ASTM_D_5016_-_16.pdf

Designation:D501616Standard Test Method forTotal Sulfur in Coal and Coke Combustion Residues Using aHigh-Temperature Tube Furnace Combustion Method withInfrared Absorption1This standard is issued under the fixed designation D5016;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.Scope1.1 This test method describes a procedure using a high-temperature tube furnace and infrared detection for the deter-mination of sulfur in coal and coke combustion residues,including lab ashes and residues from coal and coke combus-tion.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.2.Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD3174 Test Method for Ash in the Analysis Sample of Coaland Coke from CoalD3682 Test Method for Major and Minor Elements inCombustion Residues from Coal Utilization ProcessesD3683 Test Method for Trace Elements in Coal and CokeAsh by Atomic AbsorptionD4326 Test Method for Major and Minor Elements in Coaland Coke Ash By X-Ray FluorescenceD4621 Guide for Quality Management in an OrganizationThat Samples or Tests Coal and Coke(Withdrawn 2010)3D5142 Test Methods for Proximate Analysis of the AnalysisSample of Coal and Coke by Instrumental Procedures(Withdrawn 2010)3D6349 Test Method for Determination of Major and MinorElements in Coal,Coke,and Solid Residues from Com-bustion of Coal and Coke by Inductively CoupledPlasmaAtomic Emission SpectrometryD6357 Test Methods for Determination of Trace Elements inCoal,Coke,and Combustion Residues from Coal Utiliza-tion Processes by Inductively Coupled Plasma AtomicEmission Spectrometry,Inductively Coupled PlasmaMass Spectrometry,and Graphite Furnace Atomic Ab3.Terminology3.1 For definitions of terms used in these test methods,referto Terminology D121.3.2 Throughout this test method the term ash is used todescribe the sample being analyzed.The term ash is to beinterpreted as a combustion residue.4.Summary of Test Method4.1 A weighed test portion is mixed with a promoting agentand ignited in a tube furnace an operating temperature of1450 C in a stream of oxygen.The combustible sulfurcontained in the test portion is oxidized to gaseous oxides ofsulfur.Moisture and particulates are removed by traps filledwith anhydrous magnesium perchlorate.The gas stream ispassed through a cell in which sulfur dioxide is measured by aninfrared absorption detector.Sulfur dioxide absorbs IR energyat a precise wavelength within the IR spectrum.Energy isabsorbed as the gas passes through the cell body in which theIR energy is being transmitted;thus,at the detector,less energyis received.All other IR energy is eliminated from reaching thedetector by a precise wavelength filter.The absorption of IRenergy can be attributed only to sulfur dioxide whose concen-tration is proportional to the change in energy at the detector.One cell is used as both a reference and a measurementchamber.Total sulfur as sulfur dioxide is detected on acontinuous basis.4.2 This test method is applicable for use with sulfuranalyzers equipped to carry out the operations in 4.1 and must1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.29 on MajorElements in Ash and Trace Elements of Coal.Current edition approved Sept.1,2016.Published September 2016.Originallyapproved in 1989.Last previous edition approved 2008 as D5016 081.DOI:10.1520/D5016-16.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 be calibrated using reference materials(RMs)covering therange of sulfur in the ash samples being analyzed.5.Significance and Use5.1 The percent sulfur content of the ash derived from coalor coke can be calculated to sulfur trioxide content.Thisinformation can be used in combination with results from thedetermination of major,minor and or trace elements in thesame ash to calculate results on a sulfur trioxide free-basis orto calculate total recovered analyte.6.Interferences6.1 Known interferences in this test method are somealkaline earth metal ions,including b