1、Designation: D 5233 92 (Reapproved 2004)Standard Test Method forSingle Batch Extraction Method for Wastes1This standard is issued under the fixed designation D 5233; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、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 applicable to the extraction ofsamples of treated or untreated solid wastes or sludges, orsolidified w
3、aste samples, to provide an indication of theleaching potential.1.2 This test method is intended to provide an extract formeasurement of the concentration of the analytes of concern.The measured values may be compared against set or chosenacceptance levels in some applications.1.3 If the sole applic
4、ation of the test method is such apass/fail comparison and a total analysis of the waste demon-strates that individual analytes are not present in the waste, orthat the chosen acceptance concentration levels could notpossibly be exceeded, the test method need not be run.1.4 If the sole application o
5、f the test method is such apass/fail comparison and an analysis of any one of the liquidfractions of the extract indicates that the concentration of thetarget analyte is so high that, even after accounting for dilutionfrom the other fractions of the extract, it would be equal to orabove an acceptanc
6、e concentration level, then the waste failsthe test. In such a case it may not be necessary to analyze theremaining fractions of the extract.1.5 This test method is intended to provide an extractsuitable for the measurement of the concentration of analytesthat will not volatilize under the condition
7、s of the test method.1.6 Presence of volatile analytes may be established if ananalysis of the extract obtained using this test method detectsthe target volatile analyte. If its concentration is equal to orexceeds an acceptance level for that analyte, the waste fails thetest. However, extract from t
8、his test method shall not be usedto determine the concentration of volatile organic analytes.1.7 This test method is intended to describe only theprocedure for performing a batch extraction. It does notdescribe all of the sampling and analytical requirements thatmay be associated with the applicatio
9、n of this test method.1.8 The values stated in either SI or inch-pound units are tobe regarded as the standard. The values given in parenthesesare for information only.1.9 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of
10、 the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For a specificprecautionary statement, see Note 8.2. Referenced Documents2.1 ASTM Standards:2D 75 Practices for Sampling AggregatesD 420 Practice
11、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 2234 Test Method for Collection of a Gross Sample ofCoalD 3370 Practices for Sampling WaterE 12
12、2 Practice for Choice of Sample Size to Estimate AMeasure of Quality for a Lot or ProcessES 16 Practice for the Generation of Environmental DataRelated to Waste Management Activities33. Terminology3.1 DefinitionsFor definitions of terms used but not de-fined in this test method, see Terminology D 11
13、29.4. Summary of Test Method (See Fig. 1)4.1 For wastes containing less than 0.5 % dry solid material,the filtrate of the waste, after filtration through a 0.6 to 0.8-mglass fiber filter, is defined as the method extract. Extraction ofthe solid is not required for such wastes.4,54.2 For wastes conta
14、ining greater than or equal to 0.5 % drysolid material, the liquid, if any, is separated from the solid1This test method is under the jurisdiction of ASTM Committee D34 on WasteDisposal and is the direct responsibility of Subcommittee D34.01.06 on AnalyticalMethods.Current edition approved March 15,
15、 1992. Published May 1992.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Annual Book of ASTM Standards, Vol
16、 11.04 (see 1991 edition).4Federal Register, Vol 55, No. 61, March 29, 1990. Toxicity CharacteristicsRevisions, Final Rule.5Federal Register, Vol 55, No. 126, June 29, 1990. Toxicity CharacteristicRevisions, Final Rule, Corrections.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, W
17、est Conshohocken, PA 19428-2959, United States.phase and stored for later analysis. The solid phase is extractedwith an amount of extraction fluid equal to 20 times the weightof the solid phase. The extraction fluid used is a function of thealkalinity of the solid phase of the waste. Following extra
