Water and sediment samples were collected from streams in Spearfish Creek, Whitewood Creek, and Bear Butte Creek watersheds in the Black Hills, SD, an area impacted by gold mining operations. Arsenic concentrations that exceeded the U.S. Environmental Protection Agency's Maximum Concentration Limit of 50 microg/L for drinking water were found in water from Annie Creek, a tributary of Spearfish Creek, and from Whitewood Creek. Gold Run, a tributary of Whitewood Creek, and Annie Creek contained Se concentrations in water that exceeded the EPA Ecotox threshold of 5 microg/L and were classified as a high hazard for Se accumulation from water into the planktonic food chain and for resultant toxicity to fish and aquatic birds. Concentrations of As, Cd, Cu, Hg, Ni, Pb, and Zn in sediment exceeded EPA Ecotox thresholds in one or more of the watersheds suggesting potential adverse ecological effects. Sediment from Rubicon Creek, a tributary of Spearfish Creek, contained Se concentrations high enough (4.0 microg/g) to be a moderate hazard for accumulation from sediments into the benthic food chain, with resultant dietary toxicity to fish and aquatic birds. These results are discussed in light of historical mining activities and recent clean-up and reclamation efforts. Based on the results and comparisons to Ecotox tresholds, further studies of ecological effects are warranted.