Electrospray ionization in the study of the polycondensation of Ti(O-i-C3H7)(4) and Ti(O-n-C4H9)(4)

The polycondensation of Ti(O-i-C3H7)(4) (1) and Ti(O-n-C4H9)(4) (2), precur sors widely employed in sol-gel processes, has been investigated by electro spray ionization mass spectrometry, By analysis of 10(-6) M methanol soluti ons of compounds 1 and 2, the same ionic species are detected, proving that the first step in the polycondensation reaction is the i-propyl (or n-buty l) alcohol-methanol complete exchange, This reaction leads to the Ti(OCN3)( 4) (3) species, representing the synthon of the polycondensation. Various o ligomers of 3 have been detected and characterized by MS/MS experiments, an d the related mechanisms have been discussed, A minor oligomeric series due to hydroxyl-containing polycondensation products has also been characteriz ed. Copyright (C) 2000 John Wiley & Sons, Ltd.