A study has been conducted to determine the effects of flow configuration and reaction conditions on the performance of composite reverse osmosis membranes prepared by plasma polymerization of allylamine over a porous polymer substrate. It was established that superior membranes were obtained by using a gas-flow configuration avoiding direct monomer flow over the substrate. High rejections of NaCl could be attained when the plasma-deposited film was sufficiently thick to bridge all of the pores in the substrate. It was observed that in addition to influencing the rate of polymerization, the conditions used to sustain the plasma also affected the reverse osmosis characteristics of the deposited film. The effects of these conditions and other preparation procedures are discussed. Attempts to use infrared spectroscopy and ESCA to identify the relationship between polymer structure and reverse osmosis performance were not successful. ESCA did prove useful, though, in confirming an earlier postulated hypothesis that degradation of reverse osmosis performance is associated with the hydrolysis of nitrogen-containing structures in the plasma-deposited film.