1、Designation: D 5369 93 (Reapproved 2003)Standard Practice forExtraction of Solid Waste Samples for Chemical AnalysisUsing Soxhlet Extraction1This standard is issued under the fixed designation D 5369; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、case of revision, the year of 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 practice describes standard procedures for extract-ing nonvolatile and semivolatil
3、e organic compounds fromsolids such as soils, sediments, sludges, and granular wastesusing Soxhlet extraction.1.1.1 The sample must be suitable for being mixed with thesample drying agent, sodium sulfate or magnesium sulfate, toprovide drying of all sample surfaces.1.2 This practice, when used in co
4、njunction with TestMethod D 5368 is applicable to the determination of the totalsolvent extractable content (TSEC) of a soil, sediment, sludge,or granular solid waste and depends upon the solvent chosenfor extraction.1.3 This practice is limited to solvents having boiling pointsbelow the boiling poi
5、nt of water at ambient pressure.1.4 The solvent extract obtained by this practice may beanalyzed for total or specific nonvolatile and semivolatileorganic compounds but may require sample clean-up proce-dures prior to specific compound analysis.1.4.1 This practice provides sample extracts suitable f
6、oranalysis by various techniques such as gas chromatographywith flame ionization detection (GC/FID) or gas chromatogra-phy with mass spectrometric detection (GC/MS).1.5 This practice is recommended only for solid samplesthat can pass through a 10-mesh sieve (approximately 2-mmopenings), or are less
7、than 2 mm in thickness.1.6 This standard 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
8、 to use. For specificprecautions see Section 9.2. Referenced Documents2.1 ASTM Standards:2D75 Practices for Sampling AggregatesD 420 Practice for Investigating and Sampling Soil andRock for Engineering PurposesD 2234 Test Method for Collection of a Gross Sample ofCoalD 2910 Practice for Concentratio
9、n and Recovery of OrganicMatter from Water by Activated CarbonD 3086 Test Method for Organochlorine Pesticides in WaterD 3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD 3975 Practice for Preparation of Samples for Collabora-tive Testing of Methods for
10、 Analysis of SedimentsD 3976 Practice for Preparation of Sediment Samples forChemical AnalysisD 4281 Test Method for Oil and Grease (FluorocarbonExtractable Substances) by Gravimetric DeterminationD 5368 Test Method for the Gravimetric Determination ofTotal Solvent Extractable Content (TSEC) of Soli
11、d WasteSamplesE 122 Practice for Choice of Sample Size to Estimate aMeasure of Quality for a Lot or Process2.2 EPA Document:SW 846 Method 3540 Soxhlet Extraction, Test Methods forEvaluating Solid Waste, Physical/Chemical Methods SW846, Third Edition33. Terminology3.1 Definitions:3.1.1 GCgas chromato
12、graphy.3.1.2 GC/MSgas chromatography with mass spectromet-ric detection.1This practice is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved March 15, 1993. Published May 1993.2For r
13、eferenced 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.3Available from the Superintendent of Documents, U.S. Government Pr
14、intingOffice, Washington, D.C. 20402.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.3 TSECtotal solvent extractable content. The totalconcentration by weight (w/w) of organic materials that areextractable from a soil or solid wa
15、ste by the selected solvent.4. Summary of Practice4.1 The sample is mixed with sodium sulfate or magnesiumsulfate, placed in an extraction thimble, and extracted using anappropriate solvent in a Soxhlet extractor for a 15 to 20-hperiod. For additional information, see Test Method D 4281.The time req
16、uired may be longer or shorter than the statedperiod, provided the extraction time selected has been demon-strated appropriate for the compounds and matrix of interest.4.2 The solvent extract may be further processed usingsample clean-up techniques and may be analyzed using instru-mental methods for
17、 specific nonvolatile or semivolatile organiccompounds. This practice does not include sample extractclean-up methods.5. Significance and Use5.1 This practice provides a general procedure for thesolvent extraction of organics from soils, sediments, sludges,and fine-grained solid wastes. It may be us
18、ed as the initial stepin the solvent extraction of organic constituents from wastematerials for the purpose of quantifying extractable organiccompounds. When the appropriate extraction solvent is used,the procedure can be applied to the determination of the totalsolvent extractable content (TSEC) of
