Recently, we showed that reactive oxygen species (ROS) formation was involved in the toxicity of the redox-active metal Cu and mixtures of Cu plus a photomodified polycyclic aromatic hydrocarbon (PAH), phenanthrenequinone (PHQ), to Daphnia magna. It is unknown, however, if similar results can be observed for metals with lower or no redox activity and their mixtures with PHQ. In the present study using D. magna, the toxicity of Ni, a weakly redox-active metal, and of Cd, a non-redox active metal, was examined with or without PHQ. The abilities of Ni, Cd, PHQ, and binary mixtures of metal plus PHQ to generate ROS were measured using a 2',7'-dichlorofluorescein fluorescence assay. The results were compared with the results of Cu and mixtures of Cu plus PHQ from a recent study by our group. The order of metal toxicity to D. magna was found to be Cd > or = Cu > Ni. As with Cu/PHQ mixtures, synergistic toxicity was observed for mixtures of Ni and PHQ, whereas additive toxicity was observed for mixtures of Cd and PHQ. Alone, PHQ had no impact on ROS levels in D. magna. Nickel alone caused elevated ROS, which was further enhanced in the presence of PHQ. Neither Cd nor Cd/PHQ mixtures increased ROS production. Attenuation of toxicity and ROS production was observed in response to treatment with low concentrations of L-ascorbic acid. These results indicate potential toxic interactions between metals and modified PAHs. With redox-active metals, such as Cu and Ni, and modified PAHs, such as PHQ, these interactions can involve ROS formation.