A new polymer electrolyte membane for fuel cell has been developed between sulfonated polystyrene (sPS) and polyethylene grafted maleic anhydride (PE-g-MAH). This approach requires a precise sulfonate distribution across sPS backbone. Precise distribution of sulfonate groups in sPS can be achieved by gas-liquid heterogeneous sulphonation. Type of solvents, gas carrier flow rate affect the end products of sPS in term of degree of sulphonation and backbone destruction. Polymer electrolyte membrane fuel cell (PEMFC) prepared using sPS prepared by gas-liquid heterogeneous sulphonation. The membrane shows very good performance. The ion exchange capacity as good as commercial products.