The layer-by-layer (LbL) assembly of polyelectrolytes is an excellent method for the fabrication of functional ultra-thin multilayers. The functional properties of the film depend on the nature of the polyelectrolyte. Thus, to develop new applications for LbL multilayer films. it is first necessary to synthesize new functional polyelectrolytes. We have prepared a novel, optically active polyelectrolyte. an L-phenylalanine derivative of poly(ethylene-alt-maleic anhydride) (PEMA-L-Phe), via ring-opening of the succinic anhydride unit. We have characterized this polyelectrolyte by FTIR, UV-Vis spectroscopy, (1)H NMR, and polarimetric analysis. The specific rotatory power, [alpha](D), of the chiral polymer was -101.3 degrees, greater than that Of L-phenylalanine (-35.1 degrees). We fabricated an ultra-thin film of (PEMA-L-Phe)/poly(allylamine hydrochloride) (PAH) with the electrostatic LbL self-assembly method. The assembly of this ultra-thin film was monitored with a UV-Vis spectrophotometer. The results indicate that the absorbance of the multilayer at 210 nm grows exponentially with the number of bilayers, and that the mass of each bilayer is 1.263 times that of the previous bilayer. This multilayer has potential applications in chiral identification and separation. (C) 2009 Elsevier Ltd. All rights reserved.