Mining of massive sulfide deposits in southwestern Spain extending back to the Copper and Bronze Ages has resulted in the pollution of the Rio Tinto fluvial-estuarine complex, the site of Columbus' departure for the New World in 1492. Additional sources of potential pollution include the large industrial complex at Huelva near the lower portion of the estuary. Extensive analysis of surface sediment samples and cores has established that there are no geographic trends in the distribution of the pollutants, which include Cu, Fe, Pb, Zn, Ti, Ba, Cr, V and Co. These data have, however, demonstrated that tidal flux within the estuary carries phosphorus and perhaps other elements from the industrial complex at Huelva to the tidal limit of the system, several kilometers upstream from the discharge site. Radiometric analysis of short cores shows that sedimentation rates over at least the past couple of centuries have been about 0.3 cm/year. These data and that from a single deep core demonstrate that the estuary was polluted from mining activity long before the large-scale operations began in the late nineteenth century.