SynopsisCellulose acetate membranes prepared from latexes containing sodium dodecyl sulfate as a stabilizer were found to undergo phase separation. This phenomenon was studied by different techniques including autoradiography, optical and scanning electron microscopy, mechanical testing, and liquid water permeation. The concentration of sodium dodecyl sulfate in the dry membranes was found essential in controlling their structure and properties, as well as the nature and amount of plasticizer incorporated in the latex system. The method of preparation and the drying duration were also relevant. Depending on whether f i l m s were produced by casting or spraying, tensile and permeation values exhibited quite different responses to variations of the sodium dodecyl sulfate content. In Paper 11, a thermodynamic framework is proposed that accounts for the redistribution of sodium dodecyl sulfate into small islets, and thus for phase separation.