ASTM D5369 - 93(2008)e1

    Standard Practice for Extraction of Solid Waste Samples for Chemical Analysis Using Soxhlet Extraction

    Active Standard ASTM D5369 | Developed by Subcommittee: D34.01.06

    Book of Standards Volume: 11.04

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    Significance and Use

    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 Matrices

    Sample MatrixSolventCompounds or ConstituentsExtraction Time, h (cycles)Reference
    (1) Sediment1,1,1-trichloro-1,2,2-trifluoroethane (Freon)oil and grease 4 (80) (1)A Plumb (1983)
    (2) Sludges and similar materials1,1,1-trichloro-1,2,2-trifluoroethane (Freon)oil and grease 4 (80) (2) Standard Methods
    (3) Sludges from sewagehexane then methanoltotal organic C oil, grease, fats24 (3) Strachan (1983)
    (4) Municipal wastewater
    suspended solids and activated carbon
    hexane/dichloromethanesemivolatile priority pollutants24 (480) (4) Harrold (1982)
    (5) Soil and housedustacetone/hexane(1:1)organochlorine insecticides 5 (60) (5) EPA (1980)
    (6) Sedimentdichloromethanephenols 8 (6) Goldberg (1980)
    (7) Soila) acetone/n-hexane(1:1)aldrin, dieldrin12 (554) (7) Chiba (1968)
    b) acetonitrilealdrin, dieldrin14 (47)
    c) 2-propanol/n-hexane(1:1)aldrin, dieldrin18 (108)
    (8) Soilchloroform/methanol(1:1) (other
    solvents also studied)
    dieldrin 8 (160) (8) Saha (1969)
    (9) Airborne particulatesmethanol (cyclohexane also studied)gross organics 2 (9) Hill (1977)
    (10) Airborne particulatesbenzeneselected PAHs 46(10) Pierce (1975)
    (11) Airborne particulatesnumerous solvents studiedselected PAHs 6(11) Stanley (1967)
    (12) Coke oven aerosol particulatesbenzeneselected PAHs 2 (1820)(12) Broddin (1977)
    (13) Artificial aerosol particulatesmethanol/benzene
    selected PAHs
    selected phthalates
    selected aliphatics
    8 (80)
    16 (160)
    2 (20)
    (13) Cautreels (1976)
    methanolselected nitrogen aromatics 4 (40)
    benzeneselected nitrogen aromatics 2 (20)
    (14) Activated carbonchloroform
    gross organics
    44 (440)(14) Pahl (1973)
    (15) Buelow (1973)
    (15) Glass fiber filters26 solvents and 24 binary mixturestotal organic carbon 6(16) Grosjean (1975)
    (16) Surface sedimentsmethanol then dichloromethanetotal oil hydrocarbon48 (160)(17) Sporstol (1985)
    (17) Bottom sedimenthexane/acetone/isooctanechlorinated benzenes18(18) Onuska (1985)
    (18) Environmental particulatesbenzenechlorinated dioxins16(19) Lamparski (1980)
    (19) Soilshexane/acetone/methanolDDT12(20) Nash (1972)

    A The boldface numbers in parentheses refer to the list of references at the end of this practice.

    1. Scope

    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.

    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    D75 Practice for Sampling Aggregates

    D420 Guide to Site Characterization for Engineering Design and Construction Purposes

    D2234/D2234M Practice for Collection of a Gross Sample of Coal

    D2910 Method for Removal of Organic Matter from Water by Activated Carbon Absorption

    D3086 Test Method for Organochlorine Pesticides in Water

    D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents

    D3975 Practice for Development and Use (Preparation) of Samples for Collaborative Testing of Methods for Analysis of Sediments

    D3976 Practice for Preparation of Sediment Samples for Chemical Analysis

    D4281 Test Method for Oil and Grease (Fluorocarbon Extractable Substances) by Gravimetric Determination

    D5368 Test Methods for Gravimetric Determination of Total Solvent Extractable Content (TSEC) of Solid Waste Samples

    E122 Practice for Calculating Sample Size to Estimate, With Specified Precision, the Average for a Characteristic of a Lot or Process

    UNSPSC Code

    UNSPSC Code 77100000(Environmental management)

    DOI: 10.1520/D5369-93R08E01

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