The mining of gold can lead to toxic metals such as mercury (Hg) contaminating watercourses as by-products. The Reedy Creek sub-catchment, in northeast Victoria, Australia, was mined for gold in the 1850s. In 1998, samples were taken from six watercourses to measure any remaining toxic metal contamination in sediments and surface waters from two creeks with no previous gold mining (controls) and four that were mined. Although mean concentrations of Hg (measured using an ICP-OES) in sediments were below worldwide background levels, individual sites along Reedy Creek had slightly elevated Hg concentrations. In contrast, the Hg concentrations in the surface waters were above background levels. Temporal fluxes of very high Hg concentrations in the surface waters during periods of first flow and flood events revealed that Hg concentrations in the surface waters may, at certain times of the year, exceed all Australian and New Zealand Environment and Conservation Council (National Water Quality Management Strategy. Australian Water Quality Guidelines for Fresh and Marine Waters, ANZECC, 2000) guidelines for water use and the protection of the aquatic ecosystem.