This investigation presents the synthesis procedure and the results of an investigation of the crystallite growth of TiO 2 and the formation of Si-O-Ti bonds in novel silica xerogel (SiO 2 ) glass ceramic produced from an amorphous SX derived from sago waste ash. The composition had been prepared by adding various amounts of TiO 2 , from 20 wt% to 80 wt%, into the amorphous SiO 2 , and then a series of samples were sintered at 1200°C for 2 hours. The influence of the content of TiO 2 and the sintering temperature on the properties of TiO 2 , namely crystallite size and formation of Si-O-Ti bonds, has been studied in detail. The properties of the produced ceramics have been characterized on the basis of the experimental data obtained using X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. It has been found that an addition of SiO 2 confers an appreciable effect on the quantity of Si-O-Ti bonds. The interpretation of the XRD pattern allows one to explain the increase in the crystallite size of rutile TiO 2 by a decreased quantity of Si-O-Ti bonds.