The simultaneous determination of several odorous trichlorobromophenols in water has been carried out by an in-sample derivatization headspace solid-phase microextraction method (HS-SPME). The analytical procedure involved their derivatization to methyl ethers with dimethyl sulfate/NaOH and further HS-SPME and gas chromatography-mass spectrometry (GC/MS) determination. Parameters affecting both the derivatization efficiency and headspace SPME procedures, such as the selection of the SPME fiber coating, derivatization-extraction time and temperature, were studied. The commercially available polydimethylsiloxane (PDMS) 100 microm and Carboxen-polydimethylsiloxane-divinylbenzene (CAR-PDMS-DVB) fibers appeared to be the most suitable for the simultaneous determination of these compounds. The precision of the HS-SPME/GC/MS method gave good relative standard deviations (RSDs) run-to-run between 9% and 19% for most of them, except for 2,5-diCl-6-Br-phenol, 2,6-diCl-3-Br-phenol and-2,3,6-triBr-phenol (22%, 25% and 23%, respectively). The method was linear over two orders of magnitude, and detection limits were compound dependent but ranged from 0.22 ng/l to 0.95 ng/l. The results obtained for water samples using the proposed SPME procedure were compared with those found with the EPA 625 method, and good agreement was achieved. Therefore, the in-sample derivatization HS-SPME/GC/MS procedure here proposed is a suitable method for the simultaneous determination of odorous trichlorobromophenols in water.
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