ASTM_D_4239_-_14e2.pdf

Designation:D4239142Standard Test Method forSulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion1This standard is issued under the fixed designation D4239;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.1NOTESummary of Changes added and Tables 3 and A1.4 corrected editorially in November 2014.2NOTEAdded research report footnotes to Tables A1.2,A1.3,and A1.4 editorially in March 2015.1.Scope*1.1 This test method covers the determination of sulfur insamples of coal or coke by high-temperature tube furnacecombustion.1.1.1 Two analysis methods are described.1.2 When automated equipment is used,either method canbe classified as an instrumental method.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 All percentages are percent mass fractions unless other-wise noted.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.2.Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3176 Practice for Ultimate Analysis of Coal and CokeD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD7448 Practice for Establishing the Competence of Labora-tories Using ASTM Procedures in the Sampling andAnalysis of Coal and CokeD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:3ISO 11722 Solid Mineral Fuels-Hard Coal Determinationof Moisture in the general analysis test sample by dryingin nitrogen3.Summary of Test Method3.1 Combustion Method A(1350C)A weighed test por-tion of sample is burned in a tube furnace at a minimumcombustion tube operating temperature of 1350C in a streamof oxygen.During combustion at temperatures above 1350 C,the sulfur and sulfur compounds contained in the sample aredecomposed and oxidized almost exclusively to gaseous sulfurdioxide,SO2.Moisture and particulates are removed from thegas by filters.The gas stream is passed through a cell in whichsulfur dioxide is measured by an infrared(IR)absorptiondetector.Sulfur dioxide absorbs IR energy at a precise wave-length within the IR spectrum.Energy is absorbed as the gaspasses through the cell body in which the IR energy is beingtransmitted:thus,at the detector,less energy is received.Allother IR energy is eliminated from reaching the detector by aprecise wavelength filter.Thus,the absorption of IR energy canbe attributed only to sulfur dioxide whose concentration isproportional to the change in energy at the detector.One cell isused as both a reference and a measurement chamber.Totalsulfur as sulfur dioxide is detected on a continuous basis.3.1.1 One procedure for Method A uses coal or cokereference materials to calibrate the sulfur analyzer.A second1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved March 1,2014.Published March 2014.Originallyapproved in 1983.Last previous edition approved in 2013 as D4239 131.DOI:10.1520/D4239-14.2For 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.3Available from International Organization for Standardization(ISO),1,ch.dela Voie-Creuse,Case postale 56,CH-1211,Geneva 20,Switzerland,http:/www.iso.ch.*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 procedure for Method A uses a pure substance,BBOT,tocalibrate the sulfur analyzer.3.2 Combustion Method B(1150C)A weighed test por-tion of sample is burned in a quartz combustion tube in astream of oxygen with an equal or excess weight of tungstentrioxide(WO3).Sulfur is oxidized during the reaction of thesample and WO3.The tube furnace is operated at a minimumcombustion tube operating temperature of 1150C and tin(Sn)sample boats are utilized.Moisture and particulates are re-moved from the combustion gas by filters.