The ion exchange membrane using polysulfone (PSf) and polyether ether ketone (PEEK) as a basic material was prepared to apply in the polymer electrolyte membrane electrolysis (PEME). The sulfonated block copolymer of PSf and poly(phenylene sulfide sulfone) (SPSf-co-PPSS) and the sulfonated PEEK (SPEEK) were blended with tungstophosphoric acid (TPA) to avoid water swelling at elevated temperatures led to decrease in mechanical strength. These prepared ion exchange membranes showed some interesting characteristics including physicochemical stabilities, mechanical and membrane properties. The prepared ion exchange membrane was utilized to prepare the membrane electrode assembly (MEA). MEA consisted of Pt/PEM/Pt was prepared by equilibrium and non-equilibrium impregnation-reduction (I-R) methods. The prepared MEA by non-equilibrium I-R method was used in the PEME unit cell. The cell voltages of the MEA using SPSf-co-PPSS/TPA and SPEEK/TPA membranes were 1.83 V and 1.90 V at 1 A/cm(2) and 80 degrees C, with platinum loadings of 1.12 and 1.01 mg/cm(2), respectively. (c) 2008 Elsevier B.V. All rights reserved.