Cobalt-rich Co-Fe-Ti alloys, produced by spark plasma sintering of mechanically alloyed powders, possess a microstructure consisting of an intimate mixture of nanocrystalline intermetallic phases. However, some of these phases, particularly the Cc(2)Ti phases, have not been thoroughly characterized before, and the presence of iron opens several possibilities regarding the location of iron atoms in the crystalline lattices. In the present study, x-ray diffraction methods have been applied to characterize such microstructures, by evaluating the crystallite size, microstrain, volumen fraction of phases and lattice parameters of the materials.