ASTM D4793-2009 Standard Test Method for Sequential Batch Extraction of Waste with Water《含水废弃物的连续成批萃取的标准试验方法》.pdf

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1、Designation: D 4793 09Standard Test Method forSequential Batch Extraction of Waste with Water1This standard is issued under the fixed designation D 4793; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A

2、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 is a procedure for the sequentialleaching of a waste containing at least five % solids to generatesolutions to be used

3、 to determine the constituents leachedunder the specified testing conditions.1.2 This test method calls for the shaking of a known weightof waste with water of a specified purity and the separation ofthe aqueous phase for analysis. The procedure is conducted tentimes in sequence on the same sample o

4、f waste and generatesten aqueous solutions.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 ar

5、e 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 problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices

6、 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 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

7、 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2216 Test Methods for Laboratory Determination of Wa-ter (Moisture) Content of Soil and Rock by MassD 2234/D 2234M Practice for Collection of a Gross Sampleof CoalD 2777 Practice for Determination of Precision and Bias ofAppl

8、icable Test Methods of Committee D19 on WaterD 3370 Practices for Sampling Water from Closed Conduits3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method, seeTerminology D 1129.3.2 Symbols:3.2.1 Variables listed in this test method are defined in theindividual sectio

9、ns where they are discussed. A list of definedvariables is also given in Section 11.3.2.2 Explanation of Variables:Xt= total mean valueXa= analytical mean value (calculated using data fromanalysis of standards)Stt= total standard deviationSta= analytical standard deviationSte= estimated standard dev

10、iation due to the extractionprocedureSot= total single operator standard deviationSoa= analytical single operator standard deviationSoe= estimated single operator standard deviation due tothe extraction procedure4. Significance and Use4.1 This test method is intended as a means for obtainingsequenti

11、al 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 This test method is not intended to provide extracts thatare representative of the actual leachate produced from a wastein the

12、 field or to produce extracts to be used as the sole basisof engineering design.4.3 This test method is not intended to simulate site-specificleaching conditions. It has not been demonstrated to simulateactual disposal site leaching conditions.4.4 An intent of this test method is that the final pH o

13、f eachof the extracts reflects the interaction of the extractant with thebuffering capacity of the waste.1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 on WasteLeaching Techniques.Current edition approve

14、d July 1, 2009. Published October 2009. Originallyapproved in 1988. Last previous edition approved in 2004 as D 4793 93 (2004).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

15、, 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 An intent of this test method is that the water extractionsreflect conditions where the waste is the dominant facto

16、r indetermining the pH of the extracts.4.6 This test method produces extracts that are amenable tothe determination of both major and minor constituents. Whenminor constituents are being determined, it is especiallyimportant that precautions are taken in sample storage andhandling to avoid possible

17、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 3 in 5.15), or biologicallyactive samples.4.8 The agitati

18、on technique, rate, liquid-to-solid ratio, andfiltration conditions specified in the procedure may not besuitable for extracting all types of wastes (see Sections 7, 8,and the discussion in Appendix X1).5. Apparatus5.1 Straightedge (such as a thin-edged yard stick).5.2 Impermeable Sheet, of glazed p

19、aper, oil cloth, or otherflexible material of a composition suitable to the analytes ofinterest.5.3 Drying Pans or DishesTwo per waste (for example,aluminum tins, porcelain dishes, or glass weighing pans),suitable to the waste being tested and the instructions given in9.2.5.4 Drying OvenAny thermost

20、atically controlled dryingoven capable of maintaining a steady temperature of 62C ina range from 100 to 110C.5.5 Desiccator, having the capacity to hold the drying pansdescribed in 5.3 and the crucibles described in 5.8.5.6 Laboratory Balance, capable of weighing to 0.1 g.5.7 Pipet, 10-mL capacity.5

21、.8 CruciblesTwo per waste, porcelain, 20-mL capacityeach.5.9 Analytical Balance, capable of weighing to 0.1 mg.5.10 Large Glass Funnel.5.11 Wash Bottle, 500-mL capacity.5.12 pH MeterAny pH meter with a readability of 0.01units and an accuracy of 60.05 units at 25C is acceptable.5.13 Agitation Equipm

22、ent, 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 goesthrough the center of the bottle, (see Fig. 1 and the discussionof agitation in Appendix X1).NOTE 1Similar devices having a different axial

23、 arrangement may beused if equivalency can be demonstrated.5.14 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 Note 7, pertaining to 9.4).5.15 Extraction Vessels, cy

24、lindrical, 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 constituents of interest, and sturdy enough to withstand theimpact of the falling sample fragments. Container size shouldbe selected so th

25、at the sample plus extraction fluid occupyapproximately 95 % of the container. Containers must havewater-tight closure. Containers for samples where gases maybe released should be provided with a venting mechanism.NOTE 2Suitable container sizes range from 10 to 11 cm in diameterand 22 to 33 cm in he

