ASTM_D_3177_-_02.pdf

Designation:D 3177 02Standard 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:D 346 Practice for Collection and Preparation of CokeSamples for Laboratory Analysis2D 1193 Specification for Reagent Water3D 2013 Practice for Preparing Coal Samples for Analysis2D 2015 Test Method for Gross Calorific Value of Coal andCoke by the Adiabatic Bomb Calorimeter2D 3173 Test Method for Moisture in theAnalysis Sample ofCoal and Coke2D 3176 Practice for Ultimate Analysis of Coal and Coke2D 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different Bases2D 3286 Test Method for Gross Calorific Value of Coal andCoke by the Isoperibol Bomb Calorimeter2E 144 Practice for Safe Use of Oxygen CombustionBombs43.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 Coal5which 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 acertified sulfur content of 6 0.0 xx precision can be used.Sulfur values obtained by analyzing these coals,using any of1These 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 September 10,2002.Published October 2002.Origi-nally published as D 3177 73.Last previous edition D 3177 89(2002).2Annual Book of ASTM Standards,Vol 05.06.3Annual Book of ASTM Standards,Vol 11.01.4Annual Book of ASTM Standards,Vol 14.04.5Available from National Institute of Standards and Technology,Gaithersburg,MD 20899.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.the 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,platinum,alundum,orsilica crucibles of 10 to 15-mL capacity,shall be used forigniting the BaSO4.7.Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless