ASTM D3987-2006 Standard Test Method for Shake Extraction of Solid Waste with Water《含水固体废弃物的振荡萃取用标准试验方法》.pdf

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1、Designation: D 3987 06Standard Test Method forShake Extraction of Solid Waste with Water1This standard is issued under the fixed designation D 3987; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numbe

2、r 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 covers a procedure for leaching ofsolid waste to obtain an aqueous solution to be used todetermine the materials leached u

3、nder the specified testingconditions.1.2 This test method provides for the shaking of a knownweight of waste with water of specified composition and theseparation of the aqueous phase for analysis.1.3 This standard does not purport to address all of thesafety problems, if any, associated with its us

4、e. 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 Standards:2C 471M Test Methods for Chemical Analysis of Gypsumand Gypsum Products Metr

5、icD75 Practice for Sampling AggregatesD 420 Guide to Site Characterization for Engineering De-sign and Construction PurposesD 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 Mass

6、D 2234/D 2234M Practice for Collection of a Gross Sampleof CoalD 3370 Practices for Sampling Water from Closed ConduitsE 122 Practice for Calculating Sample Size to Estimate,With a Specified Tolerable Error, the Average for aCharacteristic of a Lot or Process3. Terminology Definitions3.1 For definit

7、ions of terms used in this test method, seeTerminology D 1129.4. Significance and Use4.1 This test method is intended as a rapid means forobtaining an extract of solid waste. The extract may be used toestimate the release of certain constituents of the solid wasteunder the laboratory conditions desc

8、ribed in this procedure.4.2 This test method is not intended to provide an extractthat is representative of the actual leachate produced from asolid waste in the field or to produce extracts to be used as thesole basis of engineering design.4.3 This test method is not intended to simulate site-speci

9、ficleaching conditions. It has not been demonstrated to simulateactual disposal site leaching conditions.4.4 The intent of this test method is that the final pH of theextract reflect the interaction of the extractant with the buffer-ing capacity of the solid waste.4.5 The intent of this test method

10、is that the water extractionsimulate conditions where the solid waste is the dominantfactor in determining the pH of the extract.4.6 The test method produces an extract that is amenable tothe determination of both major and minor constituents. Whenminor constituents are being determined, it is espec

11、iallyimportant 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 solidwaste. The test method has not been tested for applicability toorganic

12、 substances and volatile matter (see 5.3).4.8 The agitation technique, rate, and liquid-to-solid ratiospecified in the procedure may not be suitable for extracting alltypes of solid wastes. (See Sections 7, 8, and the discussion inAppendix X1.)5. Apparatus5.1 Agitation Equipment, of any type that ro

13、tates about acentral axis at a rate of 29 r/min, Fig. 1. (See discussion ofagitation in Appendix X1.)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 approved Oc

14、t. 1, 2006. Published October 2006. Originallyapproved in 1981. Last previous edition approved in 2004 as D 3987 85 (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, re

15、fer 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.5.2 Membrane Filter AssemblyA borosilicate glass orstainless steel funnel with a flat, fritted base of the samematerial and

16、 membrane filters.5.3 Containers, round, wide-mouth, of a composition suit-able to the nature of the solid waste and the analyses to beperformed, and constructed of materials that will not allowsorption of constituents of interest. One-gallon (or 4-L) con-tainers should be used with 140-g samples an

17、d12-gallon (or2-L) containers with 70-g samples. Multiples of these sizesmay be used for larger samples. The containers should be of thesame approximate geometry as the 2-L and 4-L bottles. Thesesizes were selected to establish suitable geometry and providethat the sample plus liquid would occupy ap

18、proximately 80 to90 % of the container. Containers must have a watertightclosure. Containers for samples where gases may be releasedshould be provided with a venting mechanism. (Note that theventing of the container has the potential to affect the concen-tration of volatile extracts in the extract.)

19、 Containers should becleaned in a manner consistent with the analyses to beperformed.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 AmericanChemical Society, wh

20、ere 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.3“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-cal Soc., Wa

21、shington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see “Reagent Chemicals and Standards,” by JosephRosin. D. Van Nostrand Co., Inc., New York, NY, and the “United StatesPharmacopeia.”FIG. 1 ExtractorD39870626.2 Purity of WaterUnless otherwise indicat

22、ed, referencesto water shall be understood to mean Type IV reagent water at18 to 27C (Specification D 1193). The method by which theType IV water is prepared, that is, distillation, ion exchange,reverse osmosis, electrodialysis, should remain constantthroughout testing.7. Sampling7.1 Obtain a repres

23、entative sample of the solid waste to betested using ASTM sample methods developed for the specificindustry where available. (See Practices D 75 and D 420 andTest Methods D 2234/D 2234M.)7.2 Where no specific methods are available, samplingmethodology for materials of similar physical form shall beu

24、sed.7.3 A minimum sample of 5000 g shall be sent to thelaboratory (see Practice E 122).7.4 It is important that the sample of the solid waste berepresentative with respect to surface area, as variations insurface area would directly affect the leaching characteristicsof the sample. Solid waste sampl

25、es should contain a represen-tative distribution of particles sizes.7.5 Keep samples in closed containers appropriate to thesample type prior to the extraction in order to prevent samplecontamination or constituent loss. Where it is desired to extractbiologically or chemically active samples in thei

26、r existingstate, store the samples at 4C (Practices D 3370) and start theextraction within 8 h. Where it is desired to extract suchsamples in a state representative of the results of biological orchemical activities, the samples may be specifically handled tosimulate such activities. Record the stor

27、age conditions andhandling procedures in the report.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

28、 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 particle size.8.1.3 Remix the sample by lifting a corner of

29、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. Continue operation with each corner,proceeding in a clockwise direction. Repeat this operation tentimes.8.1.4 Lift all four corners of the sheet

