In this work we have studied the hydrolysis of titanium tetrabutoxide (TTB) in butyl alcohol. The hydrolysis was carried out by adding H2O for a molar ratio water/alkoxide of 4. The hydrolysis has been followed by FT-IR spectroscopy, and the evolution of the Ti-O-C bands of the TTB molecule have been analysed. These bands are located at 1130, 1100 and 1039 cm−1and their intensities decrease with the hydrolysis time. However, these bands do not disappear for several days of hydrolysis confirming the difficulty to obtain a completely hydrolysed TTB molecule. Two IR bands have been assigned to Ti-OH groups and adsorbed H2O molecules. These bands appear at 3660 and 3525 cm−1respectively and they are firstly observed when a white precipitate appears in the solution. This work shows that this study can be rapidly carried out by FT-IR spectroscopy and can also be applied to the well-established sol-gel process.