ASTM_D_5513_-_15.pdf

Designation:D551315Standard 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,flyash,foundry sand,alum process residue,cement kiln dust,etc.).1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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 and health practices and determine the applica-bility of regulatory limitations prior to use.Specific hazardstatements are given in Section 7.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent Water2.2 Other Document:40 CFR 266 Subpart H,Hazardous Waste Burned in Boilersand Industrial Furnaces,Latest Revision33.Summary of Practice3.1 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 flaskand 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.4.Significance and Use4.1 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.This practice describes a multi-stage microwave-assisted di-gestion procedure that solubilizes trace elements for spectro-scopic analyses.5.Apparatus5.1 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 equivalentpressure relief device.The unit should comply with applicableregional,federal,or state standards for microwave leakage.The user must follow specific manufacturers instructions forsystem installation.NOTE1The digestion unit used in developing this practice wasequipped with a pressure controller,automatic turntable,exhaust fan,andprogramming capacity.The unit delivered 1000 W of power at 100%output.The lined digestion vessels consisted of a high-strength polymericvessel body and cap,inner PFA liner and rupture membrane housing,andPFA vent stem.These vessels have a maximum operating pressure of 2001This 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 Sept.1,2015.Published September 2015.Originallyapproved in 1994.Last previous edition approved in 2009 as D5513 99(2009).DOI:10.1520/D5513-15.2For 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 States1 psig.There are a number of suitable lab grade microwave systemsavailable to the user that meet these minimum specifications.The usermust follow specific manufacturers instructions for