Novel approach to separation and identification of organometallic compounds in complex mixtures by means of particle beam liquid chromatography/mass spectrometry: the case of diphosphine-substituted selenido iron and ruthenium clusters

Abstract

The particle beam liquid chromatography/mass spectrometry (PB LC/MS) characterization of diphosphine-substituted selenido iron and ruthenium clusters is reported. The clusters considered result from the reaction between the diphosphine diselenides (Ph2PSe)2R [R = CH2, dppmSe2; R = CH2CH2, dppeSe2; R = (C5H4)2Fe, dppfcSe2] and Fe3(CO)12 and Ru3(CO)12. Complex reaction mixtures were separated under adsorption chromatographic conditions and characterized on-line by means of the positive-ion and negative-ion chemical ionization mass spectra of the eluates. The PB LC/MS analysis of the crude reaction mixtures proved useful, avoiding sample manipulation and/or sample degradation; this is particularly important for those compounds sensitive to oxygen or light, or which are unstable in solution. The spectra obtained showed characteristic fragmentation patterns and detailed structural information. © 1998 John Wiley & Sons, Ltd.