The paper deals wi th the synthesis of ZnCl2-Cr2O3-H2SO4-graphite bi-intercalation compound (ZnCl2-CrO3-H2SO4-GBC). For observing the concentration profiles of intercalates in both ZnCl2-GIC and ZnCl2-CrO3-GBC the energy dispersive X-ray (EDX) analysis coupled with the scanning electron microscopy (SEM) were used. The X-ray diffraction (XRD) analysis and the cyclic voltammetric (CV) measurements were used to investigate the transformation of the starting ZnCl2-GIC to the ternary ZnCl2-CrO3-GIC followed by the successive electrochemical intercalation of H2SO4 resulting in the quaternary ZnCl2-CrO3-H2SO4-GBC. The present results argue for the formation of co-intercalation domains embedded in the lattice of bi-intercalation compound.