Ion pair of cationic surfactant (cetytrimethylammonium bromide) and tungestosilicic acid incorporated in PVC matrix, was used for coating a piece of copper wire as a new high sensitive SPME fiber in extraction and determination of BTEX compounds from the headspace of water samples prior to GC/FID analysis. Under optimum extraction conditions, limits of detection for benzene, toluene, ethylbenzene, p-xylene, m-xylene and o-xylene were found to be 1.18, 5.61, 0.87, 0.29, 0.22 and 0.33 ng L(-1) respectively. Low detection limits, wide linear dynamic ranges, good reproducibility (RSD% 1.48-4.27), high fiber capacity and high mechanical durability are some of the most important advantages of the new fiber.

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