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Updated: Aug 8, 2026

Gas Chromatography-Mass Spectrometry Paired with Total Vaporization Solid-Phase Microextraction as a Forensic Tool
Published on: May 25, 2021
Dynamic headspace: a single-step extraction for isotopic analysis of microg/L concentrations of dissolved chlorinated
Penny L Morrill1, Georges Lacrampe-Couloume, Barbara Sherwood Lollar
1Department of Geology, Stable Isotope Laboratory, University of Toronto, 22 Russell St., Toronto, ON M5S 3B1, Canada.
Abstract:
In this study a dynamic headspace method was developed to measure the carbon isotope values of dissolved chlorinated ethenes at microg/L concentrations. A gas chromatograph/combustion/isotope ratio mass spectrometer (GC/C/IRMS) was modified to include a headspace extraction system followed by a cryogenic trap. Extracting headspace from a 160 mL vial with 80 mL of aqueous solution and 40 g of NaCl for 8-12 min resulted in accurate and reproducible delta13C values for trichloroethene (TCE) and cis-1,2-dichloroethene (cDCE) at concentrations of 50-75 microg/L. Based on these results a conservative lower limit of quantitation of 38 microg/L can be calculated for these compounds. For more volatile compounds such as tetrachloroethene (PCE) and vinyl chloride (VC), field data analyzed using this method indicate a lower limit of quantitation in the tens of microg /L range.

