The synthesis, fabrication, fluorescence and fluorescence quenching behavior of fluorescent polymer, polyacrylic acid-poly (pyrene methanol) (PAA-PM) are reported. The Stern-Volmer plots of the electrospun membranes exhibited good linearity for Fe3+, Hg2+ and DNT and the Stern-Volmer constants K-sv are 4.4 x 10(4) (M-1), 3.5 x 10(4) (M-1) and 2.9 x 10(4) (M-1), respectively. These values are one order of magnitude more than those obtained previously from films made by electrostatic layer-by-layer adsorption of the same polymer.