Simultaneous determination of chlorinated ethenes and ethene in groundwater using headspace solid-phase microextraction with gas chromatography

Michal Ziv-El, Tomasz Kalinowski, Rosa Krajmalnik-Brown, Rolf Halden

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1 Citation (Scopus)

Abstract

Widespread contamination of groundwater by chlorinated ethenes and their biological dechlorination products necessitates the reliable monitoring of liquid matrices; current methods approved by the U.S. Environmental Protection Agency (EPA) require a minimum of 5 mL of sample volume and cannot simultaneously detect all transformative products. This paper reports on the simultaneous detection of six chlorinated ethenes and ethene itself, using a liquid sample volume of 1 mL by concentrating the compounds onto an 85-μm carboxen-polydimenthylsiloxane solid-phase microextraction fiber in 5 min and subsequent chromatographic analysis in 9.15 min. Linear increases in signal response were obtained over three orders of magnitude (∼0.05 to ∼50 μM) for simultaneous analysis with coefficient of determination (R 2) values of ≥ 0.99. The detection limits of the method (1.3-6 μg/L) were at or below the maximum contaminant levels specified by the EPA. Matrix spike studies with groundwater and mineral medium showed recovery rates between 79-108%. The utility of the method was demonstrated in lab-scale sediment flow-through columns assessing the bioremediation potential of chlorinated ethene-contaminated groundwater. Owing to its low sample volume requirements, good sensitivity and broad target analyte range, the method is suitable for routine compliance monitoring and is particularly attractive for interpreting the bench-scale feasibility studies that are commonly performed during the remedial design stage of groundwater cleanup projects.

Original languageEnglish (US)
Pages (from-to)137-142
Number of pages6
JournalJournal of Chromatographic Science
Volume52
Issue number2
DOIs
StatePublished - 2014

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Gas chromatography
Groundwater
Environmental Protection Agency
Chromatographic analysis
Dechlorination
Bioremediation
Monitoring
Liquids
Minerals
Sediments
Contamination
Impurities
Recovery
ethylene
Fibers

ASJC Scopus subject areas

  • Analytical Chemistry

Cite this

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title = "Simultaneous determination of chlorinated ethenes and ethene in groundwater using headspace solid-phase microextraction with gas chromatography",
abstract = "Widespread contamination of groundwater by chlorinated ethenes and their biological dechlorination products necessitates the reliable monitoring of liquid matrices; current methods approved by the U.S. Environmental Protection Agency (EPA) require a minimum of 5 mL of sample volume and cannot simultaneously detect all transformative products. This paper reports on the simultaneous detection of six chlorinated ethenes and ethene itself, using a liquid sample volume of 1 mL by concentrating the compounds onto an 85-μm carboxen-polydimenthylsiloxane solid-phase microextraction fiber in 5 min and subsequent chromatographic analysis in 9.15 min. Linear increases in signal response were obtained over three orders of magnitude (∼0.05 to ∼50 μM) for simultaneous analysis with coefficient of determination (R 2) values of ≥ 0.99. The detection limits of the method (1.3-6 μg/L) were at or below the maximum contaminant levels specified by the EPA. Matrix spike studies with groundwater and mineral medium showed recovery rates between 79-108{\%}. The utility of the method was demonstrated in lab-scale sediment flow-through columns assessing the bioremediation potential of chlorinated ethene-contaminated groundwater. Owing to its low sample volume requirements, good sensitivity and broad target analyte range, the method is suitable for routine compliance monitoring and is particularly attractive for interpreting the bench-scale feasibility studies that are commonly performed during the remedial design stage of groundwater cleanup projects.",
author = "Michal Ziv-El and Tomasz Kalinowski and Rosa Krajmalnik-Brown and Rolf Halden",
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T1 - Simultaneous determination of chlorinated ethenes and ethene in groundwater using headspace solid-phase microextraction with gas chromatography

AU - Ziv-El, Michal

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AU - Krajmalnik-Brown, Rosa

AU - Halden, Rolf

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AB - Widespread contamination of groundwater by chlorinated ethenes and their biological dechlorination products necessitates the reliable monitoring of liquid matrices; current methods approved by the U.S. Environmental Protection Agency (EPA) require a minimum of 5 mL of sample volume and cannot simultaneously detect all transformative products. This paper reports on the simultaneous detection of six chlorinated ethenes and ethene itself, using a liquid sample volume of 1 mL by concentrating the compounds onto an 85-μm carboxen-polydimenthylsiloxane solid-phase microextraction fiber in 5 min and subsequent chromatographic analysis in 9.15 min. Linear increases in signal response were obtained over three orders of magnitude (∼0.05 to ∼50 μM) for simultaneous analysis with coefficient of determination (R 2) values of ≥ 0.99. The detection limits of the method (1.3-6 μg/L) were at or below the maximum contaminant levels specified by the EPA. Matrix spike studies with groundwater and mineral medium showed recovery rates between 79-108%. The utility of the method was demonstrated in lab-scale sediment flow-through columns assessing the bioremediation potential of chlorinated ethene-contaminated groundwater. Owing to its low sample volume requirements, good sensitivity and broad target analyte range, the method is suitable for routine compliance monitoring and is particularly attractive for interpreting the bench-scale feasibility studies that are commonly performed during the remedial design stage of groundwater cleanup projects.

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