1、Designation: D 5284 09Standard 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 revision, the year of
2、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 test method provides a procedure for the sequentialleaching of a waste containing at least 5 % dry solids in orde
3、rto 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 specified compositionas well as the separation of the liquid phase for analysis. ThepH
4、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, and it generates tensolutions.1.3 This test method is intended to describe the p
5、rocedurefor 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 regarded asstandard. No other units of measurement are included in thisstandard.1.5 T
6、his 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 use.2. Referenced Docume
7、nts2.1 ASTM Standards:2D75 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 WaterD 2234/D 2234M Pract
8、ice for Collection of a Gross Sampleof CoalD 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD 3370 Practices for Sampling Water from Closed ConduitsD 4793 Test Method for Sequential Batch Extraction ofWaste with Water3. Terminology3.1 Definit
9、ionsFor definitions of terms used in this testmethod, see Terminology D 1129.3.2 SymbolsVariables listed in this test method are de-fined in the individual sections in which they are discussed. Alist of the defined variables is also provided in Section 11.4. Significance and Use4.1 This test method
10、is intended 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 aci
11、dic precipitation 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 seq
12、uential batch 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 provid
13、e extracts 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.4.5 This test method has not been demonstrated to simulateactual disposal site leaching conditions.4.6 This test method produces extract
14、s that are amenable tothe determination of both major and minor (trace) constituents.When minor constituents are being determined, it is especially1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 on WasteL
15、eaching Techniques.Current edition approved July 1, 2009. Published October 2009. Originallyapproved in 1992. Last previous edition approved in 2001 as D 5284 93 (2001)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Ann
16、ual 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 Conshohocken, PA 19428-2959, United States.important that precautions be taken in sample storage andhandling to avoid
17、possible contamination of 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 agita
18、tion technique, rate, liquid-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
19、, or otherflexible material 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 contro
20、lled dryingoven capable 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
21、with a mag-netic stir bar.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 readab
22、ility of 0.01units and an 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
23、.17 Analytical Balance, 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 0.5 60.03 Hz such that the axis of rotation is horizontal and it passesthrough the center of the bot
24、tle (see Fig. 1 and Appendix 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.
25、8-m pore sizefilter (see 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
26、falling sample fragments. 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.NOT
27、E 4Suitable container sizes range from 10 to 11 cm in diameterand 22 to 33 cm in height.NOTE 5Venting the container has the potential to affect the concen-tration of volatile compounds in the extracts.5.21.1 Extraction vessels should be cleaned in a mannerconsistent with the analyses to be performed
28、 (see Section 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
29、 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 understood to mean T
30、ype IV reagent 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 weight
31、percent (wt %) 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 specif
32、ic industry (see Practice D75, Guide D 420,Terminology D 653, and Test Method D 2234/D 2234M).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
33、solids content determinationas 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, as variations in surface areawould directly affect the leaching characteristics o
34、f the sample.Waste samples should contain a representative distribution ofparticle sizes.NOTE 6Information on obtaining representative samples can also be3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents
35、 notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D5284092found in Pierre Gys Sampling Theory and Sampling Practi
36、ce.47.5 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 col
37、lection 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 t
38、he approximate 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
39、thesheet.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.8.1.3 Remix the sample by lifting a corner of the sheet anddrawing it low across to the opposite corner in such a mannerthat the material is
40、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 all four corners of the sheet toward the center and,holding all four corners together, raise the entire sheet into theair
41、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 as the flattened mound of sample, gently dividethe sample into quarters. Make an effort to avoid using pressureon the stra
42、ightedge sufficient to cause damage to the particles.8.1.7 Discard the alternate quarters.4Pitard, F., Pierre Gys Sampling Theory and Sampling Practice, Vols I and II,CRC Press, 1989.FIG. 1 ExtractorsD52840938.1.8 If further reduction of the sample size is necessary,repeat the steps given in 8.1.3 t
43、hrough 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 differ
44、ent 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.4The method of subsampling should be deter-mined by the physical properties of the waste, analytes of intere
45、st, 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 be
46、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 size
47、 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 Pla
48、ce 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 in 9
49、.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 of co
