ASTM D4793-1993(2004) Standard Test Method for Sequential Batch Extraction of Waste with Water《含水废弃物的连续成批萃取的试验方法》.pdf

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1、Designation: D 4793 93 (Reapproved 2004)Standard 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

2、 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 test method is a procedure for the sequentialleaching of a waste containing at least five % solids to generates

3、olutions to be used 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 o

4、n 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 This standard

5、 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 Documents2.1 ASTM

6、Standards:2D 75 Practices for Sampling AggregatesD 420 Practice for Investigating and Sampling Soil andRock for Engineering PurposesD 653 Terminology Relating to Soil, Rock, and ContainedFluidsD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2216 Test Method for Laboratory

7、 Determination of Water(Moisture) Content of Soil, Rock, and Soil-AggregateMixturesD 2234 Test Method 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 Water3. Terminology3.1 Definitions:3.

8、1.1 For definitions of terms used in this test method, seeTerminology D 1129.3.2 Symbols:Symbols:3.2.1 Variables 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

9、mean valueXa= analytical mean value (calculated using data fromanalysis of standards)Stt= total standard deviationSta= analytical standard deviationSte= estimated standard deviation due to the extractionprocedureSot= total single operator standard deviationSoa= analytical single operator standard de

10、viationSoe= estimated single operator standard deviation due tothe extraction procedure4. Significance and 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 laborat

11、ory 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 field or to produce extracts to be used as the sole basisof engineering design.4.3 This test method is not intended to simul

12、ate 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 interaction of the extractant with thebuffering capacity of the waste.1This test method is

13、 under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 onAncillary Topics.Current edition approved Jan. 15, 1993. Published March 1993. Originallypublished as D 4793 88. Last previous edition D 4793 88.2For referenced ASTM standard

14、s, 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 Conshohocken, PA 1

15、9428-2959, United States.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 determination of both major and minor constituents. Wh

16、enminor 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 inorganic components in the waste. Thistest metho

17、d 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 besuitable for extracting all types of wastes (see S

18、ections 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 or DishesTwo per waste (for example,aluminu

19、m 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 62C ina range from 100 to 110C.5.5 Desiccator, having the capacity to hold th

20、e 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.5.10 Large Glass Funnel.5.11 Wash Bottle, 50

21、0-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 Equipment, of any type that rotates theextraction vessel in an end-over-end fashion at a rate of 30 6 2r/min such that the axis of rotation is horizontal and it

22、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 filtrationdevice of a composition suitable to the natu

23、re 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, constructed of materials that will not allow sorpti

24、onof 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 havewater-tight closure. Containers for samples where gases ma

25、ybe released should be provided with a venting mechanism.NOTE 2Suitable container sizes range from 4.0 to 4.5 in. (102 to 114mm) in diameter and 8.5 to 13.0 in. (216 to 330 mm) in height.NOTE 3The venting of the container has the potential to affect theconcentration of volatile compounds in the extr

26、acts.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 chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to t

27、he specifications of the AmericanChemical Society, where such specifications are available.3Other 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

28、se 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 exchange, reverseosmosis, electrodialysis, or a combination thereof, shouldremain constant throughout testing.7.

29、 Sampling7.1 Obtain a representative sample of the waste to be testedusing ASTM sampling methods developed for the specificindustry where available (see Practices D 75 and D 420,Terminology D 653, and Test Method D 2234).7.2 Where no specific methods are available, samplingmethodology for material o

30、f 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 100 g of sample on a dryweight basis for each extraction.7.4 It is important that the sample of the waste be re

31、presen-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 distribution ofparticle sizes.NOTE 4Information on obtaining representative samples can also befound in Pierre Gys S

32、ampling 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 closed containersappropriate to the sample type and desired analysis. SeePractices D 3370 for guidance. Record the

33、 storage conditionsand handling procedures in the report.3“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-cal Soc., Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see “Reagent Chemicals and Standards,” by JosephRosin, D

34、. Van Nostrand Co., Inc., New York, NY, and the “United StatesPharmacopeia.”D 4793 93 (2004)27.6 The time between collection 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 sa

35、mple 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-meable sheet of glazed paper, oil cloth, or other flexiblematerial as f

36、ollows: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 the sample by lifting a corner of the sheet anddrawing it across, low

37、down, to the opposite corner in 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.FIG. 1 ExtractorsD 4793 93 (2004)38.1.4 Lift all four corners of the she

38、et 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 the flattened mound of sample, gentlydivide the sample into quarters.

39、 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 give 100 g of solid for eachextraction. Provide additional samples fo

40、r 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 Sampling Practice, Volumes I and II, by F. Picard, CRC Press, 1989.The meth

41、od 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 weighing approxi-mately 100 g for testing plus samples for determination f

42、orsolids 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 fordetermination of solids content at the same time as the testsamples.9. Procedure9.

43、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 weight at 104 6 2C two dishes orpans of size suitable to the solid waste

44、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. Use a minimum of 50 g, butuse larger samples where particles larger than

45、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 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-sa

46、mple 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.A

47、verage the two values obtained. Record the solids content.9.3 Extraction ProcedureIf the entire procedure cannot beconducted without interruption, 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 ext

48、raction procedure to the nearest 0.1 g. Record themass of the extraction vessel, Mv1. Use one extraction vesselper waste throughout the 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 t

49、o 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 100 gis not recommended.9.3.3 Add a volume in millilitres, Vvl, of test water (see 6.2)to the extraction vessel determined using the following equa-tions:Msw5 M 2 1