I. Koch et al., DEMETHYLATION OF TRIMETHYLANTIMONY SPECIES IN AQUEOUS-SOLUTION DURINGANALYSIS BY HYDRIDE GENERATION GAS-CHROMATOGRAPHY WITH AAS AND ICP MSDETECTION, Applied organometallic chemistry, 12(2), 1998, pp. 129-136
The method of hydride generation for the speciation of antimony compou
nds was examined with respect to the problem of molecular 'rearrangeme
nt'. Specifically, demethylation of trimethylstilbine during the analy
sis of trimethylantimony dichloride (Me3SbCl2) was studied, Previously
published observations that enhanced demethylation takes place as a r
esult of inadequate preconditioning of the analytical apparatus were f
ound to be not reproducible, However, demethylation was enhanced as th
e pH decreased when using two different analytical methods: semi-conti
nuous how hydride generation-gas chromatography-atomic absorption spec
trometry (HG-GC-AAS), and batch-type hydride generation-gas chromatogr
aphy-inductively coupled mass spectrometry (HG-GC-ICP MS). Application
s of the hydride generation method to environmental samples revealed d
ifferences in analytical results at high and low pH, and enhanced deme
thylation taking place because of the matrix in a fungal extract sampl
e, The authors recommend that researchers using the method of hydride
generation for antimony compounds carefully test the reaction conditio
ns with standard compounds and use the method of standard addition onl
y. (C) 1998 John Wiley & Sons, Ltd.