designation D7039;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 total sulfurby monochromatic wavelength-dispersive X-ray fluorescence(MWDXRF)spectrometry in single-phase gasoline,diesel fuel,refinery process streams used to blend gasoline and diesel,jetfuel,kerosine,biodiesel,biodiesel blends,and gasoline-ethanolblends.NOTE1Volatile samples such as high-vapor-pressure gasolines orlight hydrocarbons might not meet the stated precision because of theevaporation of light components during the analysis.1.2 The range of this test method is between the pooled limitof quantitation(PLOQ)value(calculated by procedures con-sistent with Practice D6259)of 3.2 mg kg total sulfur and thehighest level sample in the round robin,2822 mg kg totalsulfur.1.3 Samples containing oxygenates can be analyzed withthis test method provided the matrix of the calibration stan-dards is either matched to the sample matrices or the matrixcorrection described in Section 5 or AnnexA1 is applied to theresults.The conditions for matrix matching and matrix correc-tion are provided in the Interferences section(Section 5).1.4 Samples with sulfur content above 2822 mg kg can beanalyzed after dilution with appropriate solvent(see 5.4).Theprecision and bias of sulfur determinations on diluted sampleshas not been determined and may not be the same as shown forneat samples(Section 15).1.5 When the elemental composition of the samples differsignificantly from the calibration standards used to prepare thecalibration curve,the cautions and recommendation in Section5 should be carefully observed.1.6 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.7 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.For specific hazardinformation,see 3.1.2.Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6259 Practice for Determination of a Pooled Limit ofQuantitationD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD7343 Practice for Optimization,Sample Handling,Calibration,and Validation of X-ray Fluorescence Spec-trometry Methods for Elemental Analysis of PetroleumProducts and Lubricants2.2 EPA Documents:340 CFR 80.584 Code of Federal Regulations;Title 40;Part80;U.S.Environmental Agency,July 1,20051This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved July 1,2015.Published August 2015.Originallyapproved in 2004.Last previous edition approved in 2015 as D7039 15.DOI:10.1520/D7039-15A.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.3Available from U.S.Government Printing Office,732 N.Capitol Street,NW,Washington,DC 20401.*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.Summary of Test Method3.1 A monochromatic X-ray beam with a wavelength suit-able to excite the K-shell electrons of sulfur is focused onto atest specimen contained in a sample cell(see Fig.1).Thefluorescent K radiation at 0.5373 nm(5.373)emitted bysulfur is collected by a fixed monochromator(analyzer).Theintensity(counts per second)of the sulfur X rays is measuredusing a suitable detector and converted to the concentration ofsulfur(mg/kg)in a test specimen using a calibration equation.Excitation by monochromatic X rays reduces background,simplifies matrix correction,and increases the signal/background ratio compared to polychromatic excitation used inconventional WDXRF techniques.4(WarningExposure toexcessive quantities of X-ray radiation is injurious to hea