1、Designation: D 5284 93 (Reapproved 2004)e1Standard Test Method forSequential Batch Extraction of Waste with Acidic ExtractionFluid1This standard is issued under the fixed designation D 5284; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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.e1NOTEReference to a research report was added in May 2004.1. Scope1.1 This test method provides a procedure
3、for the sequentialleaching of a waste containing at least 5 % dry solids in orderto generate solutions to be used to determine the constituentsleached under the specified testing conditions.1.2 This test method calls for the shaking of a known weightof waste with acidic extraction fluid of a specifi
4、ed compositionas well as the separation of the liquid phase for analysis. ThepH of the extraction fluid is to reflect the pH of acidicprecipitation in the geographic region in which the waste beingtested is to be disposed. The procedure is conducted ten timesin sequence on the same sample of waste,
5、and it generates tensolutions.1.3 This test method is intended to describe the procedurefor performing sequential batch extractions only. It does notdescribe all types of sampling and analytical requirements thatmay be associated with its application.1.4 The values stated in SI units are to be regar
6、ded as thestandard.1.5 This standard does not purport to address all of thesafety problems, 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
7、use.2. Referenced Documents2.1 ASTM Standards:2D 75 Practice for Sampling AggregatesD 420 Guide to Site Characterization for Engineering, De-sign and Construction PurposesD 653 Terminology Relating to Soil, Rock, and ContainedFluidsD 1129 Terminology Relating to WaterD 1193 Specification for Reagent
8、 WaterD 2234 Test Methods for Collection of a Gross Sample ofCoalD 2777 Practice for Determination of Precision and Bias ofMethods of Committee D-19 on WaterD 3370 Practices for Sampling WaterD 4793 Test Method for Sequential Batch Extraction ofWaste with Water3. Terminology3.1 DefinitionsFor defini
9、tions of terms used in this testmethod, see Terminology D 1129.3.2 Symbols:SymbolsVariables listed in this test methodare defined in the individual sections in which they arediscussed. A list of the defined variables is also provided inSection 11.4. Significance and Use4.1 This test method is intend
10、ed as a means for obtainingsequential extracts of a waste. The extracts may be used toestimate the release of certain constituents of the waste underthe laboratory conditions described in this test method.4.2 The pH of the extraction fluid used in this test method isto reflect the pH of acidic preci
11、pitation in the geographic regionin which the waste being tested is to be disposed.NOTE 1Possible sources of information concerning the pH of precipi-tation in the geographic region of interest include state and federalenvironmental agencies, state universities, libraries, etc.NOTE 2For sequential b
12、atch extraction of waste using a nonacidicextraction fluid, see Test Method D 4793.4.3 An intent of this test method is for the final pH of eachof the extracts to reflect the interaction of the extractant withthe buffering capacity of the waste.4.4 This test method is not intended to provide extract
13、s thatare representative of the actual leachate produced from a wastein the field or to produce extracts to be used as the sole basisof engineering design.1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 o
14、nAncillary Topics.Current edition approved Feb. 1, 2004. Published April 2004. Originallyapproved in 1992. Last previous edition approved in 1999 as D 528493(1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
15、k 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 Conshohocken, PA 19428-2959, United States.4.5 This test method has not been demonstrated to simulateactual disposal site lea
16、ching conditions.4.6 This test method produces extracts that are amenable tothe determination of both major and minor (trace) constituents.When minor constituents are being determined, it is especiallyimportant that precautions be taken in sample storage andhandling to avoid possible contamination o
17、f the samples.4.7 This test method has been tested to determine itsapplicability to certain inorganic components in the waste. Thistest method has not been tested for applicability to organicsubstances, volatile matter (see Note 5), or biologically activesamples.4.8 The agitation technique, rate, li
