1、Designation: D5233 92 (Reapproved 2017)Standard Test Method forSingle Batch Extraction Method for Wastes1This standard is issued under the fixed designation D5233; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. 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 applicable to the extraction ofsamples of treated or untreated solid wastes or sludges, orsolidified wast
3、e 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 applicati
4、on 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 of t
5、he 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 acceptance c
6、oncentration 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 conditions o
7、f 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 this
8、 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 application o
9、f 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 concerns, if any, associated with its use. It is theresponsibility of th
10、e user of this standard to establish appro-priate safety, health and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For a specific precautionary statement, see Note 8.1.10 This international standard was developed in accor-dance with internationally r
11、ecognized 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 TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D75/D75M Practice
12、 for Sampling AggregatesD420 Guide to Site Characterization for Engineering Designand Construction Purposes (Withdrawn 2011)3D653 Terminology Relating to Soil, Rock, and ContainedFluidsD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2234/D2234M Practice for Collection of a G
13、ross Sampleof CoalD3370 Practices for Sampling Water from Closed ConduitsE122 Practice for Calculating Sample Size to Estimate, WithSpecified Precision, the Average for a Characteristic of aLot or ProcessES 16 Practice for the Generation of Environmental DataRelated to Waste Management Activites43.
14、Terminology3.1 DefinitionsFor definitions of terms used but not de-fined in this test method, see Terminology D1129.1This 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 edit
15、ion approved Sept. 1, 2017. Published September 2017. Originallyapproved in 1992. Last previous edition approved in 2009 as D5233 92 (2009).DOI: 10.1520/D5233-92R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Bo
16、ok 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.4Annual Book of ASTM Standards, Vol 11.04 (see 1991 edition).Copyright ASTM International, 100 Barr Harbor Drive
17、, 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 International Standards, Guides and Recommendations issu
18、ed by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14. Summary of Test Method (See Fig. 1)4.1 For wastes containing 1 % of the original sample weight)TABLE 1 Sample Maximum Holding Times, DaysPeriod CompoundFrom Field Collectionto Method ExtractionFrom the End ofExtractio
19、n to the Start ofFiltration, hFrom Method Extractionto AnalyticalExtractionFrom the AnalyticalExtraction to theChemical AnalysisTotal Time,DaysOrganics 14 2 7 40 61Mercury 28 2 NA 28 56Inorganics except Mercury 180 2 NA 180 360D5233 92 (2017)5has obviously adhered to the container used to transfer t
20、he sample to thefiltration apparatus, determine the weight of this residue and subtract itfrom the sample weight determined in 10.2.5 to determine the weight ofthe waste sample that will be filtered.10.2.7.1 Gradually apply gentle pressure of 1 to 10 psi (7 to70 kPa), until the pressurizing gas move
21、s through the filter. Ifthis point is not reached below 10 psi (69 kPa), and if noadditional liquid has passed through the filter in any 2-mininterval, slowly increase the pressure in 10-psi (69-kPa)increments to a maximum of 50 psi (345 kPa). After eachincremental increase of 10 psi (69 kPa), if th
22、e pressurizing gashas not moved through the filter, and if no additional liquid haspassed the filter in any 2-min interval, proceed to the next10-psi (69-kPa) increment. When the pressurizing gas beginsto move through the filter, or when the liquid flow has ceasedat 50 psi (345 kPa) (that is, filtra
23、tion does not result in anyadditional filtrate within any 2-min period), stop the filtration.NOTE 6Instantaneous application of high pressure can degrade theglass fiber filter and may cause premature plugging.10.2.8 The material in the filter holder is defined as the solidphase of the waste, and the
24、 filtrate is defined as the liquidphase.NOTE 7Some wastes, such as oily and some paint wastes, willobviously contain some material that appears to be liquid. Even afterapplying the pressure filtration as outlined in 10.2.7, this material may notfilter. If this is the case, the material within the fi
25、ltration device is definedas solid. Do not replace the original filter under any circumstances. Useonly one filter.10.2.9 Determine the weight of the liquid phase by subtract-ing the weight of the filtrate container (see 10.2.3) from thetotal weight of the container plus filtrate. Determine the weig
26、htof the solid phase of the waste sample by subtracting theweight of the liquid phase from the weight of the total wastesample, as determined in 10.2.5 or 10.2.7. Record the weight ofthe liquid and solid phases. Calculate the percent solids asfollows:percent solids 5weight of solid 10.2.9!total weig
27、ht of waste 10.2.5 or 10.2.7!3100 (1)10.3 If the percent solids determined in 10.2.9 is 0.5 %,proceed with the filtered solid phase to 10.3.1. If the percentsolids determined in 10.2.9 is 5.0, add 3.5 mL 1 N HCl,slurry briefly, cover with a watch-glass, heat to 50 C, and holdat 50 C for 10 min.FIG.
