A novel approach to fabricate Nafion PFSA resin with polymer polyvinyl alcohol (PVA) into nanofiber membrane, as a functional adsorbent for heavy metal ions had been achieved. Nafion PFSA in N,N-dimethylacetamide (DMAc) was blended with aqueous solution of PVA by sol gel method and fabricated by electrospinning. Electrospun Nafion-PVA mats had exhibited more stability, better mechanical and adsorption properties. These nanofiber membranes possessed adsorption properties based on observed adsorption capacity for Cu (II) 59.1 mg g(-1), Cr (III) 42.5 mg g(-1), Co (II) 24.7 mg g(-1), and As (III) 22.7 mg g(-1) metal ions in an aqueous solution. These nanofiber membranes were characterized by Scanning Electron Microscopy (SEM), High-Resolution Transmission Electron Microscopy (HRTEM) images, Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and X-ray Photoelectron Spectroscopy (XPS) for their morphological, structural and adsorption properties. (C) 2014 Elsevier B.V. All rights reserved.