A new amphiphilic Schiff base 2-hydroxy-5-nitro-N-benzylidene hexadecylamine (2H5NHDB) has been synthesized and its monolayer properties at the air/water interface have been studied. Surface pressure/molecular area (pi -A) and surface potential/molecular area (DeltaV-A) isotherms have been used to characterize the ligand and its complexation with nickel has been monitored using surface enhanced UV-Vis reflection spectroscopy at the gas/water interface. The complexation leads to either a shift or the appearance of new bands in the spectra. The preferred orientation and organization of the ligand into dimers at the air/water interface helps formation of stable nickel complexes. Sulfidation of the nickel complex (LB film) leads to uniform spherical clusters of nickel sulfide.