Nanocrystalline TiO2 was prepared by the sol-gel method. The fine and homogenous particles were obtained by calcining the complex gel consisted of precursor TiO(NO3)(2). H2O and gelatin dispersant in air. The complex gel was analyzed by thermogravimetric analysis and differential scanning calorimetry in air and N-2. It was found that during heating a novel and stable medium material has formed at 180 degrees C by the chains entanglement between precursor and dispersant, the NO3- decomposition temperature in this medium is delayed and reaches the temperature range of dispersant oxidation and decomposition. The calcining procedure for the complex gel in N-2 is similar to in air but the dispersant oxidation in N-2 is only by means of NO; decomposition and the heat evolved is greatly decreased.