ASTM_D_1552_-_15.pdf

Designation:D155215Standard Test Method forSulfur in Petroleum Products by High TemperatureCombustion and IR Detection1This standard is issued under the fixed designation D1552;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.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope*1.1 This test method covers a procedure for the determina-tion of total sulfur in petroleum products including lubricatingoils containing additives,and in additive concentrates.This testmethod is applicable to samples boiling above 177 C(350 F)and containing a mass fraction of sulfur not less than 0.06%.This procedure uses IR detection following pyrolysis in aresistance furnace.1.2 Petroleum coke containing up to 8 mass%sulfur can beanalyzed.NOTE1The D155208(2014)version of this standard contained twoother procedures using iodate titrations.Since these procedures are nolonger being used in the industry laboratories based on a survey ofD02.SC 3 laboratories conducted in September 2014,they are beingdeleted.For earlier information on the deleted procedures,D155208(2014)may be perused.1.3The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.4 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:2D1266 Test Method for Sulfur in Petroleum Products(LampMethod)D4057 Practice for Manual Sampling of Petroleum andPetroleum 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 weighed into a special ceramic boatwhich is then placed into a combustion furnace at 1350 C(2460 F)in an oxygen atmosphere.Most sulfur present iscombusted to SO2which is then measured with an infrareddetector after moisture and dust are removed by traps.Amicroprocessor calculates the mass percent sulfur from thesample weight,the integrated detector signal and a predeter-mined calibration factor.The calibration factor is determinedusing standards approximating the material to be analyzed.4.Significance and Use4.1 This test method provides a means of monitoring thesulfur level of various petroleum products and additives.Thisknowledge can be used to predict performance,handling,orprocessing properties.In some cases the presence of sulfurcompounds is beneficial to the product and monitoring thedepletion of sulfur can provide useful information.In othercases the presence of sulfur compounds is detrimental to theprocessing or use of the product.5.Apparatus5.1 Resistance Type Furnace,capable of maintaining atemperature of at least 1350 C(2460 F).5.2 Absorber,as described in Test Method D1266.5.3 Combustion and IR Detection System,comprised ofautomatic balance,oxygen flow controls,drying tubes,com-bustion furnace,infrared detector and microprocessor.Thefurnace shall be capable of maintaining a nominal operatingtemperature of 1350 C(2460 F).5.4 Sieve,60 mesh(250 m).6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended that1This 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 April 1,2015.Published May 2015.Originallyapproved in 1958.Last previous edition approved in 2014 as D1552 08(2014)1.DOI:10.1520/D1552-15.2For 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 all reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Combustion PromoterMagnesium Oxide(Com-Aid)or Alundum(Al2O3).6.3 Magnesium Perchlorate:Anhydrone.(WarningIn ad-dition to other precautions,handle magnesium perchlorate