The analysis of purification and carbonization process in argon with use of nc-TiC x /C powder, obtained by sol-gel method, is presented. TG-DSC measurements were carried out under non-isothermal and isothermal conditions. The samples were heated up in series to 1473, 1573, 1673, and 1773 K. For this series description of process kinetics is presented. Four stages of the process have been distinguished. Kinetics was described using Coats-Redfern equation. The kinetic parameters were determined for particular stages. Using obtained kinetic data, the analysis of the process was performed. The a(T) and r(a,T) dependencies on heating rate and temperature were investigated. In order to obtain high carbonization degree and carbide particles of small size, an appropriate temperature and time of process duration have to be determined. Appropriate carbonization and particles size were obtained for series heated up to 1570 K. It has been demonstrated that the oxygen, present at trace level in argon, can react with components of the system in certain range of temperature, influencing the quality of obtained product. The particles have been depicted by TEM method, whereas characterization of structure and particles size was performed by XRD method. MS method was used to determine evolved gaseous products.