26、ight.NOTE 3Venting the container has the potential to affect the concen-tration of volatile compounds in the extracts.5.15.1 Extraction vessels should be cleaned in a mannerconsistent with the analyses to be performed. See PracticesD 3370, Section 13.6. Reagents6.1 Purity of ReagentsReagent grade ch

27、emicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of theAmericanChemical Society, where such specifications are available.3Other grades may be used, provided it is first ascertained thatthe reagent is of sufficiently hi

28、gh purity to permit its usewithout lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type IV reagent water at18 to 27C (Specification D 1193). The method by which thewater is prepared, that is, distillation, ion

29、exchange, reverseosmosis, electrodialysis, or a combination thereof, shouldremain constant throughout testing.7. Sampling7.1 Obtain a representative sample of the waste to be testedusing ASTM sampling methods developed for the specificindustry where available (see Practices D75 and D 420,Terminology

30、 D 653, and Test Method D 2234/D 2234M).7.2 Where no specific methods are available, samplingmethodology for material of similar physical form shall beused.7.3 The amount of sample to be sent to the laboratoryshould be sufficient to perform the solids content determinationas specified in 9.2 and to

31、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 of the sample.Waste samples should contain a representati

32、ve distribution ofparticle sizes.NOTE 4Information on obtaining representative samples can also befound in Pierre Gys Sampling Theory and Sampling Practice, Volumes Iand II, by F. Picard, CRC Press, 1989.7.5 In order to prevent sample contamination or constituentloss prior to extraction, keep sample

33、s in closed containersappropriate to the sample type and desired analysis. SeePractices D 3370 for guidance. Record the storage conditionsand handling procedures in the report.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on t

34、he testing of reagents 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.D47930927.6 The time between collection a

35、nd 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 approx

36、imate 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 as follows:8.1.1 Empty the sample container into the center of thesheet.8.1.2 Flatten out the sample gently with a suitable straig

37、ht-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 across, low down, to the opposite corner in a mannerthat the material is made to roll over and over and does notmerely slide along. Contin

38、ue the operation with each corner,proceeding in a clockwise direction. Repeat this operation tentimes.8.1.4 Lift all four corners of the sheet towards the centerand, holding all four corners together, raise the entire sheet intothe air to form a pocket for the sample.8.1.5 Repeat 8.1.2.8.1.6 With a

39、straightedge (such as a thin-edged yard stick),one at least as long as the flattened mound of sample, gentlydivide the sample into quarters. Make an effort to avoid usingpressure on the straightedge sufficient to cause damage to theparticles.8.1.7 Discard alternate quarters.8.1.8 If further reductio

40、n of sample size is necessary, repeat8.1.3-8.1.7. Use a sample size to give 100 g of solid for eachextraction. Provide additional samples for determination ofsolids content. If smaller samples are used in the test, reportthis fact.NOTE 5For other acceptable methods for mixing and subsamplingFIG. 1 E

41、xtractorsD4793093free-flowing solid particulate wastes, see Pierre Gys Sampling Theoryand Sampling Practice, Volumes I and II, by F. Picard, CRC Press, 1989.The method of subsampling should be determined by the physicalproperties of the waste, analytes of interest, and equipment available.8.2 For fi

42、eld-cored solid wastes or castings produced in thelaboratory, cut a representative section weighing approxi-mately 100 g for testing plus samples for determination forsolids content. Shape the sample so that the leaching solutionwill cover the material to be leached.8.3 For multiphasic wastes, mix t

43、horoughly to ensure that arepresentative sample will be withdrawn. Take samples fordetermination of solids content at the same time as the testsamples.9. Procedure9.1 Record the physical description of the sample to betested, including particle size so far as it is known.9.2 Solids ContentDetermine

44、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 Put an appropriately sized portion of sample of thewaste

45、 to be tested into each pan. Scale the weight used to thephysical form of the waste tested. Use a minimum of 50 g, butuse larger samples where particles larger than 10 mm inaverage diameter are being tested (see Test Method D 2216).9.2.3 Dry 16 to 20 h at 104 6 2C. Record the temperatureand time of

46、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 steps 9.2.3 and 9.2.4 until constant container-sample masses are obtained. Discard the dried samples follow-ing completion of this step.9.2.6 Calculate the solids content of the sample

47、 from thedata obtained in 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 Extraction ProcedureIf the entire procedure cannot beconducted without in

48、terruption, at least the first four extractionsequences must be conducted without interruption.9.3.1 Determine the mass of the extraction vessel to be usedin the extraction procedure to the nearest 0.1 g. Record themass of the extraction vessel, Mv1. Use one extraction vesselper waste throughout the

49、 sequence of extractions.9.3.2 Add 100 g (weighed to 60.1 g) of solid waste on a dryweight basis to the extraction vessel. Calculate the amount ofwaste as received to add using the following equation:M 5100S(2)where:M = mass of waste as received to add to the extractionvessel to give 100 g (weighed to 60.1 g) of solidwaste.9.3.2.1 If a mass of solid waste on a dry weight basis otherthan 100 g is used, (Eq 2) through (4) must be modified toreflect the use of a mass other than 100 g. Replace 100 in theseequations with the mass used. Use of a mass other than 10