ASTM D5284-09(2017) Standard Test Method for Sequential Batch Extraction of Waste with Acidic Extraction Fluid.pdf

1、Designation: D5284 09 (Reapproved 2017)Standard Test Method forSequential Batch Extraction of Waste with Acidic ExtractionFluid1This standard is issued under the fixed designation D5284; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi

2、on, the year of 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 % dr

3、y solids in orderto 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

4、analysis. ThepH 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 t

5、o 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 are to be regarded asstandard. No other units of measurement are included in th

6、isstandard.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 safety, health and environmental practices and deter-mine the applicability of regulatory limitations pr

7、ior 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 International Standards, Guides and Recom-mendations issued by the World Trade Organization Technical

8、Barriers 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Practice for Sampling AggregatesD420 Guide to Site Characterization for Engineering Designand Construction Purposes (Withdrawn 2011)3D653 Terminology Relating to Soil, Rock, and ContainedFluidsD1129 Terminology Rel

9、ating to WaterD1193 Specification for Reagent WaterD2234/D2234M Practice for Collection of a Gross Sampleof CoalD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD4793 Test Method for Seque

10、ntial Batch Extraction ofWaste with Water3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, see Terminology D1129.3.2 SymbolsVariables listed in this test method are definedin the individual sections in which they are discussed. A list ofthe defined variables is also prov

11、ided in Section 11.4. 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 laboratory conditions described in this test method.4.2 The pH of the extra

12、ction fluid used in this test method isto reflect the pH of acidic precipitation in the geographic regionin which the waste being tested is to be disposed.1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 o

13、n WasteLeaching Techniques.Current edition approved Sept. 1, 2017. Published September 2017. Originallyapproved in 1992. Last previous edition approved in 2009 as D5284 09. DOI:10.1520/D5284-09R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service a

14、t 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.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohoc

15、ken, 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 International Standards, Guides and Recommendations issued by the World Trade Organiz

16、ation Technical Barriers to Trade (TBT) Committee.1NOTE 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 sequential batch extraction of waste using a

17、 nonacidicextraction fluid, see Test Method D4793.4.3 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 provide extracts thatare representative of the a

18、ctual 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 extracts that are amenable tothe determination of

19、 both major and minor (trace) constituents.When minor constituents are being determined, it is especiallyimportant that precautions be 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 5), or biologically activesamples.4.8 The agitation technique, rate, liquid-to-solid ratio, andfiltration conditions specified in the procedure may not besuitable for e

21、xtracting all types of wastes (see Sections 7 and 8and Appendix X1).5. Apparatus5.1 Straightedge, such as a thin-edged yardstick.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 Dishes (for example, a

22、luminum 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 controlled dryingoven capable of maintaining a steady temperature of 62Cina range of 100 to 110 C.5.5 Desiccator, having a capac

23、ity 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 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.5.1

24、1 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 readability of 0.01units and an accuracy of 60.05 units at 25 C.5.14 Carboy-Type Container, with spigot, 20- to 50-Lcapacity, o

25、f a composition suitable to the nature of the analysesto be performed (see Practices D3370).5.15 Large Glass Funnel.5.16 Crucibles, porcelain, 20-mL capacity each, two perwaste.5.17 Analytical Balance, capable of weighing to 0.1 mg.5.18 Wash Bottle, 500-mL capacity.5.19 Agitation Equipment, of any t

26、ype 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 bottle (see Fig. 1 and Appendix X1).NOTE 3Similar devices having a different axial arrangement may beused if equivalency can

27、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 0.8-m pore sizefilter (see Note 8).5.21 Extraction Vessels, cylindrical, wide-mouth, of a com-position suitable to the natur

28、e 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 falling sample fragments. The size of thecontainer should be selected so that the sample plus extractionfluid occupy appro

29、ximately 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.NOTE 4Suitable container sizes range from 10 to 11 cm in diameterand 22 to 33 cm in height.NOTE 5Venting the container has th

30、e 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 (see Section 13 ofPractices D3370).6. Reagents6.1 Purity of ReagentsReagent-grade chemicals shall beused in all tests. Un

31、less 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 specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficientl

32、y high purity to permit its use without lessening theaccuracy of the determination.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for L

33、aboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D5284 09 (2017)26.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type IV reagent water at

34、18 to 27 C conforming to Specification D1193. 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 SolutionA60/40 weight per-cent (wt %) mixture

35、 prepared using 95 to 98 wt % sulfuric acidand 69 to 71 wt % nitric acid. (See 9.3 for instructions on thepreparation of this solution.)7. Sampling7.1 Obtain a representative sample of the waste to be testedby using, where available,ASTM sampling methods developedfor the specific industry (see Pract

36、ice D75/D75M, Guide D420,Terminology D653, and Practice D2234/D2234M).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 solids content determina

37、tionas 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 of the sample.Waste sampl

38、es should contain a representative distribution ofparticle sizes.NOTE 6Information on obtaining representative samples can also befound in Pierre Gys Sampling Theory and Sampling Practice.57.5 In order to prevent sample contamination or constituentloss prior to extraction, keep the samples in closed

39、 containersappropriate to sample type and desired analysis. See PracticesD3370 for guidance. Record the storage conditions and han-dling procedures in the report.7.6 The time between collection and extraction of thesample should be determined by the nature of the sample and5Pitard, F., Pierre Gys Sa

40、mpling Theory and Sampling Practice, Vols I and II,CRC Press, 1989.FIG. 1 ExtractorsD5284 09 (2017)3the information desired. 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 a

41、sample 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 having a composition suitable to the analytes ofinterest, as follows:8.1.1 Empty the sample container into the

42、 center of 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 m

43、aterial 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.8.1.4 Lift all four corners of the sheet toward the center and,holding all four corners together, raise the entire sheet i

44、nto theair 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 pressure

45、on the straightedge sufficient to cause damage to the particles.8.1.7 Discard the alternate quarters.8.1.8 If further reduction of the sample size is necessary,repeat the steps given in 8.1.3 8.1.7. Use a sample size toprovide 100 g of solid on a dry weight basis for eachextraction. Provide addition

46、al 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 different sample size is used, report thisfact.NOTE 7For other acceptable methods of mixing and subsamplingfree-flowing s

47、olid particulate wastes, see Pierre Gys Sampling Theoryand Sampling Practice.5The method of subsampling should be deter-mined by the physical properties of the waste, analytes of interest, andequipment available.8.2 For field-cored solid wastes or castings produced in thelaboratory, cut a representa

48、tive 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 leached.8.3 For multiphasic wastes, mix thoroughly to ensure that arepresentative sample will be withdrawn. Take sa

49、mples 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 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 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 Place 50 g of the waste to be tested into each pan.Record the