Speciation of organotin in sediments by multicapillary gas chromatography with atomic emission detection after microwave-assisted leaching and solvent extraction-derivatization

Microwave-assisted leaching of organotin compounds from sediment samples fo llowed by the si multaneous extraction-derivatization of the extracted spec ies was revisited with the goal to compare the existing procedures, improve their recoveries and extend them to phenyltin compounds. The stability of butyl- and phenyltin compounds under microwave field, real recoveries of th e whole analytical procedure, effect of the extraction solvent, and the nec essity for an internal standard were evaluated using two candidate referenc e sediments, The combination of the optimized sample preparation procedure with multicapillary chromatography resulted in a rapid (2 min leaching + 5 min extraction-derivatization + 3 min chromntographic separation) and effic ient analytical procedure for speciation analysis of organotin compounds in sediment samples, The detection limit achieved with a microwave-induced pl asma atomic emission detector was 2 ng g(-1).