ASTM D7363 - 13a

    Standard Test Method for Determination of Parent and Alkyl Polycyclic Aromatics in Sediment Pore Water Using Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry in Selected Ion Monitoring Mode

    Active Standard ASTM D7363 | Developed by Subcommittee: D19.06

    Book of Standards Volume: 11.02


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    ASTM D7363

    Significance and Use

    5.1 This method directly determines the concentrations of dissolved PAH concentrations in environmental sediment pore water samples. The method is important from an environmental regulatory perspective because it can achieve the analytical sensitivities to meet the goals of the USEPA narcosis model for protecting benthic organisms in PAH contaminated sediments. Regulatory methods using solvent extraction have not achieved the wide calibration ranges from nanograms to milligrams per litre and the required levels of detection in the nanogram-per-litre range. In addition, conventional solvent extraction methods require large aliquot volumes (litre or larger), use of large volumes of organic solvents, and filtration to generate the pore water. This approach entails the storage and processing of large volumes of sediment samples and loss of low molecular weight PAHs in the filtration and solvent evaporation steps.

    5.2 This method can be used to determine nanogram to milligram per litre PAH concentrations in pore water. Small volumes of pore water are required for SPME extraction, only 1.5 mL per determination and virtually no solvent extraction waste is generated.

    1. Scope

    1.1 The U.S. Environmental Protection Agency (USEPA) narcosis model for benthic organisms in sediments contaminated with polycyclic aromatic hydrocarbons (PAHs) is based on the concentrations of dissolved PAHs in the interstitial water or “pore water” in sediment. This test method covers the separation of pore water from PAH-impacted sediment samples, the removal of colloids, and the subsequent measurement of dissolved concentrations of the required 10 parent PAHs and 14 groups of alkylated daughter PAHs in the pore water samples. The “24 PAHs” are determined using solid-phase microextraction (SPME) followed by Gas Chromatography/Mass Spectrometry (GC/MS) analysis in selected ion monitoring (SIM) mode. Isotopically labeled analogs of the target compounds are introduced prior to the extraction, and are used as quantification references.

    1.2 Lower molecular weight PAHs are more water soluble than higher molecular weight PAHs. Therefore, USEPA-regulated PAH concentrations in pore water samples vary widely due to differing saturation water solubilities that range from 0.2 µg/L for indeno[1,2,3-cd]pyrene to 31 000 µg/L for naphthalene. This method can accommodate the measurement of microgram per litre concentrations for low molecular weight PAHs and nanogram per litre concentrations for high molecular weight PAHs.

    1.3 The USEPA narcosis model predicts toxicity to benthic organisms if the sum of the toxic units (ΣTUc) calculated for all “34 PAHs” measured in a pore water sample is greater than or equal to 1. For this reason, the performance limit required for the individual PAH measurements was defined as the concentration of an individual PAH that would yield 1/34 of a toxic unit (TU). However, the focus of this method is the 10 parent PAHs and 14 groups of alkylated PAHs (Table 1) that contribute 95 % of the toxic units based on the analysis of 120 background and impacted sediment pore water samples.3 The primary reasons for eliminating the rest of the 5-6 ring parent PAHs are: (1) these PAHs contribute insignificantly to the pore water TU, and (2) these PAHs exhibit extremely low saturation solubilities that will make the detection of these compounds difficult in pore water. This method can achieve the required detection limits, which range from approximately 0.01 µg/L, for high molecular weight PAHs, to approximately 3 µg/L for low molecular weight PAHs.

    TABLE 1 Target PAHs, Toxic Unit Factors and Performance LimitsA

    Analyte

    Added d-PAH
    Internal
    Standard

    d-PAH Internal
    Std. for Calculation

    Conc. for One
    Toxic Unit,
    Ctu, (ng/mL)

    Performance Limit
    (ng/mL)

    Basis for
    Performance
    LimitB

    Naphthalene

    A

    A

    193.47

    5.69

    B

    2-Methylnaphthalene

     

    B

    81.69

    2.40

    B

    1-Methylnaphthalene

    B

    B

    81.69

    2.40

    B

    C2-Naphthalenes

     

    A

    30.24

    0.89

    B

    C3-Naphthalenes

     

    A

    11.10

    0.33

    B

    C4-Naphthalenes

     

    A

    4.05

    0.12

    C

    Acenaphthylene

     

    C

    308.85

    9.03

    B

    Acenaphthene

    C

    C

    55.85

    1.64

    B

    Fluorene

    D

    D

    39.30

    1.16

    B

    C1-Fluorenes

     

    D

    13.99

    0.41

    B

    C2-Fluorenes

     

    D

    5.30

    0.16

    B

    C3-Fluorenes

     

    D

    1.92

    0.06

    S

    Phenanthrene

    E

    E

    19.13

    0.56

    B

    Anthracene

     

    E

    20.72

    0.61

    B

    C1-Phenanthrenes/Anthracenes

     

    E

    7.44

    0.22

    B

    C2-Phenanthrenes/Anthracenes

     

    E

    3.20

    0.09

    B

    C3-Phenanthrenes/Anthracenes

     

    E

    1.26

    0.04

    B

    C4-Phenanthrenes/Anthracenes

     

    E

    0.56

    0.02

    S

    Fluoranthene

     

    F

    7.11

    0.21

    B

    Pyrene

    F

    F

    10.11

    0.30

    B

    C1-Fluoranthenes/Pyrenes

     

    F

    4.89

    0.14

    C

    Benz[a]anthracene

     

    G

    2.23

    0.066

    B

    Chrysene

    G

    G

    2.04

    0.060

    B

    C1-Chrysenes/Benz[a]anthracenes

     

    G

    0.86

    0.025

    C

    A From Hawthorne, S. B., Grabanski, C. B., Miller, D. J., and Kreitinger, J. P., “Solid Phase Microextraction Measurement of Parent and Alkyl Polycyclic Aromatic Hydrocarbons in Milliliter Sediment Pore Water Samples and Determination of KDOC Values,” Environmental Science Technology, Vol 39, 2005, pp. 2795–2803.
    B Performance limits were determined as 3 times the background concentrations from the SPME fiber based on the analysis of water blanks (“B”), the lowest calibration standard which consistently yielded a signal to noise ratio of at least 3:1 (“C”), or (for when no calibration standard was available) for the lowest concentrations consistently found in pore water samples with a signal to noise ratio of at least 3:1 (“S”). Detection limits for alkyl PAHs are based on a single isomer.

    1.4 The test method may also be applied to the determination of additional PAH compounds (for example, 5- and 6-ring PAHs as described in Hawthorne et al.).4 However, it is the responsibility of the user of this standard to establish the validity of the test method for the determination of PAHs other than those referenced in 1.1 and Table 1.

    1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

    1.6 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, refer to 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

    D1192 Guide for Equipment for Sampling Water and Steam in Closed Conduits

    D1193 Specification for Reagent Water

    D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water

    D3370 Practices for Sampling Water from Closed Conduits

    E178 Practice for Dealing With Outlying Observations


    ICS Code

    ICS Number Code 13.080.10 (Chemical characteristics of soil)

    UNSPSC Code

    UNSPSC Code


    DOI: 10.1520/D7363

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