This work undertakes an archeometallurgical study of ferrous and non-ferrous artifacts recovered from historical sites of Rio de Janeiro. The experimental research developed an analytical methodology based on destructive techniques, such as Optical Microscopy (OM), Scanning Electronic Microscopy (SEM) and Transmission Electronic Microscopy (TEM); as well as non- destructive techniques, namely X-Ray Fluorescence (XRF) and Particle Induction X-Ray Emission (PIXE). These artifacts were analyzed in order to characterize their composition, structure and elaboration/processing methods. There are six artifacts with a non-ferrous metallic nature and one with a ferrous metallic nature. The ferrous metallic artifact was a hoe. The microstructure characteristics is related to the usage of this object at that time, and indicates that the hoe could have been made in Brazil by African slaves. The analysis of the hoe indicates that it was elaborated from puddle iron and that it had been processed by foundry and forging. The rosary, one of the non-ferrous artifacts, is formed by singlephase brass riche in copper; and according to historical research it is of European origin, deriving from pyrite ore. The medals are also of European origin and are based on brass. Historically one can deduce that they are dated from the 18th century. The two coins from the Rochedo site most probably came from distinct sources, as validated by the chemical analysis. However, the chemical composition of the 1821 coin is close to that of the 40 réis coin. The present thesis has shown the importance of a systematic methodology to characterize ancient objects combining both destructive and non- destructive techniques.