ASTM_D_5453_-_12.pdf

Designation:D545312Standard Test Method forDetermination of Total Sulfur in Light Hydrocarbons,SparkIgnition Engine Fuel,Diesel Engine Fuel,and Engine Oil byUltraviolet Fluorescence1This standard is issued under the fixed designation D5453;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 sulfurin liquid hydrocarbons,boiling in the range from approxi-mately 25 to 400C,with viscosities between approximately0.2 and 20 cSt(mm2/S)at room temperature.1.2 Three separate interlaboratory studies(ILS)onprecision,and three other investigations that resulted in anASTM research report,have determined that this test method isapplicable to naphthas,distillates,engine oil,ethanol,FattyAcid Methyl Ester(FAME),and engine fuel such as gasoline,oxygen enriched gasoline(ethanol blends,E-85,M-85,RFG),diesel,biodiesel,diesel/biodiesel blends,and jet fuel.Samplescontaining 1.0 to 8000 mg/kg total sulfur can be analyzed(Note 1).NOTE1Estimates of the pooled limit of quantification(PLOQ)for theprecision studies were calculated.Values ranged between less than 1.0 andless than 5.0 mg/kg(see Section 8 and 15.1).1.3 This test method is applicable for total sulfur determi-nation in liquid hydrocarbons containing less than 0.35%(m m)halogen(s).1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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 warningstatements,see 3.1,6.3,6.4,Section 7,and 8.1.2.Referenced Documents2.1 ASTM Standards:2D1298 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 ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance3.Summary of Test Method3.1 A hydrocarbon sample is either directly injected orplaced in a sample boat.The sample or boat,or both,is insertedinto a high temperature combustion tube where the sulfur isoxidized to sulfur dioxide(SO2)in an oxygen rich atmosphere.Water produced during the sample combustion is removed andthe sample combustion gases are next exposed to ultraviolet(UV)light.The SO2absorbs the energy from the UV light andis converted to excited sulfur dioxide(SO2*).The fluorescenceemitted from the excited SO2*as it returns to a stable state,SO2,is detected by a photomultiplier tube and the resultingsignal is a measure of the sulfur contained in the sample.(WarningExposure to excessive quantities of ultraviolet(UV)light is injurious to health.The operator must avoidexposing any part of their person,especially their eyes,notonly to direct UV light but also to secondary or scatteredradiation that is present.)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 Nov.1,2012.Published February 2013.Originallyapproved in 1993.Last previous edition approved in 2009 as D545309.DOI:10.1520/D5453-12.2For 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 4.Significance and Use4.1 Some process catalysts used in petroleum and chemicalrefining can be poisoned when trace amounts of sulfur bearingmaterials are contained in the feedstocks.This test method canbe used to determine sulfur in process feeds sulfur in finishedproducts,and can also be used for purposes of regulatorycontrol.5.Apparatus5.1 FurnaceAn electric furnace held at a temperature(1075 6 25C)sufficient to pyrolyze all of the sample andoxidize sulfur to SO2.5.2 Combustion TubeA quartz combustion tube con-structed to allow the direct injection of the sample into theheated oxidation zone of the furnace or constructed so that theinlet end of the tube is large enough to accommodate a quartzsample boat.The combustion tube must have side arms for the