ASTM_D_4503_-_86_2003.pdf

Designation:D 4503 86(Reapproved 2003)Standard Practice forDissolution of Solid Waste by Lithium Metaborate Fusion1This standard is issued under the fixed designation D 4503;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This practice covers the drying,ashing,and solubiliza-tion of solid waste using a lithium metaborate(LiBO2)fusionfor the subsequent determination of inorganic constituents byargon plasma emission spectroscopy or atomic absorptionspectroscopy.1.2 The following elements may be solubilized by thispractice:aluminumchromiumsiliconbariumirontitaniumcadmiummagnesiumvanadiumcalciummanganesezinccoppernickel1.3 This practice has been used successfully with a bauxiteore and a neutralized metal treatment sludge.The practice maybe applicable to other elements not listed above.Some metals,such as cadmium and zinc,may volatilize from some samplesduring the drying,ashing,or fusion steps.The analyst isresponsible for determining whether the practice is applicableto the solid waste being tested.1.4 This practice is intended for the solubilization of non-volatile inorganic constituents in solid waste.The LiBO2fusion is appropriate for a silicate matrix or acid resistantsamples.1.5 This standard does not purport to address all of thesafety problems associated with its use.It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.For specific hazard statements seeSection 7.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2D 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Committee D-19 on Water2D 3682 Test Method for Major and Minor Elements in Coaland Coke Ash by Atomic Absorption3E 50 Practices for Apparatus,Reagents,and Safety Precau-tions for Chemical Analysis of Metals43.Summary of Practice3.1 The solid waste is weighed,dried,and ashed at 550C toremove water and organic constituents,and reweighed.Aknown portion of the ground ash is mixed with LiBO2in agraphite crucible and fused at 1000C.Immediately afterfusion,the molten mass is poured directly into stirred diluteHNO3solution,dissolved,filtered,and made to appropriatevolume for subsequent analysis.4.Significance and Use4.1 A knowledge of the inorganic constituent compositionin a waste is often required for the selection of appropriatewaste disposal practices.Solid waste may exist in a variety offorms and contain a range of organic and inorganic constitu-ents.This practice describes a drying and ashing step that maybe applied to remove moisture and volatile and nonvolatileorganic constituents prior to determining nonvolatile metals.Generation of a dry ash concentrates the inorganic constituentsof interest and makes the LiBO2fusion feasible for a greatervariety of waste samples.Acidification of the LiBO2fusionmix results in a solution amenable to inductively coupledplasma(ICP)or atomic absorption spectrometry(AAS)analy-sis.5.Apparatus5.1 Analytical Balance,sensitive to 0.1 mg.5.2 Fusion Muffle Furnace,electrically heated,capable ofmaintaining a temperature of 1000C.5.3 Ashing Muffle Furnace,electrically heated,capable ofmaintaining a temperature of 550C6 30C and with anadequate air circulation.This may be accomplished by con-necting rubber tubing to a controlled source of clean dry air.Then,via a ceramic tube inserted into a convenient muffleopening,flow approximately 4 L/min of air into the furnace.5.4 Drying Oven,capable of operating at a temperature upto 150C.5.5 Evaporating/Ashing Dish,50 to 100-mL capacity,madeof platinum,silica,or porcelain.5.6 Fusion Crucibles,graphite,28 to 30-mL capacity.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 Nov.28,1986.Published February 1987.2Annual Book of ASTM Standards,Vol 11.01.3Annual Book of ASTM Standards,Vol 05.05.4Annual Book of ASTM Standards,Vol 03.05.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.5.7 Stirring Hot Plate,capable of operating at a surfacetemperature up to 300C with TFE-fluorocarbon-coated stirmagnet.5.8 Mortar and Pestle,agate or mullite type.5.9 Sieve and Pan,ASTM U.S.Standard Testing Sieve,200m(75 m opening).5.10 Desiccator.6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intendedthatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.5Other grades may beused provided it is first