18、quid-to-solid ratio, andfiltration conditions specified in the procedure may not besuitable for extracting all types of wastes (see Sections 7 and 8and Appendix X1).5. Apparatus5.1 Straight Edge, such as a thin-edged yardstick.5.2 Impermeable Sheet, of glazed paper, oil cloth, or otherflexible mater
19、ial of a composition suitable to the analytes ofinterest.5.3 Drying Pans or Dishes (for example, aluminum tins,porcelain dishes, glass weighing pans), two per waste, suitableto the waste being tested and the instructions given in 9.2.5.4 Drying OvenAny thermostatically controlled dryingoven capable
20、of maintaining a steady temperature of 62C ina range of 100 to 110C.5.5 Desiccator, having a capacity to hold the drying pansdescribed in 5.3 and the crucibles described in 5.16.5.6 Laboratory Balance, capable of weighing to 0.1 g.5.7 Erlenmeyer Flask, 2-L capacity, equipped with a mag-netic stir ba
21、r.5.8 Magnetic Stir Plate.5.9 Graduated Cylinder, 1 or 2-L capacity.5.10 Pipet, 1-mL capacity.5.11 Volumetric Flask, 1-L capacity.5.12 Pipet, 10-mL capacity. (Various other sized pipets,including micropipets, may be necessary for 9.3.2.)5.13 pH MeterAny pH meter with a readability of 0.01units and a
22、n accuracy of 60.05 units at 25C.5.14 Carboy-type Container, with spigot, 20 to 50-L capac-ity, of a composition suitable to the nature of the analyses to beperformed (see Practices D 3370).5.15 Large Glass Funnel.5.16 Crucibles, porcelain, 20-mL capacity each, two perwaste.5.17 Analytical Balance,
23、capable of weighing to 0.1 mg.5.18 Wash Bottle, 500-mL capacity.5.19 Agitation Equipment, of any type that rotates theextraction vessel in an end-over-end fashion at a rate of 30 62 r/min such that the axis of rotation is horizontal and it passesthrough the center of the bottle (see Fig. 1 and Appen
24、dix X1).NOTE 3Similar devices having a different axial arrangement may beused if equivalency can be demonstrated.5.20 Pressure Filtration AssemblyA pressure filtrationdevice of a composition suitable to the nature of the analysesto be performed and equipped with a 0.45 or 0.8-m pore sizefilter (see
25、Note 8).5.21 Extraction Vessels, cylindrical, wide-mouth, of a com-position suitable to the nature of the waste and analyses to beperformed, constructed of materials that will not allow sorptionof the constituents of interest, and sturdy enough to withstandthe impact of the falling sample fragments.
26、 The size of thecontainer should be selected so that the sample plus extractionfluid occupy approximately 95 % of the container. The con-tainers must have water-tight closures. Containers for samplesin which gases may be released should be provided withventing mechanisms.NOTE 4Suitable container siz
27、es range from 4.0 to 4.5 in. in diameterand 8.5 to 13.0 in. in height.NOTE 5The venting of the container has the potential to affect theconcentration of volatile compounds in the extracts.5.21.1 Extraction vessels should be cleaned in a mannerconsistent with the analyses to be performed (see Section
28、 13 ofPractice D 3370).6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specificatio
29、ns 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 understood to mean Type IV reagen
30、t water at18 to 27C conforming to Specification D 1193. The methodby which the water is prepared, that is, distillation, ionexchange, reverse osmosis, electrodialysis, or a combinationthereof, should remain constant throughout testing.6.3 Sulfuric Acid/Nitric Acid SolutionA 60/40 weightpercent (wt %
31、) mixture prepared using 95 to 98 wt % sulfuricacid and 69 to 71 wt % nitric acid. (See 9.3 for instructions onthe preparation of this solution.)7. Sampling7.1 Obtain a representative sample of the waste to be testedby using, where available, ASTM sampling methods developedfor the specific industry
32、(see Practice D 75, Guide D 420,Terminology D 653, and Test Method D 2234).7.2 Sampling methodology for materials of similar physicalform shall be used where no specific methods are available.7.3 The amount of sample to be sent to the laboratoryshould be sufficient to perform the solids content dete
33、rmination3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States P
34、harmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 5284 93 (2004)e12as specified in 9.2, and to provide 100 g of sample on a dryweight basis for each extraction.7.4 It is important that the sample of the waste be represen-tative with respect to surface area
35、, as variations in surface areawould directly affect the leaching characteristics of the sample.Waste samples should contain a representative distribution ofparticle sizes.NOTE 6Information on obtaining representative samples can also befound in Pierre Gys Sampling Theory and Sampling Practice.47.5
