Solid acid-base sensor materials were prepared by encapsulating three pH indicators (alizarin red, brilliant yellow, and acridine) within a silica matrix using a sol-gel approach through three different routes: (1) non-hydrolytic, (2) acid-catalyzed, and (3) base-catalyzed. Raman and Fourier transform infrared spectroscopies were used to evaluate the silica-indicator interactions. Because vibrational bands assigned to functional groups present in the indicator molecules were not detected, the main silica stretching mode ν<sub>Si-O</sub> between approximately 1300 and 1000 cm<sup>-1</sup> was used to detect the presence of our indicators within the silica matrix. The large band centered at 1100 cm<sup>-1</sup> was deconvoluted into four components corresponding to the longitudinal optic and transversal optic modes of the silicon monoxide (SiO)<sub>4</sub> and (SiO)<sub>6</sub> siloxane rings. Using the component area of each mode, it was possible to calculate the percentage of each structure. Such percentages ranged from 49% to 70% (SiO)<sub>6</sub> for the analyzed samples, within a confidence level of 95% (<i>p</i> = 0.05). (The confidence limits were 53-62%.) These results could be related to the pH indicator content, indicating that the quantity of the encapsulated molecule affects the (SiO)<sub>6</sub> percentage values. In addition, a comparison with the radius of gyration obtained by small angle X-ray scattering was done. These results indicate that the analyte accesses the receptor elements through the passages between the siloxane rings but not through the siloxane rings themselves.

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