Designation:D4294−21StandardTestMethodforSulfurinPetroleumandPetroleumProductsbyEnergyDispersiveX-rayFluorescenceSpectrometry1ThisstandardisissuedunderthefixeddesignationD4294;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval.ThisstandardhasbeenapprovedforusebyagenciesoftheU.S.DepartmentofDefense.1.Scope*1.1Thistestmethodcoversthedeterminationoftotalsulfurinpetroleumandpetroleumproductsthataresingle-phaseandeitherliquidatambientconditions,liquefiablewithmoderateheat,orsolubleinhydrocarbonsolvents.Thesematerialscanincludedieselfuel,jetfuel,kerosine,otherdistillateoil,naphtha,residualoil,lubricatingbaseoil,hydraulicoil,crudeoil,unleadedgasoline,gasoline-ethanolblends,biodiesel(seeNote2),andsimilarpetroleumproducts.NOTE1—Oxygenatedfuelswithethanolormethanolcontentsexceed-ingthelimitsgiveninTable1canbedealtwithusingthistestmethod,buttheprecisionandbiasstatementsdonotapply(seeAppendixX3).NOTE2—Forsampleswithhighoxygencontents(>3%byweight)sampledilutionasdescribedin1.3ormatrixmatchingmustbeperformedtoassureaccurateresults.1.2Interlaboratorystudiesonprecisionrevealedthescopetobe17mg⁄kgto4.6%bymass.Anestimateofthistestmethod’spooledlimitofquantitation(PLOQ)is16.0mg⁄kgascalculatedbytheproceduresinPracticeD6259.However,becauseinstrumentationcoveredbythistestmethodcanvaryinsensitivity,theapplicabilityofthetestmethodatsulfurconcentrationsbelowapproximately20mg/kgmustbedeter-minedonanindividualbasis.Anestimateofthelimitofdetectionisthreetimesthereproducibilitystandarddeviation,andanestimateofthelimitofquantitation2istentimesthereproducibilitystandarddeviation.1.3Samplescontainingmorethan4.6%bymasssulfurcanbedilutedtobringthesulfurconcentrationofthedilutedmaterialwithinthescopeofthistestmethod.SamplesthataredilutedcanhavehighererrorsthanindicatedinSection17thannon-dil...