Microwave-accelerated speciation analysis for butyltin compounds in sediments and biomaterials by large volume injection capillary gas chromatography quartz furnace atomic absorption spectrometry.
Résumé
A method for speciation anal. of butyltins in sediments and biomaterials by capillary GC with at. absorption spectrometric detection was developed. Mono-, di- and tributyltin in sediments were quant. leached with 50% acetic acid, whereas biomaterials were dissolved in a 25% tetra-Me ammonium hydroxide (TMAH) soln.; both processes were completed under the action of a low-power focused microwave field within 1-5min, which is 20-100 times faster than with conventional procedures. The butyltins were derivatized with sodium tetraethylborate (NaBEt4) in the aq. phase, and simultaneously extd. into hexane (5min). Online preconcn. in the injector liner by solvent venting enabled to obtain a detection limit of 5 ngg-1 for 0.2g of dry sample. A sample throughput of 5 samples h-1 was achieved. The method was validated by analyzing three certified ref. materials: PACS-1, CRM 462 and NIES 11. [on SciFinder(R)]