| Abstract: | The method of hydride generation for the speciation of antimony compounds was examined with respect to the problem of molecular "rearrangement'. Specifically, demethylation of trimethylstilbine during the analysis of trimethylantimony dichloride (Me3SbCl2) was studied. Previously published observations that enhanced demethylation takes place as a result of inadequate preconditioning of the analytical apparatus were found to be not reproducible. However, demethylation was enhanced as the pH decreased when using two different analytical methods: semi-continuous flow hydride generation–gas chromatography–atomic absorption spectrometry (HG– GC–AAS), and batch-type hydride generation– gas chromatography–inductively coupled plasma mass spectrometry (HG–GC–ICP MS). Applications of the hydride generation method to environmental samples revealed differences in analytical results at high and low pH, and enhanced demethylation taking place because of the matrix in a fungal extract sample. The authors recommend that researchers using the method of hydride generation for antimony compounds carefully test the reaction conditions with standard compounds and use the method of standard addition only. © 1998 John Wiley & Sons, Ltd. |
