1、Designation:D635711Standard Test Methods forDetermination of Trace Elements in Coal,Coke,andCombustion Residues from Coal Utilization Processes byInductively Coupled Plasma Atomic Emission Spectrometry,Inductively Coupled Plasma Mass Spectrometry,andGraphite Furnace Atomic Absorption Spectrometry1Th
2、is standard is issued under the fixed designation D6357;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 editor
3、ial change since the last revision or reapproval.1.Scope1.1 These test methods pertain to the determination ofantimony,arsenic,beryllium,cadmium,chromium,cobalt,copper,lead,manganese,molybdenum,nickel,vanadium,andzinc in coal and coke.These test methods can also be used forthe analysis of residues f
4、rom coal combustion processes.NOTE1These test methods may be applicable to the determination ofother trace elements.1.2 The values stated in SI units shall be regarded as thestandard.1.3 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is therespo
5、nsibility 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
6、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 BasesD7448 Practice for Establis
7、hing 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 Othe
8、r Documents:EPA/600/4-91/010 Methods for the Determination of Metalsin Environmental Samples33.Terminology3.1 DefinitionsDefinitions applicable to these test meth-ods are listed in Terminology D121.4.Summary of Test Method4.1 The coal or coke to be analyzed is ashed under con-trolled conditions,dige
9、sted by a mixture of aqua-regia andhydrofluoric acid,and finally dissolved in 1%nitric acid.Combustion residues are digested on an as-received basis.Theconcentration of individual trace elements is determined byeither inductively coupled atomic emission spectrometry(IC-PAES)or inductively coupled pl
10、asma mass spectrometry(ICPMS).Selected elements that occur at concentrations belowthe detection limits of ICPAES can be quantitatively analyzedby graphite furnace atomic absorption spectrometry(GFAA).5.Significance and Use5.1 Coal contains several elements whose individual con-centrations are genera
11、lly less than 0.01%.These elements arecommonly and collectively referred to as trace elements.Theseelements primarily occur as part of the mineral matter in coal.The potential release of certain trace elements from coalcombustion sources has become an environmental concern.1These test methods are un
12、der the jurisdiction ofASTM Committee D05 on Coaland Coke and are 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.Originallypublished in 1996.Last previous edition approved in 2004 as D6357
13、-04.DOI:10.1520/D6357-11.2For 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 Superintendent of Documen
14、ts,U.S.Printing Office,Washington,DC 20402.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.2 The ash prepared in accordance with these provisionaltest methods quantitatively retains the elements listed in 1.1and is representative of the
15、ir concentrations in the coal or coke.6.Apparatus6.1 Inductively Coupled Plasma Atomic Emission Spectrom-eter(ICPAES)The spectrometer system may be either simul-taneous or sequential,vacuum or purged,but must includecomputer-controlled background correction.6.1.1 Argon Gas SupplyHigh purity(99.99%).
16、6.1.2 Mass Flow ControllersA mass-flow controller toregulate the nebulizer gas is required.Mass flow controllers onthe intermediate and outer torch gas flows are recommended.6.2 Inductively Coupled Plasma Mass Spectrometer(ICPMS)The spectrometer system must be capable of scan-ning the mass range of the elements to be analyzed.6.2.1 Argon Gas Supply,high purity(99.99%).6.2.2 The use of a variable speed peristaltic pump fordelivering sample solution to the nebulizer,a mass-flowcontroller on the ga
