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In this work seven novel demulsifiers were prepared; the first four compounds were based on maleic anhydride-oleic acid adduct MO. The first of them is hexaglycerol MO (HGMO) and other three different compounds are ethoxylated MO adduct,(n 5 30, 45, and 60), namily; E(30)MO; E(45)MO, and E(60)MO. The later three demulsifiers were based on polyethylene-polypropylene oxide co-polymer and maleic anhydride-oleic acid adduct at different molecular weights of copolymer (BP), (8 3 10 3 , 12 3 10 3 , and 20 3 10 3 ), namily; MOBP8, MOBP12, and MOBP20. The surface tension (g) at 30, 40, 50, 608 8 8 8 8C of their solutions was measured. The critical micelle concentration (CMC) of theses demulsifiers was determined by the surface tension and the dynamic light scattering. From the obtained data, it was found that, the CMC values of the two methods are nearly closed. Further calculations were made to obtain the surface active properties and thermodynamic parameters of micellization and adsorption. The demulsification efficiency of these demulsifiers was determined on the basis of the time taken for complete water separation of emulsion. The discrepancies of efficiencies were discussed on the light of the chemical structure, the surface and thermodynamic properties.