Silica gel and Cab-O-Sil were chemically modified (silylated) with 3-aminopropyltriethoxysilane and 3-methacryloxypropyltrimethoxysilane under carefully controlled conditions. Subsequently the products were investigated by elemental analysis, Fourier transform IR spectroscopy, and 13C and 29Si crosspolarization magic angle spinning NMR (CP-MAS NMR). The influence of the reaction conditions of the silylation and the effect of subsequent heat treatment and water addition were studied. The resulting differences shed new light on the combined effects of reaction conditions and silica surface structures on the course of the reactions. Some assignments of 29Si NMR signals to specific structures were confirmed, while in one case a reassignment was proposed.

Poly(N‐vinylcarbazole) (PVK) samples were found to exhibit up to three glass transition temperatures Tg, corresponding to the whole chain and the syndiotactic and isotactic stereoblocks. An increasing tendency to multiple Tgs, and hence to phase separation, was observed with increasing isotacticity. Limiting values at infinite molecular weight for syndiotactic and isotactic PVK were obtained from correlations of the Tgs corresponding to the syndiotactic and isotactic stereoblocks with their respective average stereoblock lengths derived from 13C NMR measurements. They were found to be 549 and 399 K, respectively. The conventional Tg for PVK was found to exhibit the following dependence upon the syndiotactic dyad mole fraction Xs: The molecular weight dependences of the conventional Tgs for several fractionated PVK samples obeyed a Fox–Flory‐type relation with values of −dTg/d(1/M) varying between 7.6 × 103 for isotactic PVK and 2.7 × 105 for Luvican M 170.

Comparison of steroids, containing a 4,6-dien-3-one system, shows that the difference between the two frequencies of the unsaturated system in compounds with a vetro-configuration is greater than that in compounds with a natural one.