A study of near surface sediments from the Dan River (southeastern USA) was conducted to assess the use of magnetic properties as proxies of coal ash after a recent spill. The watershed geology is diverse and potentially contributes magnetic minerals to riverbed sediment from diabase dikes in the Dan River Triassic Basin and from granitic gneiss outside the basin. Coal ash is heterogeneous, including aluminosilicate spheres, amorphous particles and carbonaceous rods and lacy particles. The magnetic fraction of ash from the failed storage pond is up to 17 wt% and is mostly composed of black spheres with maghemite and magnetite. Ash was detected in riverbed sediment from quiet water settings such as inside of meander bends, the confluence of tributary streams and near islands between the spill site and 20 miles downstream in the Schoolfield Reservoir, Danville, VA. The strong magnetic signal is detected above background in riverbed samples and is strongly positively correlated with total ash; elevated low field magnetic susceptibility (χ LF) is evident in samples with ≥ 12% ash content. Anhysteretic remanent magnetization and hysteresis parameters delineate native sediment, ash-bearing sediment, and diabase dikes. Between 20 and 70 miles downstream of the spill site, ash concentrations were either buried or too low due to dilution with native sediment to be detected with χ LF in riverbed samples.