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Full PaperSampling and determination of metal hydrides by solid phase microextraction thermal desorption inductively coupled plasma mass Direct coupling of solid phase microextraction (SPME) with inductively coupled plasma mass spectrometry (ICP-MS) was used for the non-selective determination of arsenic, selenium, antimony and tin species amenable to hydride generation. A thermal desorption interface consisting of a heated glass-lined splitless type GC injector was placed directly at the base of the torch to minimize the length of the transfer-line. The effects of time and concentrations of sodium borohydride and hydrochloric acid on the extraction ef®ciency were optimized. Polydimethylsiloxane (PDMS) and polydimethylsiloxane/Carboxen (PDMS/Carboxen) SPME coatings were compared for the headspace extraction of the hydrides. PDMS/Carboxen showed better extraction capacity and enhanced selectivity for tin hydrides. SPME provided good sensitivity and an approximately 3.5...