ASTM_D_6414_-_14.pdf

Designation:D641414Standard Test Methods forTotal Mercury in Coal and Coal Combustion Residues byAcid Extraction or Wet Oxidation/Cold Vapor AtomicAbsorption1This standard is issued under the fixed designation D6414;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 These test methods cover procedures to determine thetotal mercury content in a sample of coal or coal combustionresidue.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 Warning:Mercury has been designated by many regu-latory agencies as a hazardous material that can cause seriousmedical issues.Mercury,or its vapor,has been demonstrated tobe hazardous to health and corrosive to materials.Cautionshould be taken when handling mercury and mercury contain-ing products.See the applicable product Safety Data Sheet(SDS)for additional information.Users should be aware thatselling mercury and/or mercury containing products into yourstate or country may be prohibited by law.1.4 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 CokeD1193 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 AnalysisE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodIEEE/ASTM SI 10 Standard for Use of the InternationalSystem of Units(SI):The Modern Metric System2.2 ISO Standard3ISO 5725-6:1994 Accuracy of measurement methods andresults-Part 63.Terminology3.1 For definitions of terms used in this standard,refer toTerminology D121.4.Summary of Test Method4.1 Test Method AMercury in the analysis sample issolubilized by heating the test sample at a specified tempera-ture in a mixture of nitric and hydrochloric acids.The acidsolutions produced are transferred into a vessel in which themercury is reduced to elemental mercury.The mercury vapor isdetermined by flameless cold-vapor atomic absorption spec-troscopy.4.2 Test Method BMercury in the analysis sample issolubilized by heating the test sample in a mixture of nitric andsulfuric acids with vanadium pentoxide.4The acid solutionsproduced are transferred into a vessel in which the mercury isreduced to elemental mercury.The mercury vapor is deter-mined by flameless cold-vapor atomic absorption spectros-copy.NOTE1Mercury and mercury salts can be volatilized at low tempera-tures.Precautions against inadvertent mercury loss should be taken whenusing this method.5.Significance and Use5.1 The emission of mercury during coal combustion can bean environmental concern.1These test methods are under 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 March 1,2014.Published March 2014.Originallyapproved in 1999.Last previous edition approved in 2006 as D6414-01(2006).DOI:10.1520/D6414-14.2For 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.4Crock,J.G.,Open-File Report,U.S.Geological Survey,8784,p.19.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.2 When representative test portions are analyzed accord-ing to one of these procedures,the total mercury is represen-tative of concentrations in the sample.6.Apparatus6.1 Apparatus for Test Method A:6.1.1 Analytical Balance,with a sensitivity of 0.1 mg.6.1.2 Atomic Absorption Spectrophotometer,with a flame-less cold-vapor mercury analysis system.6.1.3 Digestion Vessels,100-to 250-mL bottles with anO-ring seal and screw cap.Bottle must be compatible for usewith aqua regia.Polycarbonate and HDPE are acceptable.Bottles and cap assemblies shall be washed in 1-to-1 HCl thendried before each use.NOTE2Other bottle and cap assemblies may be used provided theyare compatible for use with aqua regia at a temperature of 80C.6.1.4 Heat Source,a water bath capable of maintaining atem