<i>n</i>-Octadecyltriethoxysilane (C<sub>18</sub>-TEOS) and tetraethoxysilane (TEOS) were used as the precursors to fabricate an organic-inorganic hybrid composite by sol-gel processing. The hydrolysis and initial condensation reactions of TEOS and C<sub>18</sub>-TEOS/TEOS mixtures were studied by <sup>29</sup>Si-NMR spectroscopy. The rate of disappearance of the silane precursors and the evolution of the various silicon species during the reaction indicate that TEOS hydrolyzes and condenses faster than C<sub>18</sub>-TEOS. The rate of hydrolysis for C<sub>18</sub>-TEOS, however, increases when reacting in the C<sub>18</sub>-TEOS/TEOS hybrid mixture, indicating that the condensation reactions involving TEOS species drive the reaction of C<sub>18</sub>-TEOS. The formation of cross-condensed products leads to the composite with octadecyl groups incorporated into the final glass material. The maximum degree of condensation in the C<sub>18</sub>-TEOS/TEOS mixture was observed after 2 h of reaction. Fused-silica capillary columns were coated with the C<sub>18</sub>-TEOS/TEOS mixture while in its liquid-like stage. After drying, the columns were tested for open tubular capillary electrochromatography (OT-CEC). Coating of the columns was performed after the maximum degree of condensation was achieved, which has been shown to correlate with maximum chromatographic retention.

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