The main land use/land cover changes (LULCC) have been associated with population growth and energy policies in the São Paulo State, Brazil, since 1970. The LULCC can alter the behavior of trace elements in different environmental systems, with the riverbed sediments being the main reservoirs or sinks for trace elements, and thus become a valuable environmental archive on temporal changes. Thus, the main purpose of the study was to apply a multi-tracer analysis to estimate the historical evolution of pollution in riverbed sediment of a subtropical watershed, the lower course of the Piracicaba River, São Paulo, Brazil. Pb measurements done on river sediment core samples allowed estimating a sedimentation rate of 9 mm yr between 1971 and 2001. Zn was the most abundant trace element in the sediment core, followed by Cr, Cu, Ni, Pb, Sc and Cd. The total concentrations of Cd, Cr, Ni, Sc and Pb presented practically no variations in the sediment core, with a continuous excess of ca. 0.27 μg g yr of Cu and of ca. 0.54 μg g yr of Zn between 1971 and 2001. The excess of Cu and Zn was associated with labile fractions, in particular with carbonate bound to Zn and organic matter bound to Cu. The assessment of trace metal pollution indicated that most of the trace elements were of geogenic origin, except for Cu and Zn. According to the sediment quality guidelines used in Brazil, Pb showed no potential toxic effect, Cu, Cr and Zn were intermediate to Threshold Effect Level (TEL) and Probable Effect Level (PEL) and the Cd and Ni concentrations were above the PEL limits. The elemental and isotopic analysis of C and N and the C/N ratio indicated that the anthropogenic origin of POM found in the sediment core is related mainly to domestic sewage.

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