Rapid speciation of butyltin compounds in sediments and biomaterials by capillary gas chromatography-microwave-induced plasma atomic emission spectrometry after microwave-assisted leaching/digestion

Abstract

A rapid procedure for the simultaneous determination of mono-, di- and tributyltin in sediments and biological materials is described. The target compounds in sediments were subject to quantitative microwave-assisted leaching with acetic acid. Biomaterials were dissolved in a tetramethylammonium hydroxide solution under the action of a low-power microwave field in such a way that the organotin moiety remained intact. The leaching of the analytes from a sediment as well as the dissolution of a biomaterial in a focused microwave field took only 1–5 min, which is much faster than previously reported methods. It was also demonstrated that the leaching efficiency of monobutyltin from certified reference sediments was superior to that of most literature procedures. The butyltins were derivatized with sodium tetraethylborate (NaBEt₄) in the aqueous phase, and simultaneously extracted into isooctane (5 min). The analysis was carried out by capillary gas chromatography (GC) with microwave-induced plasma atomic emission detection. The sample throughput was limited by the duration of the GC run (10 min). The detection limit was 2 ng g^–1 for 0.2 g of sample (dry) without preconcentration; it could be improved by a factor 10 if preconcentration was applied. The developed method was applied to a variety of real samples and was validated by analysing three certified reference materials: PACS-1, CRM 462 and NIES 11.