ABSTRACT:The three-step polymerization process of a well-defined polymeric silane coupling agent, 3-(triethoxysilyl)propyl-terminated polystyrene, catalyzed by 1 mol/kg KOH-H 2 O, was traced as a function of reaction time using a gel-permeation chromatography (GPC) technique. A set of GPC traces collected during the polymerization was then converted to two-dimensional (2D) correlation maps, by using generalized 2D correlation analysis. The 2D correlation GPC maps reflected the details of the aggregational behavior (in particular, the aggregate-aggregate correlations) in each step of the polymerization, thus demonstrating the promising potential of this technique.