RAPID SPECIATION OF BUTYLTIN COMPOUNDS IN SEDIMENTS AND BIOMATERIALS BY CAPILLARY GAS-CHROMATOGRAPHY - MICROWAVE-INDUCED PLASMA-ATOMIC EMISSION-SPECTROMETRY AFTER MICROWAVE-ASSISTED LEACHING DIGESTION

A rapid procedure for the simultaneous determination of mono-, di- and tributyltin in sediments and biological materials is described, The t arget compounds in sediments were subject to quantitative microwave-as sisted leaching with acetic acid, Biomaterials were dissolved in a tet ramethylammonium hydroxide solution under the action of a low-power mi crowave field in such a way that the organotin moiety remained intact, The leaching of the analytes from a sediment as well as the dissoluti on of a biomaterial in a focused microwave field took only 1-5 min, wh ich is much faster than previously reported methods. It was also demon strated that the leaching efficiency of monobutyltin from certified re ference sediments was superior to that of most literature procedures, The butyltins were derivatized with sodium tetraethylborate (NaBEt(4), ) in the aqueous phase, and simultaneously extracted into isooctane (5 min), The analysis was carried out by capillary gas chromatography (G C) with microwave-induced plasma atomic emission detection, The sample throughput was limited by the duration of the GC run (10 min), The de tection limit was 2 ng g(-1) for 0.2 g of sample (dry) without preconc entration; it could be improved by a factor 10 if preconcentration was applied, The developed method was applied to a variety of real sample s and was validated by analysing three certified reference materials: PACS-1, CRM 462 and NIES 11.