18、ction,the liquid extract is separated from the solid phase by filtrationthrough a 0.6 to 0.8-m glass fiber filter.4.3 If compatible (that is, multiple phases will not formupon combination), the initial liquid phase of the waste isadded to the liquid extract, and these are analyzed together. Ifincomp
19、atible, the liquids are analyzed separately and theresults are combined mathematically to yield a volume-weighted average concentration.5. Significance and Use5.1 This test method is intended to generate an extract witha concentration of the target analyte(s) representative of theexpected release un
20、der the scenario simulated, and which canbe compared with concentration levels acceptable in wastedisposal, treatment, or production activities.5.2 The extraction conditions of the test method werechosen to simulate a potential disposal scenario to which thewastes may be exposed.5.3 One intent of th
21、is test method is that the amount of acidin the extraction fluids reflect the acid available from theleachate of a specific landfill where municipal and industrialwastes were co-disposed.65.4 One intent of this test method is to not allow the pH ofthe extraction fluid to be lower than that of the le
22、achate of aspecific landfill where municipal and industrial wastes wereco-disposed. Therefore, the pH of the extraction fluid waschosen with the following considerations:(1) Not to be less than 4.93 6 0.05 for the extraction ofwastes with an acid neutralization capacity of less than the acid6Kimmel,
23、 T. A., and Friedman, D. A., “Model Assumptions and RationaleBehind the Development of EP III,” ASTM STP 886, J. K. Petros, et al, Eds., ASTM,Philadelphia, PA, 1986, pp. 3653.FIG. 1 Method Flow ChartD 5233 92 (2004)2available in the total volume of extraction fluid used in themethod (Extraction Flui
24、d No. 1).(2) At 2.88 6 0.05, as defined by the pH of the acid, for theextraction of wastes with an acid neutralization capacity ofmore than the acid available in the extraction fluid used in themethod (Extraction Fluid No. 2).5.5 The interpretation and use of the results of this testmethod are limit
25、ed by the assumptions of a single co-disposalscenario and by the factors affecting the composition of alandfill leachate and chemical or other differences between aselected extraction fluid and the real landfill leachate.5.6 This test method may be affected by biological changesin the waste, and it
26、is not designed to isolate or measure theeffect of such processes.5.7 This test method produces extracts that are amenable tothe determination of both minor and major constituents. Whenminor constituents are being determined, it is especiallyimportant that precautions be taken in sample storage andh
27、andling to avoid possible contamination of the samples.5.8 The agitation technique, rate, liquid-to-solid ratio, andfiltration conditions specified in the method may not be suitablefor extracting all types of wastes.5.9 This test method is intended to extract the samples intheir original physical st
28、ate as is, without any size reduction.However, the sample/extractor interaction is expected to cor-relate with the environmental conditions to which a waste maybe exposed.75.10 The extraction conditions defined by this test methodare expected to yield steady-state concentrations, determinedby the ex
29、traction liquid-to-solid ratio and the duration of theextraction, which may or may not agree with the concentrationof an equilibrium.6. Apparatus and Materials6.1 Agitation Apparatus, capable of rotating the extractionvessel in an end-over-end fashion (see Fig. 2), at 30 6 2 r/min,such that the axis
30、 of rotation is horizontal and passes throughthe center of the bottle.NOTE 1Similar devices may be used having a different axle arrange-ment if equivalency can be demonstrated.6.2 Extraction VesselSuitable vessels include cylindri-cally shaped, minimum 2-L size, with capacity sufficient tohold the s
31、ample and the extraction fluid. Head-space is allowedin this vessel. The extraction bottles may be constructed fromvarious plastic materials, depending on the analytes of interestand the nature of the waste. Plastic bottles, other than polytet-rafluoroethylene, shall not be used if organics are to b
32、einvestigated. The bottles should be sturdy, in order to withstandthe impact of the falling sample fragments, and shall have aleak-free seal. The use of polytetrafluoroethylene tape isrecommended to ensure a tight seal. Due to their potential forbreakage, the use of glass bottles is not recommended.
