The present study aimed to evaluate Cu, Cr, Ni, Zn, Pb, Mn, Al, and Fe contents, as well as their geochemical partitioning in Sinos River basin sediments in southern Brazil. This basin is a densely populated area with a substantial number of industries, especially metallurgy, electroplating works, steel mills, petrochemicals, and tanneries. The total metal concentrations were determined by X-ray fluorescence and the sediment phase concentrations were determined by applying the BCR-701 sequential extraction method proposed by the Community Bureau of Reference of the European Community, using ICP/OES. The contents extracted by a solution of 0.5 mol/L HCl were also considered. Metal contents were evaluated in the sediment fraction <63 µm. Results in the industrialized and densely populated region showed an increase in the total concentrations of Cu, Cr, Zn, and Pb, and in the potentially mobile fractions for Cu, Cr, Zn and Ni sequentially extracted. Cr stood out particularly in the Portão stream, showing 1,286 mg/kg as a result of the total concentration, considering the tannery region influence.