ASTM_D_5513_-_22.pdf

Designation:D551322Standard Practice forMicrowave Digestion of Industrial Furnace Feed Streamsand Waste for Trace Element Analysis1This standard is issued under the fixed designation D5513;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 practice describes the multi-stage microwave di-gestion of typical industrial furnace feed stream materials usingnitric,hydrofluoric,hydrochloric,and boric acids for thesubsequent determination of trace metals.1.2 This practice has been used successfully on samples ofcoal,coke,cement raw feed materials,and waste-derived fuelscomposed primarily of waste paint-related material in prepa-ration for measuring the following trace elements:Ag,As,Ba,Be,Cd,Cr,Hg,Pb,Sb,and Tl.This practice may be applicableto elements not listed above.1.3 This practice is also effective for other waste materials(for example,fly ash,foundry sand,alum process residue,cement kiln dust,etc.).1.4 The values stated in SI units are to be regarded asstandard.Other units of measurement in parentheses in thisstandard are informational.1.5 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.Specific hazard statements are given in Section 8.1.6 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:2D1193 Specification for Reagent WaterD5681 Terminology for Waste and Waste Management2.2 Other Document:40 CFR 266 Subpart H,Hazardous Waste Burned in Boilersand Industrial Furnaces,Latest Revision33.Terminology3.1 For definitions of terms used in this practice,refer toTerminology D5681.4.Summary of Practice4.1 A weighed portion of the feed stream material iscombinedwithconcentratednitricacidinapolytetrafluoroethylene-lined digestion vessel,and heated in amicrowave digestion unit.Following a programmed heatingcycle,the vessel is vented and specified quantities of hydro-fluoric and hydrochloric acids are added,and the mixtureundergoes further microwave heating.Following this heatingcycle,the vessel is vented and a specified quantity of boric acidsolution is added,and the mixture undergoes a final microwaveheating.Following this final heating cycle,the vessel is vented,the contents are quantitatively transferred to a volumetric flask,and brought to volume.Typically,the only undissolved mate-rial is particulate carbon.If particulate matter is observed,filtration or centrifugation may be needed.The digested sampleis ready for analysis.5.Significance and Use5.1 TheU.S.EnvironmentalProtectionAgencyRegulations,40 CFR 266,require that boilers,cement kilns,and other industrial furnaces utilizing waste-derived fuel ad-here to specific guidelines in assessing potential metals emis-sions.A common approach for estimating potential emissionsis performing total metals analysis on all feed stream materials.1This practice is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Oct.1,2022.Published October 2022.Originallyapproved in 1994.Last previous edition approved in 2015 as D5513 15.DOI:10.1520/D5513-22.2For 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 Standardization Documents Order Desk,Bldg.4 Section D,700Robbins Ave.,Philadelphia,PA 19111-5094,Attn:NPODS.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.1This practice describes a multi-stage microwave-assisted di-gestion procedure that solubilizes trace elements for spectro-scopic analyses.6.Apparatus6.1 Microwave Digestion UnitEquipped with an auto-matic turntable,pressure and/or temperature controller,andclosed perfluoroalkoxy(PFA)-lined digestion vessels equippedwith pressure relief/rupture membrane fittings or