In this work we characterize sediment samples from several points in the River Toledo-PR, using the PIXE (Particle Induced X-Ray Emission) spectroscopy technique, in order to quantify trace elements in these samples aiming to provide information about pollution levels for trace elements. The samples were collected in six points of river, during a period of twelve months (12/2001 to 11/2002). The collected material was air-dried at room temperature and then pressed in pellets. The samples were irradiated under vacuum using a H beam of 2,39MeV in the LAMFI (Laboratório de Análises de Materiais por Feixe Iônico). Produced xrays were detected using a Si(Li) detector and a standard electronics. Using the Axil program to analyze PIXE spectra it was possible to identify and quantify some elements present in the samples. A multi-elemental referenced material (Buffalo River sediment-RM 8704) was used to validate the PIXE analysis with thick targets. Twelve months of monitoring of six river points were analyzed and these allowed us to identify 18 elements such as Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr e Pb. The following elements were monitored: V, Cr, Mn, Co, Ni, Cu, Zn e Pb. © 2009 American Institute of Physics.