This work was undertaken in order to develop a convenient and reliable method for the determination of phthalate esters in propellants. The method described is based upon a titanous chloride reduction of nitroesters and nitroaromatic bodies, which allows a separation of phthalate esters, by a petroleum ether extraction, and their volumetric determination.This method has been applied to the determination of dimethyl phthalate, diethyl phthalate, dibutyl phthalate, diamyl phthalate, and diphenyl phthalate, in the presence of nitroglycerin, dinitro toluene, dipheny lamine, ethyl centralite, and ethyl acetate.