ASTM_D_6021_-_12.pdf

Designation:D602112Standard Test Method forMeasurement of Total Hydrogen Sulfide in Residual Fuelsby Multiple Headspace Extraction and Sulfur SpecificDetection1This standard is issued under the fixed designation D6021;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 a method suitable for measuringthe total amount of hydrogen sulfide(H2S)in heavy distillates,heavy distillate/residual fuel blends,or residual fuels as definedin Specification D396 Grade 4,5(Light),5(Heavy),and 6,when the H2S concentration in the fuel is in the 0.01 to 100g/g(ppmw)range.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 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 specificwarning statements,see 7.5,8.2,9.2,10.1.4,and 11.1.2.Referenced Documents2.1 ASTM Standards:2D396 Specification for Fuel OilsD1193 Specification for Reagent WaterD2420 Test Method for Hydrogen Sulfide in LiquefiedPetroleum(LP)Gases(Lead Acetate Method)D3609 Practice for Calibration Techniques Using Perme-ation TubesD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4084 Test Method for Analysis of Hydrogen Sulfide inGaseous Fuels(Lead Acetate Reaction Rate Method)D4323 Test Method for Hydrogen Sulfide in theAtmosphereby Rate of Change of ReflectanceD5504 Test Method for Determination of Sulfur Compoundsin Natural Gas and Gaseous Fuels by Gas Chromatogra-phy and ChemiluminescenceD5705 Test Method for Measurement of Hydrogen Sulfidein the Vapor Phase Above Residual Fuel OilsD7621 Test Method for Determination of Hydrogen Sulfidein Fuel Oils by Rapid Liquid Phase Extraction3.Terminology3.1 Definitions:3.1.1 heavy distillate,na fuel produced from the distilla-tion of crude oil which has a kinematic viscosity at 40Cbetween 5.5 and 24.0 mm2/s,inclusive.3.1.2 heavy distillate/residual fuel blend,na blend ofheavy distillate and residual fuel oil having a viscosity at 40Cbetween 5.5 and 24.0 mm2/s,inclusive.3.1.3 multiple headspace extraction,na technique to de-termine the total concentration of a gas trapped in a liquid byanalysis of successive gas extractions from the vapor space ofa closed vessel containing a known amount of the sample.3.1.4 residual fuel oil,nany liquid or liquefiable petro-leum product having a kinematic viscosity at 100C between5.0 and 50.0 mm2/s,inclusive,burned for the generation ofheat in a furnace or firebox or for the generation of power in anengine.4.Summary of Test Method4.1 A representative sample of residual fuel oil is obtainedin sufficient quantity to completely fill the sample container.The sample is taken to the laboratory preferably within one to4 h,within 24 h maximum and placed in a refrigerator until thehydrogen sulfide analysis can be run.At that time,the sampleis removed from the refrigerator and allowed to sit at ambienttemperature until it flows freely.4.2 A 0.05 to 5.0 g test specimen(aliquot)is placed in aheadspace vial and heated in an oven at 60C for more than fivebut less than 15 min.The headspace gas is sampled andinjected into either of two types of apparatus capable ofmeasuring the hydrogen sulfide concentration in the gaseous1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.14 on Stability and Cleanliness of Liquid Fuels.Current edition approved April 15,2012.Published May 2012.Originallyapproved in 1996.Last previous edition approved in 2006 as D602106.DOI:10.1520/D6021-12.2For 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 sample.3The two types of apparatus are those using thereaction of lead acetate with H2S(see Test Method D4084 orTest Method D4323)and those based on chemiluminescence(see Test Method D5504).4.3 The remaining contents of the headspace vial are cooledfor 5 min,then again heated in the oven.The headspacecontents are again transferred to the hydrogen sulfide measur-ing instrument.The procedure is repeated for a third time.Thisis known as multiple headspace extraction procedure(MHE).4.4 A linear plot of the natural logarithm of the area