28、3 Determination of the Extraction FluidD5233 92 (2017)610.4.4 Let the solution cool to room temperature and recordthe pH. If the pH is 5.0, use Extraction Fluid No. 2. Proceed to Section 11.10.5 If the aliquot of the waste used for the preliminaryevaluation (10.2 10.4) was determined to be 100 % sol
29、ids at10.2.1, it can be used for Section 11 extraction (assuming thatat least 100 g remains). The aliquot subjected to the procedurein 10.2.7 might be appropriate for use in Section 11 if anadequate amount of solids (as determined by 10.2.9) wasobtained. The amount of solids necessary is also depend
30、ent onwhether a sufficient amount of extract will be produced tosupport the analyses for the target analytes. If an adequateamount of solids remains, proceed to 11.11.11. Extraction11.1 A sample size of minimally 100 g (solid and liquidphases) is required. A larger sample size may be appropriate ins
31、ome cases, depending on the solid contents of the wastesample (percent solids; see 10.2); whether the initial liquidphase (filtrate) will be miscible with the aqueous extract of thesolid; and whether inorganics, semivolatile organics, pesticidesand herbicides are all analytes of concern. If the amou
32、nt ofextract generated by a single extraction will not be sufficient toperform all of the analyses, more than one extraction may beperformed and the extracts from each combined and aliquotedfor analysis.11.2 If the waste will obviously yield no liquid whensubjected to pressure filtration (that is, i
33、s 100 % solid; 10.2),weigh out a sub-sample of the waste (100 g minimum) andproceed to 11.10.11.3 If the sample is liquid-like or multi-phasic, liquid-solidseparation is required. This involves the filtration devicedescribed in 6.3 and is outlined in 11.4 11.9.11.4 Pre-weigh the container that will
34、receive the filtrate.11.5 Assemble the filter holder and filter following themanufacturers instructions. Place the filter on the supportscreen and secure. Acid wash the filter if inorganics are ofconcern (see 6.4).NOTE 9Acid-washed filters may be used for all extractions, evenwhen inorganics are not
35、 of concern.11.6 Weigh out a sub-sample of waste (100-g minimum)and record the weight. If the waste contains 0.5 % drysolids (10.2 or 10.3), use the percent solids informationobtained in 10.2 to determine the optimum sample size (100 gminimum) for filtration. Sufficient solid should be generated byf
36、iltration to support the analyses to be performed on the methodextract.11.7 Allow slurries to stand to permit the solid phase tosettle. Wastes that settle slowly may be centrifuged prior tofiltration. Use centrifugation only as an aid to filtration. If thewaste is centrifuged, the liquid should be d
37、ecanted and filteredfollowed by filtration of the solid portion of the waste throughthe same filtration system.11.8 Quantitatively transfer the waste sample (liquid andsolid phases) to the filter holder. Spread the waste sampleevenly over the surface of the filter. Allow the sample to warmto room te
38、mperature in the device before filtering.NOTE 10If some waste material (1 % of original sample weight) hasobviously adhered to the container used to transfer the sample to thefiltration apparatus, determine the weight of this residue and subtract itfrom the sample weight determined in 10.2.5 to dete
39、rmine the weight ofthe waste sample that will be filtered.11.8.1 Gradually apply gentle pressure of 1 to 10 psi (7 to70 kPa), until the pressurizing gas moves through the filter. Ifthis point is not reached below 10 psi (69 kPa), and if noadditional liquid has passed through the filter in any 2-mini
40、nterval, slowly increase the pressure in 10-psi (69-kPa)increments to a maximum of 50 psi (345 kPa). After eachincremental increase of 10 psi (69 kPa), if the pressurizing gashas not moved through the filter, and if no additional liquid haspassed the filter in any 2-min interval, proceed to the next
41、10-psi (69-kPa) increment. When the pressurizing gas beginsto move through the filter, or when the liquid flow has ceasedat 50 psi (345 kPa) (that is, filtration does not result in anyadditional filtrate within any 2-min period), stop the filtration.NOTE 11Instantaneous application of high pressure
42、can degrade theglass fiber filter and may cause premature plugging.11.9 The material in the filter holder is defined as the solidphase of the waste, and the filtrate is defined as the liquidphase. Measure the pH of the filtrate. Measure the volume ofthe filtrate (V1) if the data are to be combined m
43、athematically.Use a graduated measuring cylinder for the volume measure-ment. The liquid phase may now be analyzed (see 11.13)orstored at 4 C until the time of analysis.NOTE 12Some wastes, such as oily and some paint wastes, willobviously contain some material that appears to be liquid. Even afterap
44、plying the pressure filtration as outlined in 10.2.7, this material may notfilter. If this is the case, the material within the filtration device is definedas solid. Do not replace the original filter under any circumstances. Useonly one filter.11.10 If the waste contains 0.5 % solids (see 10.2or 10
45、.3), proceed to 11.11.11.11 Quantitatively transfer the solid residue retained bythe filter, or the solid sample if it did not require filtration, intoan extractor bottle. Include the filter if it was used to separatethe initial liquid from the solid phase.11.12 Determine the amount of extraction fl
46、uid to add to theextractor as follows:weight of extraction fluid 520 3percent solids 10.2.9!3weight of waste filter 11.6 or10.2.9!100(3)Slowly add this amount of appropriate extraction fluid (see10.4) to the extractor vessel. Close the extractor bottle tightly(it is recommended that polytetrafluoroe
47、thylene tape be used toensure a tight seal), secure in a rotary agitation device, andD5233 92 (2017)7rotate at 30 6 2 r/min for 18 6 2 h. Ambient temperature (thatis, temperature of the room in which the extraction takes place)shall be maintained at 23 6 2 C during the extraction period.NOTE 13As ag
48、itation continues, pressure may build up within theextractor bottle for some types of wastes (for example, limed or calciumcarbonate-containing waste may evolve gases such as carbon dioxide). Torelieve excess pressure, the extractor bottle may be taken under a hood andopened carefully from time to t
49、ime (for example, after 15 min, 30 min, and1 h).11.13 Within 2 h, following the 18 6 2 h extraction, initiatethe separation of the material in the extraction vessel into itscomponent liquid and solid phases by filtering through a newglass fiber filter, as outlined in 11.8. For final filtration of themethod extract, the glass fiber filter may be changed, ifnecessary, to facilitate filtration. Filter(s) shall be acid washed(see 6.4) if inorganics are of concern.11.14 Prepare the method extract as follows:11.14.1 If the waste contained no initial liquid phase,
