1、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 ye
2、ar 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)
3、fusionfor the subsequent determination of inorganic constituents byargon plasma emission spectroscopy or atomic absorptionspectroscopy.1.2 The following elements may be solubilized by thispractice:aluminum chromium siliconbarium iron titaniumcadmium magnesium vanadiumcalcium manganese zinccopper nic
4、kel1.3 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
5、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
6、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
7、. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Committee D-19 on WaterD 3682 Test Method for Major and Minor Elements in Coaland Coke Ash by Atomic AbsorptionE50 Practices for Apparatus,
8、Reagents, and Safety Precau-tions for Chemical Analysis of Metals3. 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. Immedi
9、ately 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 appropria
10、tewaste 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
11、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) an
12、aly-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
13、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
14、to 100-mL capacity, madeof platinum, silica, or porcelain.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 1987.2For referenced
15、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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consh
16、ohocken, PA 19428-2959, United States.5.6 Fusion Crucibles, graphite, 28 to 30-mL capacity.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 Testin
17、g 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 Chemi
18、cal Society,where such specifications are available.3Other grades may beused provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be
19、 understood to mean Type II reagent water asdefined in Specification D 1193.6.3 Lithium MetaborateLiBo2, anhydrous powder.6.4 Nitric Acid, Solution (5 6 95)Add while stirring50-mL of nitric acid (HNO3, sp. gr. 1.42) to 900 mL of water.Make to 1 L volume and store in a polyethylene bottle.6.5 Dessica
20、ntAnhydrous calcium sulfate (CaSO4)orequivalent.7. Hazards7.1 Samples known or suspected of containing toxic orhazardous materials must be handled in a fume hood. Safetyinformation relative to the handling of any known toxicmaterials must be obtained and implemented prior to anysample handling.7.2 F
21、lammable materials must be kept from heat, sparks, orflames.7.3 Drying should be conducted on an explosion proofelectrical heater in a fume hood if use of a conventional dryingapparatus may result in toxic, flammable, or irritating vapors.7.4 Ashing at 550C must be conducted in a hood withadequate v
22、entilation and shielding. Refer to Practices E50foradditional information.8. Procedure8.1 Prepare the analytical sample from a thoroughly mixedrepresentative laboratory sample.8.2 Weigh sufficient sample to the nearest 1 mg into a taredashing dish so that after drying and ashing at least 2 g remains
23、for use in 8.6. Typically 5 to 10 g of waste is sufficient unlessmoisture and organic content are a major portion of the sample.8.3 Dry the sample at 110 to 150C. If appreciable freemoisture or volatiles are present, continue drying until thesample is suitable for ashing.8.4 Place the sample into an
24、 ashing furnace set at about300C and increase heat gradually so the furnace reaches550C in 1 h. Ash at 550C until no carbonaceous matter isapparent. Stirring the sample once an hour may increase theoxidation of carbonaceous matter. The ashing time requiredwill depend on the nature of the sample. Sev
25、eral hours, or evenovernight, may be required by difficult-to-ash samples.8.5 Remove the ashing dish and sample from the muffle,cool in a desiccator, and weigh to determine the combined losson ashing and drying.8.6 Quantitatively transfer the ash to a mortar and grind topass a No. 200 sieve, if nece
26、ssary. Transfer back to the ashingdish and reheat the ground ash at 550C for 1 h, remove fromthe ashing furnace and cool in a desiccator. Transfer quantita-tively to a weighing bottle. Weigh approximately 0.3 g ofsample to the nearest 0.0001 g by difference into a graphitecrucible containing 1.5 g o
