An investigation was carried out on ethanol-water separation employing a PSA adsorption cycle with zeolite 3A as the adsorbent. The cycle was operated under the following operating variables: feed flow (2, 4, 6 and 8 L/h), adsorption temperature (200°C) and adsorption pressures (2, 4 and 6 bar). All experimental runs were performed under vacuum of 0.2 bar in the desorption step. The effect of these variables on the enrichment and recovery percentage of the product, on the productivity and on the total cycle time was studied, using the adsorption pressure as a parameter. The results showed that these variables significantly affect the responses of interest. We also studied the influence of such variables as: adsorption pressures, desorption pressures, flow rates and adsorption temperatures (T), on the enrichment, recovery, productivity and on the total cycle time. The data were obtained from operational cycles in a Kahle's system. The experiments were organized by a three level factorial design. The results obtained were compared with from the fitted empirical equations as well as with the corresponding surface responses and all variables showed to be influential. Last, by an optimal combination of the variables was obtained by means of the ridge analysis method and the optimized multi-response method.