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The early occurrence of intentional heat treatment of silica rocks has recently become a key element in the discussion about the cultural modernity of prehistoric populations. Lithic vestiges are the only sources that remain of this process and the understanding of the material’s properties and transformations are essential for reconstructing the conditions and parameters applied during heat treatment. Several models of the structural transformations upon heating have been proposed in the current literature. These models are often contradictory and do not account for the most recent structural and mineralogical data on chalcedony. In order to propose a new model, we elaborated an experimental procedure and applied different techniques involving infrared spectroscopy, solid state NMR, X-ray diffraction and electron microscopy. The results show that the major transformation to happen is the loss of silanole (SiOH …