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Hydrothermal synthesis of titanium dioxide (Ti02) nanoparticles has been studied in situ using synchrotron radiation energy dispersive X-ray diffraction (EDXRD) together with other analytical techniques. The main objective of this research study was to investigate the reaction kinetics and mechanisms of Ti02 crystallization under hydrothermal conditions. The nanoparticles have been produced from hydrothermal treatments of acid (HN03) and alkaline (tetrabutylammonium hydroxide; TBA) peptized sol-gels of different compositions at various temperatures, pressures and time durations. The in situ EDXRD spectra clearly showed that pure Ti02 anatase phase particles were crystallized from TBA peptized sol-gels, whereas pure Ti02 rutile phase particles were produced from the HN03 peptized sol-gels. The crystallization curves constructed from the EDXRD data showed that the rate of the particle formation increased with an increase in the hydrothermal process temperature for both types of sol-gel processes.