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Analysis of t-Butyldimethylsilyl Derivatives of Chlorophenols in the Atmosphere of Urban and Rural Areas in East of France
Authors:C. Schummer  M. Sadiki  P. Mirabel  M. Millet
Affiliation:(1) Centre de Géochimie de la Surface, UMR 7517, CNRS – Université Louis Pasteur, Laboratoire de Physico-Chimie de l′Atmosphère, 1, rue Blessig, 67084 Strasbourg Cedex, France
Abstract:A method using GC-MS and derivatization with N-(t-butyldimethylsilyl)-N-ethyltrifluoroacetamide (MTBSTFA) was developed for the analysis of 19 chlorophenols compounds in atmospheric samples (gas and particles). Air sampling was carried out using a Hi-Vol sampler with glass fibre filter and XAD-2 resin at a flow rate of 60 m3 h?1. The particle and gas phases were collected separately over a period of 4 h. Samples were Soxhlet extracted, evaporated to dryness under nitrogen and refilled with acetonitrile. 100 mL of these extracts were derivatized with 100 μL of MTBSTFA at 80 °C for 1 h under strong stirring. Sylylated chlorophenols were injected into a GC-MS in splitless mode and quantified as their TBDMS derivatives in the SIM mode. Mass spectral analysis of the derivatives of the 19 compounds studied indicates that the spectra are highly specific showing an ion at [M - 57]+ which is useful for structure confirmation or analysis at low levels using selected ion monitoring. Quantification limits varied between 5 µg L?1 and 10 µg L?1 which correspond to 20 pg m?3 and 40 pg m?3 for 250 m3 of air sampled. This method was successfully applied to atmospheric samples collected simultaneously in winter 2004 in an urban (Strasbourg) and rural (Erstein) areas in east of France.
Keywords:Gas chromatography –   mass spectrometry  Sylilation  Chlorophenols in the atmosphere
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