ASTM_D_6349_-_13.pdf

Designation:D634913Standard Test Method forDetermination of Major and Minor Elements in Coal,Coke,and Solid Residues from Combustion of Coal and Coke byInductively Coupled PlasmaAtomic EmissionSpectrometry1This standard is issued under the fixed designation D6349;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 covers a procedure for the analysis ofthe commonly determined major and minor elements in coal,coke,and solid residues from combustion of coal and coke.These residues may be laboratory ash,bottom ash,fly ash,fluegas desulfurization sludge,and other combustion processresidues.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 CokeD346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3174 Test Method for Ash in the Analysis Sample of Coaland Coke from CoalD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD7348 Test Methods for Loss on Ignition(LOI)of SolidCombustion ResiduesD7582 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/IEC Guide 99:2007 International vocabulary of metrol-ogy-Basic and general concepts and associated terms(VIM)3.Terminology3.1 For definitions of terms used in this test method,refer toTerminology D121.4.Summary of Test Method4.1 The sample to be analyzed is ashed under standardconditions and ignited to constant weight.The ash is fused witha fluxing agent followed by dissolution of the melt in diluteacid solution.Alternatively,the ash is digested in a mixture ofhydrofluoric,nitric,and hydrochloric acids.The solution isanalyzed by inductively coupled plasma-atomic emission spec-trometry(ICP)for the elements.The basis of the method is themeasurement of atomic emissions.Aqueous solutions of thesamples are nebulized,and a portion of the aerosol that isproduced is transported to the plasma torch where excitationand emission occurs.Characteristic line emission spectra areproduced by a radio-frequency inductively coupled plasma.Agrating monochromator system is used to separate the emissionlines,and the intensities of the lines are monitored by photo-mutilplier tube or photodiode array detection.The photocur-rents from the detector are processed and controlled by acomputer system.A background correction technique is re-quired to compensate for variable background contribution tothe determination of elements.Background must be measuredadjacent to analyte lines of samples during analysis.The1This 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 Oct.1,2013.Published October 2013.Originallyapproved in 1998.Last previous edition approved in 2009 as D6349-09.DOI:10.1520/D6349-13.2For 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 rue deVaremb,Case postale 56,CH-1211,Geneva 20,Switzerland,http:/www.iso.ch.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 position selected for the background intensity measurement,oneither or both sides of the analytical line,will be determined bythe complexity of the spectrum adjacent to the analyte line.Theposition used must be free of spectral interference and reflectthe same change in background intensity as occurs at theanalyte wavelength measured.5.Significance and Use5.1 A compositional analysis of coal and coke and theirassociated combustion residues are often useful in assessingtheir quality.Knowledge of the elemental composition of theassociated residues is also useful in predicting the elementalenrichment/depletion compositional behavior of ashes andslags in comparison to the concentration levels in the parentcoal.Utilization of