This thesis describes the synthesis of sol-gel glass materials under different experimental conditions and the result of doping these materials with optical probes. The probes used were Eu3*, U 0 22+ and Cr3+. Changes in optical parameters such as fluorescence, absorption and decay times were used to determine the structure of the material. Eu3+ was easily incorporated into the silica structure. The fluorescence spectra and decay times measured were used to evaluate structural changes of the ion matrix. The use of U022+ as a probe is investigated in this study. U 0 22+ was used as an optical pump for Eu3* when codoped in silica, and energy transfer effects were used to investigate the porosity.