1、Designation:D460615Standard 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
2、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 and selenium in coal.1.2 The values state
3、d 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 heal
4、th practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:3D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in th
5、e 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 aweighed c
6、oal sample 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 measurem
7、ent of the totalarsenic and selenium content of 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 repre
8、sentativeof the total amounts 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-
9、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 weighing to a resolutionof 0.0001 g.6.Reagent
10、s6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.41This test method
11、 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 Nov.1,2015.Published December 2015.Originallyapproved in 1986.Last previous edition approved in 2007 as
12、 D4606 03(2007).DOI:10.1520/D4606-15.2For 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,
13、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 ref
14、erenced 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.4Reagent Chemicals,American Chemical Society Specifications,AmericanChemic
15、al Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.Copyrig
16、ht ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.2 Purity of WaterUse high-purity,conductivity water,prepared by passing distilled water(or equivalent)through anion exchange resin.6.3 Eschka MixturePrepare(with thorough mixing)amixture that has a mass fraction of 67%light calcinedmagnesium oxide(MgO)and 33%anhydrous sodium carbon-ate(Na2CO3).The mixture shall be as free as possible fromarsenic and selenium.6.4 Hydrochloric Acid Concentrated
