A novel analytical method called two-dimensional correlation gel permeation chromatography (2D GPC) is introduced. In 2D GPC, generalized two-dimensional (2D) correlation analysis is combined with time-resolved gel permeation chromatography (GPC). This technique can be used effectively, for example, to study intricate details of a polymerization process. In this study, a sol−gel polymerization process of octyltriethoxysilane catalyzed by 1.0 M HCl·H2O is traced as a function of reaction time using the GPC technique. A set of GPC traces sequentially collected at different sampling points during the polymerization reaction are then converted to two-dimensional correlation maps. It has been found that the 2D GPC maps created by the correlation analysis directly reflect the reaction mechanism in the polymerization process, thus demonstrating the promising potential of this technique.

The novel analytical technique, two-dimensional (2D) correlation analysis, has been applied to a set of time-resolved gel permeation chromatography (GPC) profiles of 1H,1H,2H,2H-perfluorooctyltriethoxysilane (PFOTES) to investigate intricate details of the process of its polymerization, catalyzed by 1 M HCl·H2O, over a thirty minute period. In particular, the splitting behavior of the correlation cross-peaks and their intensity variation have been examined in detail, leading to the conclusion that the mechanism of the growth process of polymeric aggregates is strongly reflected in the patterns of the observed spectra. The 2D correlation GPC method, which has been used to follow the time-dependence of the split components, has proved to be a powerful tool in elucidation of the reaction mechanism.

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