【国外标准】 Standard Practice for Extraction of Solid Waste Samples for Chemical Analysis Using Soxhlet Extraction (Withdrawn 2016)

This practice provides a general procedure for the solvent extraction of organics from soils, sediments, sludges, and fine-grained solid wastes. It may be used as the initial step in the solvent extraction of organic constituents from waste materials for the purpose of quantifying extractable organic compounds. When the appropriate extraction solvent is used, the procedure can be applied to the determination of the total solvent extractable content (TSEC) of the sample. The extraction of nonvolatile or semivolatile organic compounds from the above solid waste should use solvents listed in Table 1 or SW846 Method 3540.The detection limit, linear concentration range, and sensitivity of the method for specific organic compound analysis will depend upon the method used for instrumental analysis and will also depend upon the sample clean-up and solvent concentration methods used. Typical detection limits that can be achieved for GC or GC/MS are in the parts per million and sub-parts per million range.The method detection limit can be adjusted by varying the volume of extract used and by additional sample clean-up prior to analysis.Soxhlet extraction has an advantage when analyzing solid waste and soil/waste mixtures which form emulsions with more rigorous solvent mixing extraction techniques.TABLE 1 Selected Applications of Soxhlet Extraction for Extraction of Organic Constituents from Solid MatricesSample Matrix Solvent Compounds or Constituents Extraction Time, h (cycles) Reference(1) Sediment 1,1,1-trichloro-1,2,2-trifluoroethane (Freon) oil and grease 4 (80) (1)A Plumb (1983)(2) Sludges and similar materials 1,1,1-trichloro-1,2,2-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 activated carbon hexane/dichloromethane semivolatile priority pollutants 24 (480) (4) Harrold (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(1:1) 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 4–6 (10) Pierce (1975)(11) Airborne particulates numerous solvents studied selected PAHs 6 (11) Stanley (1967)(12) Coke oven aerosol particulates benzene selected PAHs 2 (18–20) (12) Broddin (1977)(13) Artificial aerosol particulates methanol/benzenemethanol/benzenemethanol/benzene selected PAHsselected phthalatesselected aliphatics 8 (80)16 (160)2 (20) (13) Cautreels (1976) methanol selected nitrogen aromatics 4 (40) benzene selected nitrogen aromatics 2 (20) (14) Activated carbon chloroformchloroform/ethanol phenolsgross organics 44 (440) (14) Pahl (1973)(15) Buelow (1973)(15) Glass fiber filters 26 solvents and 24 binary mixtures total 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) Lamparski (1980)(19) Soils hexane/acetone/methanol DDT 12 (20) Nash (1972)A The boldface numbers in parentheses refer to the list of references at the end of this practice.1.1 This practice describes standard procedures for extracting nonvolatile and semivolatile organic compounds from solids such as soils, sediments, sludges, and granular wastes using Soxhlet extraction.1.1.1 The sample must be suitable for being mixed with the sample drying agent, sodium sulfate or magnesium sulfate, to provide drying of all sample surfaces.1.2 This practice, when used in conjunction with Test Method D 5368 is applicable to the determination of the total solvent extractable content (TSEC) of a soil, sediment, sludge, or granular solid waste and depends upon the solvent chosen for extraction.1.3 This practice is limited to solvents having boiling points below the boiling point of water at ambient pressure.1.4 The solvent extract obtained by this practice may be analyzed for total or specific nonvolatile and semivolatile organic compounds but may require sample clean-up procedures prior to specific compound analysis.1.4.1 This practice provides sample extracts suitable for analysis by various techniques such as gas chromatography with flame ionization detection (GC/FID) or gas chromatography with mass spectrometric detection (GC/MS).1.5 This practice is recommended only for solid samples that can pass through a 10-mesh sieve (approximately 2-mm openings), or are less than 2 mm in thickness.1.6 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautions see Section 9.