ABSTRACT.-Two different types of ancient bricks (XII-XIVth centuries) collected from historical buildings of Toledo (Spain) were characterized by Optical Microscopy, SEM/EDS, Electron microprobe, XRD, DTA and 57 Fe-Mössbauer spectroscopy. Physical properties such as water absorption and suction, porosity, density and compression strength were also determined.Several minerals found in the brick matrix, such as garnet, let us infer raw material sources; calcite, dolomite, illite and neo-formed gehlenite and diopside phases, on temperature reached in firing; secondary calcite, on first cooling scenarios; and manganese micro-nodules, on late pollution environments. XRD and DTA of original and re-fired samples supply information about firing temperatures. Additional data on firing conditions and type of the original clay are provided by the Mössbauer study. Physical properties of both types of bricks were compared and correlated with raw materials and fabric and firing technology employed. The physicochemical characterization of these bricks provides valuable data for restoration purposes to formulate new specific bricks using neighbouring raw materials.