The preparation of membranes from polymer solutions by the phase inversion method, the immersion—precipitation technique has proved since the beginning of obtaining technological membranes the most versatile and simple possibility to create polymeric membrane nanostructures. Classically, the phase inversion technique involves four essential steps: Preparation of a polymer solution in the desired solvent, the formation of the polymer solution film on a flat support, the immersion of the film in a coagulation bath containing polymer solvents, and membrane conditioning. All phase inversion stages are important for the prepared membrane’s nanostructure and have been studied in detail for more than six decades. In this paper, we explored, through an electrochemical technique, the influence of the contact time with the polymer film’s environment until the introduction into the coagulation bath. The system chosen for membrane preparation is polysulfone-dimethylformamide-aqueous ethanol solution (PSf-DMF-EW). The obtained nanostructured membranes were characterized morphologically and structurally by scanning electron microscopy (SEM) and thermal analysis (TA), and in terms of process performance through water permeation and bovine serum albumin retention (BSA). The membrane characteristics were correlated with the polymeric film exposure time to the environment until the contact with the coagulation bath, following the diagram of the electrochemical parameters provided by the electrochemical technique.