ASTM D6520 - 06(2012)

    Standard Practice for the Solid Phase Micro Extraction (SPME) of Water and its Headspace for the Analysis of Volatile and Semi-Volatile Organic Compounds

    Active Standard ASTM D6520 | Developed by Subcommittee: D19.06

    Book of Standards Volume: 11.02


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    Significance and Use

    This practice provides a general procedure for the solid-phase microextraction of volatile and semi-volatile organic compounds from an aqueous matrix or its headspace. Solid sorbent extraction is used as the initial step in the extraction of organic constituents for the purpose of quantifying or screening for extractable organic compounds.

    Typical detection limits that can be achieved using SPME techniques with gas chromatography with flame ionization detector (FID), electron capture detector (ECD), or with a mass spectrometer (MS) range from mg/L to μg/L. The detection limit, linear concentration range, and sensitivity of the test method for a specific organic compound will depend upon the aqueous matrix, the fiber phase, the sample temperature, sample volume, sample mixing, and the determinative technique employed.

    SPME has the advantages of speed, no desorption solvent, simple extraction device, and the use of small amounts of sample.

    Extraction devices vary from a manual SPME fiber holder to automated commercial device specifically designed for SPME.

    Listed below are examples of organic compounds that can be determined by this practice. This list includes both high and low boiling compounds. The numbers in parentheses refer to references at the end of this standard.

    Volatile Organic Compounds (1,2,3)
    Pesticides, General (4,5)
    Organochlorine Pesticides (6)
    Organophosphorous Pesticides (7,8)
    Polyaromatic Hydrocarbons (9,10)
    Polychlorinated biphenyls (10)
    Phenols (11)
    Nitrophenols (12)
    Amines (13)

    SPME may be used to screen water samples prior to purge and trap extraction to determine if dilution is necessary, thereby eliminating the possibility of trap overload.

    1. Scope

    1.1 This practice covers procedures for the extraction of volatile and semi-volatile organic compounds from water and its headspace using solid-phase microextraction (SPME).

    1.2 The compounds of interest must have a greater affinity for the SPME-absorbent polymer or adsorbent or combinations of these than the water or headspace phase in which they reside.

    1.3 Not all of the analytes that can be determined by SPME are addressed in this practice. The applicability of the absorbent polymer, adsorbent, or combination thereof, to extract the compound(s) of interest must be demonstrated before use.

    1.4 This practice provides sample extracts suitable for quantitative or qualitative analysis by gas chromatography (GC) or gas chromatography-mass spectrometry (GC-MS).

    1.5 Where used, it is the responsibility of the user to validate the application of SPME to the analysis of interest.

    1.6 The values stated in SI units are to be regarded as the standard.

    1.7 This standard does not purport to address all of the safety concerns, 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 hazard statements, see Section 10.


    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

    D1129 Terminology Relating to Water

    D1193 Specification for Reagent Water

    D3370 Practices for Sampling Water from Closed Conduits

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

    D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water

    D4210 Practice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data

    D4448 Guide for Sampling Ground-Water Monitoring Wells


    ICS Code

    ICS Number Code 13.060.50 (Examination of water for chemical substances)

    UNSPSC Code

    UNSPSC Code


    DOI: 10.1520/D6520-06R12

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