This paper describes the interaction of a octa (3-chloropropyl)octasilsesquioxane (SS) functionalized with imidazole (SSI) groups, and its subsequent reaction with silver (AgSSI) and hexacyanoferrate (III) (AgHSSI). The materials SS, SSI were characterized by infrared (FTIR); solid state 13 C and 29 Si nuclear magnetic resonance (NMR). The AgSSI and AgHSSI were characterized by electronic (Uv-Vis) and infrared spectroscopy (FTIR). The AgHSSI was incorporated into a graphite paste electrode and the electrochemical studies were conducted with cyclic voltammetry. The AgSSI system was studied first, followed by the AgHSSI. The spectroscopic studies reveals that preparation was conducted with success.