Tetrabutyl-ammonium and -phosphonium montmorillonites were treated with HCl. Bu4P-S was slightly more susceptible to decomposition in HCl than Bu4N-S. TG and IR of evolved gasses showed higher thermal stability of Bu4P-S than Bu4N-S. Surfactants present on acid-treated samples were released at higher temperature. Variable temperature NIR spectra of solids proved higher stability of Bu4P-S.