ASTM_D_4606_-_21.pdf

Designation:D460621Standard Test Method forDetermination of Arsenic and Selenium in Coal by theHydride Generation/Atomic Absorption Method1This standard is issued under the fixed designation D4606;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 method2covers the determination of totalarsenic in the range of 0.7 ug g to 12 ug g and selenium in therange of 0.6 ugg to 5 ug g in coal.1.2 UnitsThe values stated in SI units are to be regardedas standard.The values given in parentheses after SI units areprovided for information only and are not considered standard.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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 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:3D2013 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 Analysis3.Summary of Test Method3.1 Arsenic and selenium are determined by mixing a coalsample of known mass with Eschka mixture and igniting at750 C.The mixture is dissolved in hydrochloric acid and thegaseous hydride of each element is generated from the appro-priate oxidation state and determined by atomic absorptionspectrophotometry.4.Significance and Use4.1 This test method permits measurement of the total massfraction of arsenic and selenium in coal for the purpose ofevaluating these elements where they can be of concern,forexample,in coal combustion.When coal samples are preparedfor analysis in accordance with this test method,the arsenicand selenium are quantitatively retained and are representativeof the total mass fraction in the coal.5.Apparatus5.1 Atomic Absorption Spectrophotometer,with backgroundcorrection system and peak profile recording device.5.2 Hydride Generation Apparatus,for producing the hy-drides of arsenic and selenium.5.3 Burner or Heated Quartz Cell,for thermal decomposi-tion of the hydrides.5.4 Hotplate,capable of maintaining a temperature of asolution at 60 C to 90 C.5.5 Ignition CruciblesPorcelain crucible of 30 mL capac-ity.Do not use a porcelain crucible in which the glaze is flaked.5.6 Analytical Balance,capable of a resolution of 0.0001 g.5.7 Beakers150 mL and 500 mL.5.8 Polypropylene Flasks100 mL and 500 mL also usedas a reaction vessel.6.Reagents6.1 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 Dec.1,2021.Published December 2021.Originallyapproved in 1986.Last previous edition approved in 2015 as D4606 15.DOI:10.1520/D4606-21.2For information concerning experimental work on which this test method isbased see:Bosshart,R.E.,Price,A.A.,and Ford,C.T.,“Evaluation of the Effectof Coal Cleaning on Fugitive Elements,Phase II Final Report,Part II AnalyticalMethods,”ERDA Report No.C00-44727-35,1980,pp.94102;Fernandez,F.J.,“Atomic Absorption Determination of Gaseous Hydrides Utilizing Sodium Boro-hydride Reduction,”Atomic Absorption Newsletter,Vol 12,No.4,1973,pp.9397;and Brodie,K.G.,“A Comparative StudyDetermining Arsenic and Selenium byAAS,”American Laboratory,March 1977,pp.7378.3For 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 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?all reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where su