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

Standard No.

ASTM D7363-13a

Release Date

2013

Published By

American Society for Testing and Materials (ASTM)

Latest

ASTM D7363-13a

Scope

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.

1.1 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 318201;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 (ΣTU_c) 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 958201;% 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 det......

ASTM D7363-13a Referenced Document

• ASTM D1192 Standard Guide for Equipment for Sampling Water and Steam in Closed Conduits
• ASTM D1193 Standard Specification for Reagent Water
• ASTM D2777 Standard Practice for Determination of Precision and Bias of Applicable Methods of Committee D-19 on Water
• ASTM D3370 Standard Practices for Sampling Water from Closed Conduits
• ASTM E178 Standard Practice for Dealing With Outlying Observations

ASTM D7363-13a history

• 2013 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
• 2021 ASTM D7363-13A(2021)e1 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 Monito
• 2013 ASTM D7363-13 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
• 2011 ASTM D7363-11 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
• 2007 ASTM D7363-07 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 Monito