19、 the sample. The extrac-tion of nonvolatile or semivolatile organic compounds from theabove solid waste should use solvents listed in Table 1 orSW846 Method 3540.5.2 The detection limit, linear concentration range, andsensitivity of the method for specific organic compoundanalysis will depend upon t
20、he method used for instrumentalanalysis and will also depend upon the sample clean-up andsolvent concentration methods used. Typical detection limitsthat can be achieved for GC or GC/MS are in the parts permillion and sub-parts per million range.5.2.1 The method detection limit can be adjusted by va
21、ryingthe volume of extract used and by additional sample clean-upprior to analysis.5.3 Soxhlet extraction has an advantage when analyzingsolid waste and soil/waste mixtures which form emulsions withmore rigorous solvent mixing extraction techniques.6. Interferences6.1 Solvents, reagents, glassware,
22、and other sample process-ing hardware may yield discrete artifacts or elevated baselineswhich cause misinterpretation of follow-up analyses. All ofthese materials must be demonstrated to be free of interferenceunder the conditions of the follow-up analysis. Specific selec-tion of reagents or the pur
23、ification of solvents by distillation inall glass systems, or both, are required when organic compo-nent analysis follows extraction.6.1.1 Glassware should be cleaned by washing with deter-gent or non-chromate cleaning solution, rinsing first with tapwater, then reagent water, then redistilled aceto
24、ne, and finallywith pesticide quality solvent (that is, the solvent used forextraction). If the type and size of glassware permits, it may becleaned by heating in a muffle furnace at 400C for 15 to 30min. Alternatively, glassware may be oven dried at 103C forTABLE 1 Selected Applications of Soxhlet
25、Extraction for Extraction of Organic Constituents from Solid MatricesSample Matrix Solvent Compounds or ConstituentsExtraction Time, h(cycles)Reference(1) Sediment 1,1,1-trichloro-1,2,2-trifluoroethane(Freon)oil and grease 4 (80) (1)APlumb (1983)(2) Sludges and similar materials 1,1,1-trichloro-1,2,
26、2-trifluoroethane(Freon)oil and grease 4 (80) (2) Standard Methods(3) Sludges from sewage hexane then methanol total organic C oil, grease, fats 24 (3) Strachan (1983)(4) Municipal wastewatersuspended solids and activatedcarbonhexane/dichloromethane semivolatile priority pollutants 24 (480) (4) Harr
27、old (1982)(5) Soil and housedust acetone/hexane(1:1) organochlorine insecticides 5 (60) (5) EPA (1980)(6) Sediment dichloromethane phenols 8 (6) Goldberg (1980)(7) Soil a) acetone/n-hexane(1:1) aldrin, dieldrin 12 (554) (7) Chiba (1968)b) acetonitrile aldrin, dieldrin 14 (47)c) 2-propanol/n-hexane(1
28、:1) aldrin, dieldrin 18 (108)(8) Soil chloroform/methanol(1:1) (othersolvents also studied)dieldrin 8 (160) (8) Saha (1969)(9) Airborne particulates methanol (cyclohexane also studied) gross organics 2 (9) Hill (1977)(10) Airborne particulates benzene selected PAHs 46 (10) Pierce (1975)(11) Airborne
29、 particulates numerous solvents studied selected PAHs 6 (11) Stanley (1967)(12) Coke oven aerosol particulates benzene selected PAHs 2 (1820) (12) Broddin (1977)(13) Artificial aerosol particulates methanol/benzenemethanol/benzenemethanol/benzeneselected PAHsselected phthalatesselected aliphatics8 (
30、80)16 (160)2 (20)(13) Cautreels (1976)methanol selected nitrogen aromatics 4 (40)benzene selected nitrogen aromatics 2 (20)(14) Activated carbon chloroformchloroform/ethanolphenolsgross organics44 (440) (14) Pahl (1973)(15) Buelow (1973)(15) Glass fiber filters 26 solvents and 24 binary mixtures tot
31、al organic carbon 6 (16) Grosjean (1975)(16) Surface sediments methanol then dichloromethane total oil hydrocarbon 48 (160) (17) Sporstol (1985)(17) Bottom sediment hexane/acetone/isooctane chlorinated benzenes 18 (18) Onuska (1985)(18) Environmental particulates benzene chlorinated dioxins 16 (19)
32、Lamparski (1980)(19) Soils hexane/acetone/methanol DDT 12 (20) Nash (1972)AThe boldface numbers in parentheses refer to the list of references at the end of this practice.D 5369 93 (2003)2at least 1 h, after solvent rinsing and draining. Volumetricglassware should not be heated in a muffle furnace.6
33、.1.2 Plastics, except PTFE-fluorocarbon, can be a source ofserious interference, especially when specific organic constitu-ents are of analytical interest. Their use must be avoided.Samples should be collected in glass bottles with PTFE-fluorocarbon-lined caps. Alternatively, caps may be lined withp
34、recleaned aluminum foil when the pH of the sample is nearneutral and the salt content of the sample is low. To minimizethe possibility of contamination of containers after cleaning,these items should be cleaned immediately prior to use andcapped. A glassware rinse should be performed with theextract
