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The intercalation of lithium in nanosized TiO₂ has been studied for its application as an electrode for rechargeable Li-ion batteries. In this paper, we use a synthesis process in order to obtain a low-density anatase TiO₂ presenting monocrystalline particles of 7−8 nm. These textural characteristics allow this material to host almost twice as much Li (300 mAh·g⁻¹) than that of a micrometer sized anatase. In this study, in situ X-ray absorption spectroscopy is used to monitor and understand the structural changes that happen upon lithium insertion/removal, leading to a reversible two-phase transition process: TiO₂ (I4₁/amd) → Li-titanate (Imma) → Li₁TiO₂ (I4₁/amd).