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International audienceNanoparticles of TiO2 crystallizing as anatase and TiO2(B) phases with different ratios were synthesized by a three step treatment. including an initial reflux process in highly alkaline medium. For the first time, the ratio of each variety has been quantified by analysing the galvanostatic curves during the lithium electrochemical insertion. The weight percentage of TiO2(B) reaches 95% (110 m(2) g(-1) specific surface area). In order to get quantitative information based on the ratios deduced from electrochemistry, the same TiO2 samples have also been investigated by Raman spectroscopy. This technique shows a sensitivity seven times higher for anatase than TiO2(B) detection compared to electrochemical method. The equation deduced from Raman refinement and electrochemical quantification permits, for the first time, to quantify the anatase/TiO2(B) ratio simply by using Raman spectroscopy