36、In order to prevent sample contamination or constituentloss prior to extraction, keep the samples in closed containersappropriate to sample type and desired analysis. See PracticesD 3370 for guidance. Record the storage conditions andhandling procedures in the report.7.6 The time between collection
37、and extraction of thesample should be determined by the nature of the sample andthe information desired. See Practices D 3370 for guidance.Report the length of time between sample collection andextraction.8. Sample Preparation8.1 For free-flowing particulate solid wastes, obtain asample of the appro
38、ximate size required in the test by quarter-ing the sample (Section 7) received for testing on an imper-meable sheet of glazed paper, oil cloth, or other flexiblematerial having a composition suitable to the analytes ofinterest, as follows:8.1.1 Empty the sample container into the center of thesheet
39、.8.1.2 Gently flatten the sample out with a suitable straight-edge until it is spread uniformly to a depth at least twice themaximum particle diameter.4Pitard, F., Pierre Gys Sampling Theory and Sampling Practice, Vols I and II,CRC Press, 1989.FIG. 1 ExtractorsD 5284 93 (2004)e138.1.3 Remix the samp
40、le by lifting a corner of the sheet anddrawing it low across to the opposite corner in such a mannerthat the material is made to roll over and over and does notmerely slide along. Continue the operation with each corner,proceeding in a clockwise direction. Repeat this operation tentimes.8.1.4 Lift a
41、ll four corners of the sheet toward the center and,holding all four corners together, raise the entire sheet into theair to form a pocket for the sample.8.1.5 Repeat the procedure described in 8.1.2 to flatten thesample out.8.1.6 With a straightedge (such as a thin-edged yardstick) atleast as long a
42、s the flattened mound of sample, gently dividethe sample into quarters. Make an effort to avoid using pressureon the straightedge sufficient to cause damage to the particles.8.1.7 Discard the alternate quarters.8.1.8 If further reduction of the sample size is necessary,repeat the steps given in 8.1.
43、3 through 8.1.7. Use a sample sizeto provide 100 g of solid on a dry weight basis for eachextraction. Provide additional samples for the determination ofsolids content (see 9.2). Use of a sample size other than 100 gof solid on a dry weight basis for extraction is not recom-mended; however, if a dif
44、ferent sample size is used, report thisfact.NOTE 7For other acceptable methods of mixing and subsamplingfree-flowing solid particulate wastes, see Pierre Gys Sampling Theoryand Sampling Practice.5The method of subsampling should be deter-mined by the physical properties of the waste, analytes of int
45、erest, andequipment available.8.2 For field-cored solid wastes or castings produced in thelaboratory, cut a representative section weighing approxi-mately 100 g for testing, plus samples for the determination ofsolids content. Shape the sample so that the leaching solutionwill cover the material to
46、be leached.8.3 For multiphasic wastes, mix thoroughly to ensure that arepresentative sample will be withdrawn. Take samples for thedetermination of solids content at the same time that testsamples are taken.9. Procedure9.1 Record a physical description of the sample to be tested,including particle s
47、ize so far as it is known.9.2 Solids ContentDetermine the solids content of twoseparate portions of the sample as follows:9.2.1 Dry to a constant weight, at 104 6 2C, two dishes orpans of size suitable to the solid waste being tested. Cool in adesiccator and weigh. Record the values to 60.1 g.9.2.2
48、Place 50 g of the waste to be tested into each pan.Record the mass of sample in each pan to 60.1 g.9.2.3 Dry 16 to 20 h at 104 6 2C. Record the temperatureand time of the drying period.9.2.4 Cool to room temperature in a desiccator and reweigh.Record the mass to 60.1 g.9.2.5 Repeat the steps given i
49、n 9.2.3 and 9.2.4 until constantcontainer-sample masses are obtained. Discard the driedsamples following completion of this step.9.2.6 Calculate the solids content of the sample from thedata obtained in 9.2.1, 9.2.2, and 9.2.4 as follows:S 5 A/B (1)where:A = mass of sample after drying, g,B = original mass of sample, g, andS = solids content, g/g.Average the two values obtained. Record the solids content.9.3 Preparation of Extraction FluidPrepare a 60/40 wt %mixture of sulfuric acid/nitric acid. Cautiously mix 60 g ofconcentrated sulfuric acid with 40 g o
