ASTM_D_3682_-_21.pdf

Designation:D368221Standard Test Method forMajor and Minor Elements in Combustion Residues fromCoal Utilization Processes by Atomic Spectrometry1This standard is issued under the fixed designation D3682;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 method covers the analysis of the commonlydetermined major and minor elements in combustion residuesfrom coal utilization processes.1.2 Use Test Method D5016 for determination of sulfur.1.3 UnitsThe values stated in SI units are to be regardedas standard.The values given in parentheses are provided forinformation only and are not considered standard.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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 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:2D121 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 CokeD3174 Test Method for Ash in the Analysis Sample of Coaland Coke from CoalD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD5016 Test Method for Total Sulfur in Coal and CokeCombustion Residues Using a High-Temperature TubeFurnace Combustion Method with Infrared AbsorptionD7348 Test Methods for Loss on Ignition(LOI)of SolidCombustion ResiduesD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3.Terminology3.1 For definitions of terms used in this test method,refer toTerminology D121.4.Summary of Test Method4.1 The combustion residue to be analyzed is ignited in airat 750 C to a constant mass.The ash is fused within lithiumtetraborate(Li2B4O7)followed by a final dissolution of themelt in either dilute hydrochloric acid(HCl)or dilute nitricacid(HNO3).The solution is analyzed by atomic absorption forapplicable elements.5.Significance and Use5.1 A compositional analysis of the ash in coal is oftenuseful in the total description of the quality of the coal.Knowledge of ash composition is also useful in predicting thebehavior of ashes and slags in combustion chambers.Utiliza-tion of the ash by-products of coal combustion sometimesdepends on the chemical composition of the ash.5.2 Note that the chemical composition of laboratory-prepared coal ash may not exactly represent the composition ofmineral matter in the coal or the composition of fly ash and slagresulting from commercial-scale burning of the coal.6.Apparatus6.1 Ashing Furnace,with an adequate air circulation andcapable of having its temperature regulated at 500 C and750 C.6.2 Fusion Furnace,with an operating temperature of1000 C.1This 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 January 2022.Originallyapproved in 1978.Last previous edition approved in 2013 as D3682 13.DOI:10.1520/D3682-21.2For 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.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.16.3 Platinum Vessels(Dish or Crucible),35 mL to 85 mLcapacity.Graphite crucibles with 10 mLto 15 mLcapacity mayalso be used(Note 1).NOTE1The use of graphite crucibles and subsequent dissolution offused beads from them was not investigated;however,their successful usein similar methods has been reported.36.4 Stirring Hotplate and Bars,operating temperature of200 C.6.5 Flame Atomic Absorption Spectrophotomet