The properties of polyacryloylacetone (PAA) monolayers adsorbed at dichloromethane-water (DCM/W) interfaces were investigated by using the dynamic pendant drop method and a new rheological approach. The results were compared with those obtained at the air-water (A/W) interface. The role of the two interfaces on the interfacial organization of enolic units and the formation of tridimensional structures was discussed. The adsorption kinetics of Cu2+ ions on PAA monolayers leading to metal-polymer complex formation were followed. The observed large difference in the kinetic rates at the two interfaces is probably related to the different interfacial organization of the enolic units.