Four organosilicate polymers synthesized by addition of vinyl- and H-s
ubstituted double four-ring silicic acid derivatives were characterize
d using DSC and simultaneous TG-DTA measurements. Thermooxidative deco
mposition proceeds in several steps: Oxidation of (Si-H) groups, oxida
tion of (Si-CH2-CH2-Si) bridges, and oxidation of (Si-CH3) groups, wit
h formation of new (Si-O-Si) bonds. Si-29-NMR-spectroscopic measuremen
ts confirm this interpretation. Thermoanalytical methods of investigat
ion proved useful to characterize these organosilicate polymers.