AbstractHydrolytic exchange was performed experimentally on four smectitic clays to evaluate the extent of clay alteration induced by this process and the associated ‘auto-transformation’ of H⁺ clays. Clay samples were Na-saturated and submitted to 10, 50 and 100 wetting-drying (WD) cycles and characterized after treatment using X-ray diffraction (XRD), infrared spectroscopy (FTIR) and cation exchange capacity analysis. Evidence for hydrolytic exchange was given by increasing amounts of exchangeable Mg²⁺ and precipitation of Na soluble salts for samples subjected to 100 WD cycles. Results indicated a decrease in the interlayer charge after 10 WD cycles but no further decrease was observed after 50 and 100 WD cycles. For one sample, XRD data indicated a decrease in the proportion of the smectite phase and a relative increase in the concentration of illite-smectite mixed layers also present in the sample. The results suggested that the reaction induces first a decrease in the layer charge and then a partial dissolution of some smectite layers.