ASTM_D_6334_-_12.pdf

Designation:D633412Standard Test Method forSulfur in Gasoline by Wavelength Dispersive X-RayFluorescence1This standard is issued under the fixed designation D6334;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 quantitative determinationof total sulfur in gasoline and gasoline-oxygenate blends.ThePooled Limit of Quantitation(PLOQ)was determined to be 15mg/kg.Therefore,the practical range for this test method isfrom 15 to 940 mg/kg.NOTE1This concentration range is based on that used in theinterlaboratory round robin,which shows that the range of sulfur in theround robin samples was from 1.5 to 940 mg/kg;however,below 15mg/kg,the reproducibility approaches 100%of the concentration.1.2 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 limitation prior to use.1.3 The values stated in SI units are to be regarded as thestandard.The preferred units are mg/kg sulfur.2.Referenced Documents2.1 ASTM Standards:2D2622 Test Method for Sulfur in Petroleum Products byWavelength Dispersive X-ray Fluorescence SpectrometryD3210 Test Method for Comparing Colors of Films fromWater-Emulsion Floor PolishesD4045 Test Method for Sulfur in Petroleum Products byHydrogenolysis and Rateometric ColorimetryD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4294 Test Method for Sulfur in Petroleum and PetroleumProducts by Energy Dispersive X-ray Fluorescence Spec-trometryD5453 Test Method for Determination of Total Sulfur inLight Hydrocarbons,Spark Ignition Engine Fuel,DieselEngine Fuel,and Engine Oil by Ultraviolet FluorescenceD5842 Practice for Sampling and Handling of Fuels forVolatility MeasurementD5854 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 PerformanceD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing Laboratories3.Summary of Test Method3.1 The sample is placed in the X-ray beam,and theintensity of the sulfur K line at 5.373 is measured.Theintensity of a corrected background,measured at a recom-mended wavelength of 5.190,or if a rhodium tube is used,5.437,is subtracted from this intensity.The resultant netcounting rate is then compared to a previously preparedcalibration curve or equation to obtain the concentration ofsulfur in mg/kg.(WarningExposure to excessive quantitiesof X radiation is injurious to health.Therefore,it is imperativethat the operator avoid exposing any part of his or her person,not only to primary X-rays,but also to secondary or scatteredradiation that might be present.The X-ray spectrometer shouldbe operated in accordance with the regulations of recommen-dations governing the use of ionizing radiation.)4.Significance and Use4.1 Knowledge of the presence of sulfur in petroleumproducts,especiallyfuels,helpspredictperformancecharacteristics,potential corrosion problems,and vehicle emis-sion levels.In addition,some regulatory agencies mandatereduced levels of sulfur in reformulated type gasolines.5.Interferences5.1 Fuels with compositions that vary from those specifiedin 9.1 may be analyzed with standards made from basematerials that are of similar composition to minimize matrixeffects.1This 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 Dec.1,2012.Published December 2012.Originallyapproved in 1962.Last previous edition approved in 2007 as D633407.DOI:10.1520/D6334-12.2For 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.*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 5.1.1 Fuels containing oxygenates may be analyzed usingstandards prepared with similar amounts of the same oxygenateadded to the standard dilution matrix.However,round robinstudies done by the Western States PetroleumAssociation haveshown no significant bias in determining sulfur in gasolineswith and without oxygenates at regulatory levels(0 to 2.7weight percent oxygen).5.1.2 Methanol fuels(M85 and M100)exhibit interferences