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 HC1.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.