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The levels of CO2 emissions generated by the cement industry and the growth in demand for its products have led to a search for ways to reduce these emissions. The use of supplementary cementitious materials has become one of the solutions proposed for this problem. Illite, which is found all over the world, is a possible supplementary cementitious material. Before illite can be used, it must be milled and treated thermally in order to activate it, so that the alkalis (Na+ and K+) are free and available to react. Alkalis in cement participate in deleterious reactions (alkali-silica reaction) or have a beneficial effect (alkaline activation). The alkalis present in the rocks can play an active role in these phenomena, however. In addition, the material could be influenced by the alkaline environment produced by the cement. The current study was aimed at analyzing whether an alkali release occurs and if so, how it is affected when a milled and thermally treated illitic rock is in contact with water or an alkaline solution. The material was characterized by X-ray fluorescence, polarizing microscopy, and X-ray diffraction (XRD). The sample was treated thermally at 300, 600, and 900°C, and the thermal activation was evaluated through XRD, density, and Atterberg limits. The evolution of alkali release was studied by determining the sodium and potassium concentration of contact water obtained by mixing the samples with different pH solutions for various lengths of time. In addition, the calcium concentration was determined. The concentrations of sodium and potassium in the contact water were determined by flame photometry, and of calcium by EDTA (ethylenediaminetetraacetic acid) titration. The results showed that with increasing age, increasing solution pH, and higher treatment temperatures, alkali release occurred and increased, whereas Ca2+ concentration decreased.