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In this paper, FTIR spectroscopy using attenuated total reflection (ATR) and KBr pressed disk techniques has been used to characterize sorbed water and HDTMA⁺ in organo-clay. Sorbed water content decreases with the intercalation of HDTMA⁺. With the decrease of the sorbed water content, the position of the ν₂ mode shifts to higher frequency dramatically while the stretching vibration shifts to lower frequency slightly, indicating that H₂O is less strongly hydrogen bonded. This might be resulted from the polarization of H₂O molecules by the changeable cations and HDTMA⁺. FTIR spectra show that both antisymmetric and symmetric CH₂ stretching absorption bands shift to low frequencies with increase of amine concentration within the galleries of montmorillonite, elucidating the increase of ordered conformation. Furthermore, the present study demonstrates that the antisymmetric CH₂ stretching mode is more …