Polyluminol was synthesized from sulfuric acid aqueous solution (1 to 5 mol L-1) containing luminol (0.5 to 10 mmol L-1 ) on platinum electrode by cyclic voltammetry. A systematic investigation was performed on the synthesis parameters, resulting in optimized conditions to obtain polyluminol, which are: (i) 2 mol L-1 H2SO4 aqueous solution; ii) containing 7.5 mmol L-1 of luminol; (iii) using thirty potential cycles; (iv) at 100 mVs(-1) . Preparation parameters and electrosynthesis solutions play important roles in eletropolymerization of polyluminol. In general way, all polyluminol films were electroactives in H2SO4 solution independent of synthesis conditions.