ASTM_D_3177_-_02_2007.pdf

Designation:D 3177 02(Reapproved 2007)Standard Test Methods forTotal Sulfur in the Analysis Sample of Coal and Coke1This standard is issued under the fixed designation D 3177;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 These test methods cover two alternative procedures forthe determination of total sulfur in samples of coal and coke.Sulfur is included in the ultimate analysis of coal and coke.1.2 The procedures appear in the following order:SectionsMethod AEschka MethodMethod BBomb Washing Method6-910 and 111.3 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.Specific precau-tionary statements are given in Sections 11.1.1-11.1.1.7.1.4 The values stated in SI units are to be regarded as thestandard.2.Referenced Documents2.1 ASTM Standards:2D 346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD 1193 Specification for Reagent WaterD 2013 Practice for Preparing Coal Samples for AnalysisD 2015 Test Method for Gross Calorific Value of Coal andCoke by the Adiabatic Bomb Calorimeter3D 3173 Test Method for Moisture in theAnalysis Sample ofCoal and CokeD 3176 Practice for Ultimate Analysis of Coal and CokeD 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD 3286 Test Method for Gross Calorific Value of Coal andCoke by the Isoperibol Bomb Calorimeter3E 144 Practice for Safe Use of Oxygen Combustion Bombs3.Summary of Test Methods3.1 Eschka MethodA weighed sample and Eschka mix-ture are intimately mixed and ignited together.The sulfur isdissolved in hot water and then precipitated from the resultingsolution as barium sulfate(BaSO4).The precipitate is filtered,ashed,and weighed.3.2 Bomb Washing MethodSulfur is precipitated asBaSO4from oxygen-bomb calorimeter washings,and theprecipitate is filtered,ashed,and weighed.4.Significance and Use4.1 Determination of sulfur is,by definition,part of theultimate analysis of coal.4.2 Sulfur analysis results obtained by these methods areused to serve a number of interests:evaluation of coalpreparation,evaluation of potential sulfur emissions from coalcombustion or conversion processes,evaluation of the coalquality in relation to contract specification,and other purposesof commercial or scientific interest.5.Sample5.1 The sample shall be the material pulverized to pass No.60(250-m)sieve in accordance with Method D 2013 orMethod D 346.5.2 A separate portion of the analysis sample should beanalyzed for moisture content in accordance with Test MethodD 3173,so that calculation to other than the as-determinedbasis can be made.5.3 Procedures for converting as-determined sulfur valuesobtained from the analysis sample to other bases are describedin Practice D 3176 and Method D 3180.5.4 Standard Reference Material(SRM),such as SRM Nos.2682 through 2685Sulfur in Coal4which consist of fourdifferent coals that have been individually crushed and groundto pass a No.60(250-m)sieve,and bottled in 50-g units,orother commercially available reference material coals with a1These test methods are under the jurisdiction ofASTM Committee D05 on Coaland Coke and are the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved May 1,2007.Published May 2007.Originallyapproved in 1973.Last previous edition approved in 2002 as D 3177 02.2For 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.3Withdrawn.4Available from National Institute of Standards and Technology(NIST),100Bureau Dr.,Stop 1070,Gaithersburg,MD 20899-1070,http:/www.nist.gov.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.certified sulfur content of 6 0.0 xx precision can be used.Sulfur values obtained by analyzing these coals,using any ofthe methods described in this test method,may be used forchecking the accuracy of analytical results.ALTERNATIVE PROCEDURESTEST METHOD AESCHKA METHOD6.Apparatus6.1 Gas(Note 1)or Electric Muffle Furnace,or Burners,for igniting the sample with the Eschka mixture and forigniting the barium sulfate(BaSO4).NOTE1Gas can contain sulfur compounds.6.2 Crucibles or CapsulesPorcelain capsules,22 mm(78in.)in depth and 44 mm(134in.)in diameter,or porcelaincrucibles of 30-mL capacity,high or low form,or platinumcrucibles of similar size shall be used for igniting the samplewith the Eschka mixture.Porcelain,p