In this work, the formation of Langmuir monolayers of 12,13-bis(hydroxyimino)-11,14-diazatetracosane (DTC), 14,15-bis(hydroxyimino)13,16-dithiaoctacosane (DOC) and 14,15-bis(hydroxyimino)-13-thiaoctacosane (TOC) molecules at the air-water interface, surface pressure-area (pi-A) isotherm and stability of these monolayers were investigated as a function of pH of subphase. We also studied the monolayer properties of these ligands spread on a subphase containing different metal ions. It is showed that the metal ion concentration, complexation time and counter ions play important roles for the complexation behaviour of these ligands. The optimal conditions for the formation of stable, metal complex containing monolayers and transfer as their Langmuir-Blodgett (LB) films were determined. (c) 2005 Elsevier B.V. All rights reserved.