Crystallite size determination of MoS2 particles is still a controversial problem fuelling the debate on the morphology of hydro-treating catalysts, The size of MoS2 crystallites determined from extended X-ray absorption fine structures (EXAFS) is close to 1 nm, whereas TEM picture analysis give an average size of 3 to 3 mo, It is obvious that these techniques have intrinsic strengths and weaknesses and that the results may not be comparable because of these differences, However, it is our intention to obtain a better understanding of these crystallite sizes by studying the dispersed unsupported solids, Various techniques were used : nitrogen adsorption-desorption, X-hay diffraction (XRD), XAFS, TEM, and temperature-programmed reduction (TPR) and the results were compared and discussed, The samples were prepared by thiosalt decomposition or molten salt synthesis, These solids presented different morphologies, the latter method providing higher surface area samples. The specific surface areas varied from 4 to 125 m(2)/g and, depending on the method of preparation, microporous and mesoporous solids were obtained. XRD, TEM, and TPR were found to be complementary and coherent methods for determining the size parameter, EXAFS interpretation does not give consistent results due to local reorganization at the periphery of the crystallites,