The adsorption of acetylacetone on layer silicates containing various cations has been studied by means of infrared spectroscopy, X-ray diffraction, and thermogravimetric analysis. An analysis of several split bands in the region of 1740-1520 cm(-1) was made. The bands were attributed to the interaction of carbonyl with structural hydroxyl and cationic hydroxyl groups and were responsible for the formation of acetylacetonate complexes between enolic or anionic acetylacetone and metal cations in the silicate layers.