The aqueous redox chemistry of quadricyclo(2.2.1.0(2.6).0(3.5))heptane. commonly known as quadricyclane, and its environmentally important hydrolysis product, nortricyclanol, was investigated through the use of cyclic voltammetry, chronocoulometry, and rotating disk electrochemical methods. Oxidation of both compounds in aqueous environments yields polymeric films that rapidly foul the working electrode. A novel experimental approach was developed to circumvent the problems associated with the formation of the fouling films, which were further characterized using attenuated total reflectance infrared spectroscopy.