Preparation of sol-gel polyethylene glycol-polydimethylsiloxane-poly(vinyl alcohol)-coated sorptive bar for the determination of organic sulfur compounds in water

A novel headspace sorptive extraction (HSSE) using a glass bar coated with carbowax (polyethylene glycol)-polydimethylsiloxane-poly(vinyl alcohol) (CW/PDMS/PVA) prepared by sol-gel technology method was proposed for the determination of volatile organic sulfur compounds (VOSs) in water. After the extraction, the sorptive bar was desorbed with 60 mu L of ethanol and 30 mu L of the extract was analysed by large volume injection (LVI) into a gas chromatography-flame photometric detector (GC-FPD). The parameters affecting the headspace sorptive extraction of VOSs such as extraction and desorption time, extraction temperature, stirring speed, desorption solvent, headspace phase ratio, salt and pH were carefully investigated and the optimized experimental conditions were established. The limits of detection (LODs) for the studied VOSs ranged from 0.04 to 4.8 mu g/L with the relative standard deviations (RSDs) ranging from 4.5 to 10.2% (n = 6). The reproducibility for the preparation of CW/PDMS/PVA-coated sorptive bar ranged from 3.2 to 9.2% in one batch, and from 2.8 to 18.5% in batch-to-batch, and more than 50 extractions can be achieved without apparent loss. The proposed method was compared with polydimethylsiloxane-HSSE and carboxen/PDMS-headspace-solid phase microextraction (CAR/PDMS-HS-SPME) under their optimum conditions, CW/PDMS/PVA-HSSE shows the highest adsorption capacity (larger surface area and more active sites), the highest sensitivity (about 10 times) and the best polarity matching for VOSs. (C) 2008 Elsevier B.V. All rights reserved.