Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative standard deviations (RSD), were below 20%. Real wastewaters and seawaters were analyzed. The method permits controlling legislated annual average values.
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