Optimisation of a Headspace Solid-Phase Micro- Extraction Procedure for the Determination of 2,4,6-Trichloroanisole and Various Related Compounds in Cork Washing Waste Water by Use of Gas Chromatography-Mass Spectrometry

A method for the determination of 2,4,6-trichloroanisole (TCA), other haloanisoles and halophenols in water was optimised by using headspace solid-phase micro-extraction (SPME) and gas chromatography with mass spectrometric detection. The optimised method uses divinylbenzene–carboxen–polydimethylsiloxane (DVB–CAR–PDMS) fiber and allows the determination of TCA at very low concentrations (LOD = 0.1 ng L−1) with good precision (RSD = 8%). The optimum operating conditions were found to be SPME time of 40 min, an extraction temperature of 65 °C, a sample volume of 25 mL, a pH 2.4 an added salt concentration of 20% and magnetic stirring at 700 rpm. The proposed method was used to determine for the first time haloanisoles and halophenols in cork washing waste water as real samples.