Speciation without chromatography - Part I. Determination of tributyltin in aqueous samples by chloride generation, headspace solid-phase microextraction and inductively coupled plasma time of flight mass spectrometry

An analytical procedure was developed for the determination of tributyltin in aqueous samples. The relatively high volatility of the organometal halid e species confers suitability for their headspace sampling from the vapour phase above natural waters or leached solid samples. Tributyltin was collec ted from the sample headspace above various chloride-containing matrices, i ncluding HCl, sodium chloride solution and sea-water, by passive sampling u sing a polydimethylsiloxane/divinylbenzene (PDMS/DVB)-coated solid-phase mi croextraction (SPME) fiber. Inductively coupled plasma time-of-flight mass spectrometry (ICP-TOFMS) was used for detection following thermal desorptio n of analytes from the fiber. A detection limit of 5.8 pg ml(-1) (as tin) w as realized in aqueous samples. Method validation was achieved using NRCC P ACS-2 (Sediment) certified reference material, for which reasonable agreeme nt between certified and measured values for tributyltin content was obtain ed.