27、f LiBO2. Mix the ash and LiBO2well, then add an additional 0.5 g of LiBO2on top of the mix.NOTE 1Ashing at 550C typically gives a free flowing or friable ash,so quantitative transfer is possible with careful brushing. Should a portionof the ash melt or stick to the dish so quantitative transfer is i
28、mpossible,the analyst should use a lower ashing temperature or consider analternative dissolution practice.8.7 Place the crucible in a muffle furnace preheated to1000C and fuse for 20 min. Remove the crucible from themuffle, swirl to consolidate the molten bead, and pour into a250-mL beaker containi
29、ng 150 mL of HNO3solution (5 6 95).The acid solution should be warm (50 to 70C) and stirred witha stirring hot plate. Complete dissolution of the melt, other thantraces of graphite particles from the crucible, should occur in10 to 15 min.8.8 Gravity filter the solution through a medium filter, sucha
30、s Whatman No. 41, into a 250-mL volumetric flask. Quanti-tatively wash the beaker and filter with water. Add the washwater to the filtrate, cool, dilute to volume with water, and mix.This solution is ready for ICP or AAS analysis. Refer to TestMethod D 3682 for an AAS analysis method.8.9 Carry a LiB
31、O2blank as in 8.6-8.8 for use as a methodblank in the analytical step.9. Precision and Bias9.1 Six laboratories participated in a collaborative testprogram. Two wastes were tested with a single operator at eachlaboratory performing the practice once on each of 3 days. Acentral laboratory analyzed al
32、l the prepared solutions using aninductively coupled argon plasma spectrometer.9.1.1 The mean, single-operator precision (So), and overallprecision (ST) for the elements solubilized by this practice areshown in Table 1. Practice D 2777 was used in developingthese precision estimates.9.2 Determinatio
33、n of the bias of this practice is not possible,as no suitable standard reference material exists.9.2.1 Comparison of the analytical values obtained usingthis practice with those obtained by a single laboratory usingclassical dissolution and analytical methods is shown in Table2. The data indicate a
34、suitable degree of agreement betweenindependent methods.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Reagent Chemicals and Standards,Joseph Rosin, D.
35、Van Nostrand and Co., Inc., New York, NY, and the United StatesPharmacopeia.D 4503 86 (2003)2TABLE 1 Mean, Single Operator Precision, and Overall PrecisionConstituentsSample 1Bauxite OreSample 2Metal Treatment SludgeX,% SoSTX,% SoSTAluminum 31.17 1.14 2.11 3.24 0.13 0.22Barium 0.0087 0.0003 0.0009 0
36、.0087 0.0002 0.0008Cadmium 0.0051 0.0003 0.0007AAACalcium 0.093 0.019 0.025 24.79 0.79 1.02Copper 0.0063 0.0011 0.0027 0.0063 0.0014 0.0030Chromium 0.24 0.012 0.019 3.13 0.11 0.18Iron 17.20 0.62 1.17 1.21 0.42 0.07Magnesium 0.07 0.003 0.006 0.92 0.018 0.033Manganese 0.25 0.009 0.013 0.02 0.0007 0.00
37、14Nickel 0.020 0.0009 0.0012 0.017 0.0009 0.0032Silicon 0.73 0.020 0.071 5.58 0.26 0.52Titanium 2.09 0.07 0.14 0.05 0.002 0.004Vanadium 0.09 0.004 0.005 0.016 0.0004 0.001Zinc 0.03 0.0019 0.003 0.18 0.002 0.008AAt or less than detection limit.TABLE 2 Comparison of Analytical ValuesConstituentsSample
38、 1 Sample 2This Work(ICP), %Classical,A%This Work,%Classical,%Aluminum 31.17 33.2 3.24 3.38Iron 17.20 18.6 1.21 1.17Titanium 2.09 2.16 0.05 0.05Silicon 0.73 0.86 5.58BManganese 0.25 0.31 0.02 0.02Chromium 0.24 0.19 3.13 3.24Calcium 0.093B24.79 26.4Magnesium 0.07 0.08 0.92 0.92Nickel 0.02 0.03 0.017B
39、Vanadium 0.09 0.07 0.016 0.015OthersCASingle laboratory values using gravimetric, titrimetric, and colorimetric methods are reported.BND = not determined.COne collaborative laboratory determined other constituents in Sample 2 and found the following:Sulfate (SO4)7.6Organic carbon (C) 9.6Carbonate (C
40、O3)4.4Phosphate (P2O5) 16.0Fluoride (F) 1.9D 4503 86 (2003)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such pa
41、tent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited ei
42、ther for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair
43、 hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4503 86 (2003)4
