The recovery of gold from ores containing arsenopyrite releases significant amounts of arsenic into the environment. Arsenic releases primarily result from the processing and oxidation of stored mine tailings. This investigation examines: (1) the distribution of arsenic, iron, manganese and their chemical species in sediment cores extracted from a tailings impoundment in the Kemerovo region of southwestern Siberia; and (2) the weathering of arsenic minerals collected from its tailings dam. The data demonstrate that during storage of the sediments within the impoundment, arsenic is predominantly present as residual arsenopyrite and, to a lesser degree, as substances co-precipitated with iron hydroxide. The arsenic released from the sediment results from an oxidative dissolution of arsenopyrite and reductive dissolution of Fe oxides.