Glass plates coated with TiO2 were used in a photocatalytic process to collect mercury, lead, copper and cadmium from aqueous solutions containing individual metals and mixtures. Stripping voltammetry, verified to achieve 1-10 ppb detection limits, was used to show that individual metals at concentrations of 1000 to 5200 ppb were reduced to undetectable levels in 3 to 55 min. Capillary electrophoresis (CE) with 8-hydroxyquinoline-5-sulfonic acid as complexing agent was used when appropriate, since it could quantitate all four metals under study in one run although it was less sensitive. It was demonstrated that 100 mL solutions containing 10 ppm of each of the four metals could be treated with a 10 cm2 TiO2-coated plate to leave undetectable metal concentrations in one hour. Stripping voltammetry using carbon electrodes coated with mercury films was estimated to generate daily about 1.1 L of aqueous waste containing 0.1 ppm of each metal. The results indicate the feasibility of assembling an apparatus capable of treating the waste generated by stripping voltammetry to render the latter suitable for routine on-site analyses without environmental concern. Data were also obtained to show the effectiveness in treating silver containing solutions, indicating suitability of the photocatalytic process in treating photographic processing wastes.