ASTM D4793-09(2017) Standard Test Method for Sequential Batch Extraction of Waste with Water.pdf

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1、Designation: D4793 09 (Reapproved 2017)Standard Test Method forSequential Batch Extraction of Waste with Water1This standard is issued under the fixed designation D4793; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l

2、ast 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 is a procedure for the sequentialleaching of a waste containing at least five percent solids togenerat

3、e 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 water of a specified purity and the separation ofthe aqueous phase for analysis. The procedure is conducted tentimes in sequenc

4、e on the same sample of 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

5、 stated in SI units are 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 concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safet

6、y, health and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of In

7、ternational Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D75/D75M Practice for Sampling AggregatesD420 Guide to Site Characterization for Engineering Designand Construction Purposes

8、 (Withdrawn 2011)3D653 Terminology Relating to Soil, Rock, and ContainedFluidsD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2216 Test Methods for Laboratory Determination of Water(Moisture) Content of Soil and Rock by MassD2234/D2234M Practice for Collection of a Gross Sam

9、pleof CoalD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed Conduits3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method, seeTerminology D1129.3.2 Symbols:3.2.1 Var

10、iables listed in this test method are defined in theindividual sections 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 d

11、eviationSta= analytical standard deviationSte= estimated standard deviation 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

12、 Use4.1 This test method 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.1This test method is under the jurisdiction of ASTM Committee

13、 D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 on WasteLeaching Techniques.Current edition approved Sept. 1, 2017. Published September 2017. Originallyapproved in 1988. Last previous edition approved in 2009 as D4793 09. DOI:10.1520/D4793-09R17.2For referenced AST

14、M 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.3The last approved version of this historical standard is referenced onwww.astm.

15、org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of I

16、nternational Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.2 This test method is not intended to provide extracts thatare representative of the actual leachate produced from a wastein the field or to produce extracts to be

17、 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 of eachof the extracts reflects the

18、interaction of the extractant with thebuffering capacity of the waste.4.5 An intent of this test method is that the water extractionsreflect conditions where the waste is the dominant factor indetermining the pH of the extracts.4.6 This test method produces extracts that are amenable tothe determina

19、tion 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 contamination of the samples.4.7 This test method has been tested to determine itsapplicability to certain inor

20、ganic 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 agitation technique, rate, liquid-to-solid ratio, andfiltration conditions specified in the procedure may not besuitab

21、le 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 paper, oil cloth, or otherflexible material of a composition suitable to the analytes ofinterest.5.3 Drying Pans

22、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 thermostatically controlled dryingoven capable of maintaining a steady temperature of 62Cina range from 100 to 110 C.5.5

23、 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.5.8 CruciblesTwo per waste, porcelain, 20-mL capacityeach.5.9 Analytical Balance, capable of weighing to 0.1 mg.5

24、.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 25 C is acceptable.5.13 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 t

25、hat 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 arrangement may beused if equivalency can be demonstrated.5.14 Pressure Filtration AssemblyA pressure filtratio

26、ndevice 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, cylindrical, wide-mouth, of a com-position suitable to the nature of the waste and analyses to beperformed, constr

27、ucted 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 that the sample plus extraction fluid occupyapproximately 95 % of the container. Containers must havewatertight cl

28、osure. Containers for samples where gases may bereleased should be provided with a venting mechanism.NOTE 2Suitable container sizes range from 10 to 11 cm in diameterand 22 to 33 cm in height.NOTE 3Venting the container has the potential to affect the concen-tration of volatile compounds in the extr

29、acts.5.15.1 Extraction vessels should be cleaned in a mannerconsistent with the analyses to be performed. See Section 13 ofPractices D3370.6. Reagents6.1 Purity of ReagentsReagent-grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to

30、the specifications of theAmericanChemical Society, where such specifications are available.4Other grades may be used, provided it is first ascertained thatthe reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwi

31、se indicated, referencesto water shall be understood to mean Type IV reagent water at18 to 27 C (Specification D1193). The method by which thewater is prepared, that is, distillation, ion exchange, reverseosmosis, electrodialysis, or a combination thereof, shouldremain constant throughout testing.7.

32、 Sampling7.1 Obtain a representative sample of the waste to be testedusing ASTM sampling methods developed for the specificindustry where available (see Practice D75/D75M, GuideD420, Terminology D653, and Test Method D2234/D2234M).4Reagent Chemicals, American Chemical Society Specifications, America

33、nChemical Society, Washington, DC. For Suggestions on the 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),

34、 Rockville,MD.D4793 09 (2017)27.2 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 provide 10

35、0 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 representative distrib

36、ution 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 samples in close

37、d containersappropriate to the sample type and desired analysis. SeePractices D3370 for guidance. Record the storage conditionsand handling procedures in the report.7.6 The time between collection and extraction of thesample should be determined by the nature of the sample andthe information desired

38、. See Practices D3370 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 approximate size required in the test by quarter-ing the sample (Section 7) received for testing on an imper-

39、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 straight-edge until it is spread uniformly to a depth at least twice themaximum particle diameter.8.1.3 Remix

40、 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 notFIG. 1 ExtractorsD4793 09 (2017)3merely slide along. Continue the operation with each corner,proceeding in a clockwise direction.

41、 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 straightedge (such as a thin-edged yard stick),one at least as long as

42、 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 reduction of sample size is necessary, repeat8.1.3 8.1.7. Use a sample size to

43、 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 subsamplingfree-flowing solid particulate wastes, see Pierre Gys Sampling Theoryand Sampl

44、ing 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 field-cored solid wastes or castings produced in thelaboratory, cut a representative section weig

45、hing 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 thoroughly to ensure that arepresentative sample will be withdrawn. Take samples fordeterminatio

46、n 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 the solids content of twoseparate portions of the sample as follows:9.2.1 Dry to a constant wei

47、ght at 104 6 2 C 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 to be tested into each pan. Scale the weight used to thephysical form of the waste tested. Us

48、e a minimum of 50 g, butuse larger samples where particles larger than 10 mm inaverage diameter are being tested (see Test Methods D2216).9.2.3 Dry 16 to 20 h at 104 6 2 C. Record the temperatureand time of the drying period.9.2.4 Cool to room temperature in a desiccator and reweigh.Record the mass

49、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 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 interruption, at least the first four extractionsequenc