A new material of cotton fiber/Al 2 O 3 / SiPy þ Cl À , COTALPy, was prepared containing on its surface the polymer silsesquioxane 3-n-propylpyridinium chloride strongly adhered. This new composite based on long fibers of natural cotton is chemically stable and had its adsorption properties studied. The COTALPy presented a maximum ionic exchange capacity of 0.85 mmol g À1 by potentiometric titulation. The adsorption isotherms of CuCl 2 , ZnCl 2 , CdCl 2 , NiCl 2 , and FeCl 2 in ethanol solutions were determined for each metal. The adsorption process was studied and data compared with the Langmuir model. The maximum adsorption capacities (in mmol g