Pollution prevention is a major economic and environmental issue in the chemical processing industries. This paper addresses the design of cost-effective recovery systems for vaporous emissions, systems that allow environmentally sound recycling of the recovered components for re-use within the process as a means of pollution prevention. A methodology is proposed to design optimal hybrid systems that involve gas permeation membranes and vapor condensation systems. The design methodology is presented as a mixed-integer, nonlinear program. Based on a fixed structure of the system, a short-cut formulation is derived. Additionally, the incorporation of the system into the emerging mass integration methodology is presented. It is demonstrated, through an industrial case study, that hybrid membrane/condensation systems possess advantages over either separation technique alone.