ASTM_D_4239_-_18e1.pdf

Designation:D4239181Standard 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.1NOTETable 1 was corrected editorially in October 2018.1.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.The values given in parentheses after SI units areprovided for information only and are not considered standard.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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D346/D346M Practice for Collection and Preparation ofCoke Samples for Laboratory AnalysisD2013/D2013M Practice for Preparing Coal Samples forAnalysisD3173/D3173M Test Method for Moisture in the AnalysisSample of Coal 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 5725-6 Accuracy(trueness and precision)of measure-ment methods and resultsPart 6:Use in practice ofaccuracy valuesISO 11722 Solid mineral fuelsHard coalDeterminationof moisture in the general analysis test sample by dryingin nitrogen3.Summary of Test Method3.1 Combustion Method A(1350 C)A weighed test por-tion of sample is burned in a tube furnace at a minimumcombustion tube operating temperature of 1350 C 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 being1This 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 Sept.1,2018.Published October 2018.Originallyapproved in 1983.Last previous edition approved in 2017 as D4239 17.DOI:10.1520/D4239-18E01.2For 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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 transmitted: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 me