Uranyl is a hexavalent, dicationic form of uranium possessing a linear [O=U=O]2+ arrangement. Uranyl is well known to be photoactive, generating a highly reactive excited state complex that can perform hydrogen atom abstraction chemistry. The goal of this project is to make silicate monoliths using tetraethoxysilane doped with uranyl to perform photochemistry. Xerogels are a porous material made from the sol-gel process—which is the hydrolysis, condensation, and gelation of siloxanes. These transparent materials can be made into fibers, films, and monoliths—the last of which is of interest for this project. Research has shown that vanadium and chromium can be immobilized within xerogel glasses while still allowing for reactivity at the metal sites. Additionally, it has been reported that uranyl-doped sol-gels remain photoactive while immobilized in sol-gel glasses. In our study, we are preparing monoliths containing various concentrations of uranyl in order to better understand the surface dynamics and photochemistry of the immobilized uranyl. This work will provide a greater understanding of the photoactivity of various uranyl sources when suspended in a glass matrix