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Two-dimensional correlation gel permeation chromatography (2D GPC) was used to elucidate intricate details of the initial ten minutes of the sol–gel transition of n-octyltriethoxysilane (OTES), catalysed by 0.5 and 2.0 M HCl·H 2 O. The results demonstrate that the features of 2D GPC correlation spectra directly reflect the dynamic variation of reactions or interactions present during the polymerization process.

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