Fourier Transform Infrared (FTIR) grazing angle (GAIR) and Horizontal Attenuated Total Reflectance (HATR) techniques were used to characterize Langmuir-Blodgett (LB) films of 12,13-bis(hydroxyimino)-11,14-diazatetracosane (DTC) deposited on an aluminium plated substrate. The LB films of DTC were prepared successfully by transferring onto the solid substrate. The molecular structure of LB films was investigated by comparing the GAIR and HATR spectra. The results suggest that the alkyl chains in DTC are nearly in all-trans conformational state and the alkyl chain tilt, which is the angle between the axis which bisects the C-C bonds and the surface normal, is getting large, when the numbers of monolayer are increased. The splitting of the bands due to the methylene scissoring mode indicates that in LB films of DTC alkyl chains are packed in either an orthorhombic or a monoclinic structure with an orthorhombic subcell containing two mutually orthogonal molecules. (C) 2006 Elsevier B.V. All rights reserved.