Graphite was intercalated with NiCl2 and FeCl3 (8:2) by heating at 450 degrees C for 72 h. The intercalated graphite (3:1) was studied for chem. and electrochem. exfoliation under treatment with H2O2 and H-2 sorption/desorption, resp. The exfoliation resulted in an increase in electrochem. activity of intercalated graphite electrodes. Their cathodic polarization resulted in a sec. exfoliation by action of absorbed H2 which underwent desorption during the subsequent anodic polarization.