AbstractThe monitoring of different reactions such as the stabilization of the alkoxides with polymerizable organic additives, the building of the inorganic network during the hydrolysis process, and in a same manner, the polymerization of the organic additives, can be of great importance for the development of hybrid materials with improved processability.NIR spectroscopy is a very versatile technique but lacks of specificity. IR and Raman give more interpretative results but are not always easy to run on a process. We used both techniques along with chemometric tools to extract relevant information from our processes. Then 2D correlation allowed to benefit from the specificity of IR and Raman to develop robust NIR methods able to be used on line to control the different steps of the sol-gel process.The hydrolysis of mixed species of titanium containing chloro, isopropoxo and methacrylato ligands will be discussed in terms of mechanism occuring during the sol-gel process.