35、ion solvent immediately prior to use.6.2 A blank Soxhlet extraction and analysis should beperformed in order to determine the solvent, drying agent, andapparatus background. If necessary, the glass (or paper)thimble and glass wool should be leached with solvent prior touse in order to minimize conta
36、mination. Method blanks shouldbe less than 20 % of the concentration of the minimum neededreportable concentration. A method blank(s) must be reportedwith method data.6.3 A relatively high TSEC background (20 % of theminimum TSEC of interest) can result from solubility ofsodium sulfate or other dryi
37、ng agent in the extraction solvent.This will preclude the application of the method for TSECdeterminations.6.4 Impurities in the extracting solvent can be a source ofinterference or TSEC background. Solvent blanks should beanalyzed with each new bottle of solvent. Whenever a highTSEC background, or
38、interfering compounds, are traced to thesolvent, a new source of solvent should be obtained. Alterna-tively, impurities can often be removed by distillation in glass.6.5 If organic compound interferences are found in theanhydrous sodium sulfate or magnesium sulfate, the dryingagent may be rinsed wit
39、h pure extraction solvent, or alterna-tively, Soxhlet extracted, followed by oven drying.6.6 Inorganic constituents extractable from the waste by theextraction solvent will result in a positive interference in thedetermination of TSEC. This potential for interference must bedetermined by the analyst
40、 on a case-by-case basis.6.7 When specific organic compound analysis is of interest,matrix interferences may be caused by compounds that arecoextracted from the sample (but are not of interest). Theextent of such matrix interferences will vary considerablydepending on the sample and the specific ins
41、trumental analysismethod used. Matrix interferences may be reduced by ajudicious choice of extracting solvent, or alternatively, by usinga clean-up technique on the extract following Soxhlet extrac-tion.7. Selection of the Extraction Solvent7.1 The selection of solvent for extraction will depend upo
42、nmany factors, including the following (see Table 1 for selectedapplications):7.1.1 Boiling point of the solvent.7.1.2 Boiling point of the compounds or class of compoundsof interest.7.1.3 Tendency of the solvent and matrix to form emulsions.7.1.4 Solvent strength (that is, polarity, solubility of c
43、om-pounds of interest).7.1.5 Safety of solvent use (that is, toxicity, flammability).7.1.6 Purity of solvent.7.1.7 Solvent compatibility with analytical instrumentation.7.2 The analyst should demonstrate a recovery using aspiking procedure in the matrix of interest before using thisprocedure.7.3 Bec
44、ause the extraction is carried out at temperaturesapproaching the boiling point of the solvent for the entireextraction period, the analyst must ensure that heat-labile andmore volatile solutes that may be of interest are stable andrecoverable by the method. Low-boiling fractions can also belost in
45、the solvent evaporation steps where Kuderna-Danishsolvent concentration is performed or where TSEC is deter-mined gravimetrically after solvent evaporation.7.4 The rate and extraction efficiency of the Soxhlet extrac-tion process are not only a function of the solubility of theconstituents of intere
46、st in solvent versus the matrix, but are alsorelated to the dissolution process. This depends upon the easeof penetration of the solvent into the solid sample matrix. Fineparticles are extracted more easily than large particles becauseof the increased surface area they provide. Therefore theparticle
47、 nature of the sample must be evaluated and docu-mented.7.5 In many cases where the extraction efficiency of theconstituent of interest during the extraction period is less than100 %, the efficiency of the solvent extraction process is highlydependent upon the control of conditions during the Soxhle
48、textraction process. Extraction efficiency will depend upon thecombined effect of the specific solvent used, the temperature atwhich extraction occurs, the cycle time for the Soxhlet appa-ratus, and the total extraction time. Therefore the rate andduration of extraction must be closely controlled.8.
49、 Apparatus8.1 Soxhlet extraction apparatus consisting of Soxhlet ex-tractor, Allihn condenser, and 500-mL round-bottom boilingflask.8.1.1 Allihn Condenser, bottom standard taper joint 45/50.8.1.2 Boiling Flask, flat bottom, standard taper joint 24/40.8.1.3 Soxhlet Extractor, 85-mL, top standard taper joint45/50, bottom standard taper joint 24/40.8.2 Glass or Paper Thimble or Glass Wool to retain samplein Soxhlet extraction device. It should drain freely and mayrequire cleaning before use. To clean the thimbles, pre-extractthem with the solvent to be used for sample extraction.8.
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