33、NOTE 2Suitable bottles range from 4.0 to 4.5 in. (102 to 114 mm) indiameter and from 8.5 to 13.0 in. (216 to 330 mm) in height.6.3 Filtration DeviceIt is recommended that all filtrationsbe performed in a hood. Wastes should be filtered usingpositive-pressure filtration using a pre-purified grade ine
34、rt gassuch as nitrogen.6.3.1 Filter Holder, capable of supporting a glass fiber filterand able to withstand the pressure needed to accomplishseparation (maximum 50 psi or 345 kPa). These devices shallhave a minimum internal volume of 300 mL and shall beequipped to accommodate a minimum filter size o
35、f 47 mm.(Filter holders having an internal capacity of 2.2 L andequipped to accommodate a 142-mm diameter filter are rec-ommended.)6.3.1.1 Materials of ConstructionFiltration devices shallbe made of inert materials that will not leach or adsorb theanalytes of concern. Glass, polytetrafluoroethylene,
36、 or type 316stainless steel equipment may be used when both organic andinorganic analytes are of concern. Devices made of high-density polyethylene (HDPE), polypropylene (PP), or polyvi-nylchloride (PVC) may be used when only inorganics are ofconcern.6.4 Filters, made of borosilicate glass fiber, co
37、ntaining nobinder materials, and having an effective pore size of 0.6 to0.8 m. Pre-filters must not be used. When inorganic analytesare of concern, the filter shall be acid washed prior to use byrinsing with 1 N nitric acid followed by three consecutiverinses with Type II reagent water as defined in
38、 SpecificationD 1193. (A minimum of 1 L per rinse is recommended.) Glassfiber filters are fragile and should be handled with care.6.5 pH Meter, with a readability of 0.01 unit and anaccuracy of 60.05 unit at 25C.6.6 Laboratory Balance, accurate to within 60.01 g. (Allweight measurements are to be wi
39、thin6 0.1 g.)6.7 Beakers or Erlenmeyer Flasks, glass 500-mL, and 2-L.6.8 Watch-Glass, with an appropriate diameter to cover thebeaker or Erlenmeyer flask.6.9 Magnetic Stirrer.6.10 Mold, cylindrical, made of inert, non-adsorbing andnon-contaminating material for casting of laboratory samples.6.11 Str
40、aightedge, made of stainless steel.6.12 Impermeable Sheet or Glazed Paper.6.13 Volumetric Flask, 1-L size.6.14 Drying OvenAny thermostatically controlled dryingoven capable of maintaining a temperature between 85 and115C within 65C.7Federal Register, Vol 53, No. 100, May 24, 1988. Proposed Cage Modi
41、ficationof TCLP.FIG. 2 Rotary Agitation ApparatusD 5233 92 (2004)36.15 Graduated Pipet, readable to 0.1 mL.6.16 Hot Plate, equipped for agitation and temperaturecontrol capable of maintaining a 50 6 3C temperature.6.17 Graduated Measuring Cylinder, with a precision of63%.7. Reagents7.1 Purity of Rea
42、gentsReagent grade chemicals shall beused in all tests. Unless 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.8Other grades may beused, provided
43、 it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterReagent water is defined as water inwhich an interfering analyte is not observed at or above themethod detection limit of the analyte(s) of
44、interest. Type II ofSpecification D 1193 or equivalent meets the definition ofreagent water.7.3 Hydrochloric Acid (HCl), 1 N, made from ACS reagentgrade.7.4 Nitric Acid (HNO3), 1 N, made from ACS reagentgrade.7.5 Sodium Hydroxide (NaOH), 1 N, made from ACSreagent grade.7.6 Glacial Acetic Acid (CH3CO
45、OH), ACS reagent grade.7.7 Extraction FluidsSeveral batches or multiple volumesof extraction fluids should be prepared in accordance with thenumber of extractions. The volume needed for an individualextraction is approximately 2 L. The extraction fluids should bemonitored frequently for impurities.
46、The pH should be exam-ined prior to extraction to ensure that these fluids were made upaccurately. If impurities are found or the pH is not within thespecifications, the fluid shall be discarded and fresh extractionfluid prepared.7.7.1 Extraction Fluid No. 1Add 5.7 mL glacial aceticacid to 500 mL of
47、 reagent water, add 64.3 mL of 1 N NaOH,and dilute to a volume of 1 L. When correctly prepared, the pHof this fluid will be 4.93 6 0.05.7.7.2 Extraction Fluid No. 2Dilute 5.7 mL glacial aceticacid with reagent water to a volume of 1 L. When correctlyprepared, the pH of this fluid will be 2.88 6 0.05
48、.8. Sampling8.1 If representative samples of the waste must be tested,use ASTM Sampling methods developed for the specificindustry where available (see Practices D 75, D 420, D 3370,Terminology D 653, and Method D 2234).8.2 All samples shall be collected using an appropriatesampling plan to ensure s
49、ample integrity and representative-ness (see Practice E 122).8.3 Where no specific methods are available, samplingmethodology for materials of similar physical form shall beused.8.4 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 extraction characteristics of thesample. Waste samples should contain a representative distri-bution of particle sizes.NOTE 3Information on obtaining representative samples can also befound in Pierre Gys Sampling Theory and Practice.98.5
