S. Tutschku et al., PRECONCENTRATION AND DETERMINATION OF SN-ORGANIC AND PB-ORGANIC SPECIES IN ENVIRONMENTAL-SAMPLES BY SPME AND GC-AED, Fresenius' journal of analytical chemistry, 354(5-6), 1996, pp. 587-591
A new sample preparation and preconcentration technique - solid phase
microextraction (SPME) - is reported for the application of several ti
norganic compounds and tetrabutyllead in aqueous samples. The solvent-
free procedure is rapid in comparison with liquid-liquid extraction or
SFE but also sensitive. Analytical variables of the extraction such a
s adsorption and desorption time, stirring rate and temperature has be
en investigated. The determination has been performed by GC coupled wi
th atomic emission detection (AED). After optimization of the conditio
ns of SPME a calibration was realized on the basis of a multicomponent
standard solution, prepared by ethylation of organotin salts directly
in the sample using sodium tetraethylborate (NaBEt(4)) without prior
separation of the analytes from the matrix. The method permits preconc
entration. Values of about 10 can be reached. A detection limit of 0.0
9 pg Sn and 0.08 pg Pb can be achieved under optimized conditions. The
proposed procedure has been successfully applied to the analysis of o
rganotin compounds in various slurry samples.