30、 towards the center andholding all four corners together, raise the entire sheet into theair to form a pocket for the sample.8.1.5 Repeat 8.1.2.8.1.6 With a straightedge at least as long as the flattenedmound of sample (such as a thin-edged yard stick), gentlydivide the sample into quarters. An effo

31、rt should be made toavoid using pressure on the straightedge sufficient to causedamage to the particles.8.1.7 Discard alternate quarters.8.1.8 If further reduction of sample size is necessary, repeat8.1.3 through 8.1.7. A minimum sample size of 70 g isrecommended for each extraction. Additional samp

32、les shouldbe provided for determination of solids content. If smallersamples are used in the test, report this fact.8.2 For field-cored solid wastes or castings produced in thelaboratory, cut a representative section weighing approxi-mately 70 or 140 g for testing, plus samples for determinationof s

33、olids content. Shape the sample so that the leachingsolution will cover the material to be leached.8.3 For fluid solid wastes, mix thoroughly in a manner thatdoes not incorporate air to assure uniformity before withdraw-ing a 70 or 140 g sample for test. Take samples for determi-nation of solids con

34、tent at the same time as the test samples.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 sepa-rate portions of the sample as follows:9.2.1 Dry to constant weight two dishes or p

35、ans of sizesuitable to the solid waste being tested at 104 6 2C. Cool ina desiccator and weigh. Record the value to 6 0.1 g.9.2.2 Put an appropriately sized portion of sample of thesolid waste to be tested into each pan. Scale the weight used tothe physical form of the solid waste tested. Use a mini

36、mum of50 g but use larger samples where particles larger than 10-mmin average diameter are being tested. Weigh. Record the weightto 6 0.1 g.9.2.3 Dry 16 to 20 h at 104 6 2C. Certain solid wastes,such as scrubber sludges, may contain compounds that aresubject to calcination at the specified drying te

37、mperature. Drythese compounds at lower temperatures. For example, gypsummay be successfully dried at 45C (Test Methods C 471M) andCaSO31/2H2O wastes at 85C. Record the actual temperatureand time of the drying period.9.2.4 Cool to room temperature in a desiccator and reweigh.Record the weight to 6 0.

38、1 g.9.3 Shake ProcedureWeigh or tare the container to beused in the shake test to the nearest or within 1 g.9.4 Add to the container approximately 70 g of solid waste(Section 8) and determine and record the weight of sampleused to12 g. If weights other than 70 g are used, note in thereport.9.5 Add t

39、o the container a volume of test water (6.2) equalin millilitres to 20 times the weight in grams of the sample usedin 9.4. See discussion of dilution ratio in Appendix (Example:70 g sample = 1400 mL water).9.6 Agitate continuously for 18 6 0.25 h at 18 to 27C.9.7 Open the container. Observe and reco

40、rd any physicalchanges in the sample and leaching solution.9.8 Let the sample settle for 5 min; then separate the bulk ofthe aqueous phase from the solid phase by decantation,centrifugation, or filtration through a coarse filter paper asappropriate. Then vacuum or pressure filter the liquid througha

41、 0.45-m filter. If the separation method results in prolongedfiltering time, an 8-m filter or other device may be used.Record any deviations in the report.D39870639.9 The filtrate obtained in 9.8 is the extract mentionedelsewhere in this test method. Measure the pH of the extractimmediately, then pr

42、eserve the extract in a manner consistentwith the chemical analysis or biological testing procedures tobe performed (Practices D 3370). If sufficient liquid phase isnot available for the analyses, so indicate in the report and donot continue the procedure; or alternatively, perform theextraction pro

43、cedure on additional samples of the solid wasteto obtain sufficient liquid phase. Where phase separation occursduring the storage of the extract, appropriate mixing should beused to ensure the homogeneity of the extract prior to its use insuch analysis or testing.9.10 Analyze the extract for specifi

44、c constituents or proper-ties or use the extract for biological testing procedures asdesired using appropriate ASTM standard methods. Where noappropriate ASTM methods exist, other methods may be usedand recorded in the report.10. Calculation10.1 Calculate the solids content of the individual samples

45、from the data obtained in 9.2 as follows:S 5 A/B (1)where:A = weight in grams of sample after drying,B = original weight in grams of sample, andS = solid content, g/g.Average the two values obtained. Record as the solidscontent.11. Report11.1 The report shall include the following:11.1.1 Source of t

46、he solid waste, date of sampling, andsample preservation used,11.1.2 Description of the solid waste including physicalcharacteristics and particle size, if known (9.1),11.1.3 Solids content (9.2) (see Test Method D 2216),11.1.4 Sample weight if other than 70 g,11.1.5 Drying time and temperature if o

47、ther than 16 to 20 hat 104 6 2C,11.1.6 pH and results of specific analyses calculated inappropriate units. State analytical procedures used, and filterused if other than 0.45 m,11.1.7 Observation of changes in test material or leachingsolution recorded in 9.8.11.1.8 Date leach testing started, prese

48、rvation used forextract, and date of analysis.12. Precision and Bias12.1 No information is presently available as to the preci-sion or bias of the analysis of specific constituents in theextract. It is recommended that users of this test methodvalidate the applicability of their chosen methods of de

49、tectionby spiking portions of the extract, before using these testmethods for the analysis of the extract.12.2 Based on a collaborative series of tests on five solidwastes including fly ash, cutting waste, aluminum industrywaste, foundry waste, and non-ferrous foundry waste, theoverall precision of this test method was improved.12.3 The precision of this test method may vary dependingon the solid waste being tested and on the element beingextracted.12.4 Determination of the bias of this test method is notpossible, as no standard reference material exists.APPENDIX