ASTM_D_3683_-_11.pdf

Designation:D368311Standard Test Method forTrace Elements in Coal and Coke Ash by AtomicAbsorption1This standard is issued under the fixed designation D3683;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 method2describes a procedure for the deter-mination of beryllium,chromium,copper,manganese,nickel,lead,vanadium,and zinc in coal ash or coke ash.1.2 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.1.3 The values stated in SI units(IEEE/ASTM SI 10)shouldbe regarded as the standard.2.Referenced Documents2.1 ASTM Standards:3D121 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 CokeD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisIEEE/ASTM SI 10 Standard for Use of the InternationalSystem of Units(SI):The Modern Metric SystemNOTE1Practice D2013 specifies coal ground to pass through a60-mesh(250-m)screen.For the trace element determinations in this testmethod 100-mesh(150-m)coal is recommended.3.Terminology3.1 DefinitionsDefinitions applicable to this test methodare listed in D121,Terminology of Coal and Coke.4.Summary of Test Method4.1 Coal or coke is ashed,the ash is dissolved by mineralacids,and the individual elements determined by atomicabsorption spectrometry.5.Significance and Use5.1 Many trace elements occur in coal,primarily as a part ofthe mineral matter but may also be associated with the organicmatrix.Concern over release of certain trace elements to theenvironment as a result of coal utilization has made thedetermination of these elements an increasingly importantaspect of coal analysis.5.2 When coal ash is prepared in accordance with this testmethod,the eight elements listed in 1.1 are quantitativelyretained in the ash and are representative of concentrations inthe coal.Concentrations of these and other elements in powerplant ash,industrial process ash,fly ash,and so forth,may ormay not be representative of total quantities in the coal.6.Apparatus6.1 Atomic Absorption SpectrometerAny dual-channel in-strument using a deuterium(D2)arc background corrector orother comparable simultaneous background correction system.6.2 Muffle Furnace,with temperature control.6.3 Bottles,polyethyleneorpolytetrafluoroethylene,125-mL capacity,with screw-cap lids,capable of withstandingtemperatures up to 130C.6.4 Volumetric Flasks,100-mL capacity.6.5 Steam Bath.6.6 Analytical Balance,capable of weighing to 0.1 mg.6.7 Crucibles,50-mL quartz or high silica.7.Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended that1This 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 April 1,2011.Published April 2011.Originallyapproved in 1978.Last previous edition approved in 2004 as D3683 04.DOI:10.1520/D3683-11.2For information concerning experimental work on which this test method isbased,see Bernas,B.,A New Method for the Decomposition and ComprehensiveAnalysis of Silicates by Atomic Absorption Spectrometry,Analytical Chemistry,ANCHA,Vol 40,1968,pp 168286.3For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 all reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Reagent WaterReagent water,conforming to Type IIof Specification D1193,shall be used for preparation ofreagents.7.3 Aqua Regia SolutionMix one part concentrated nitricacid(HNO3,sp gr 1.42),three parts concentrated hydrochloricacid(HCl,sp gr 1.19),and one part water.7.4 Boric Acid Solution,SaturatedDissolve 60 g of boricacid(H3BO3)in 1 L of deionized water