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), precursors widely employed in sol-gel processes, has been investigated by electrospray ionization mass spectrometry, By analysis of 10(-6) M methanol solutions 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-butyl) alcohol-methanol complete exchange, This reaction leads to the Ti(OCN3)(4) (3) species, representing the synthon of the polycondensation. Various oligomers of 3 have been detected and characterized by MS/MS experiments, and the related mechanisms have been discussed, A minor oligomeric series due to hydroxyl-containing polycondensation products has also been characterized.