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Chromium hexacyanoferrate (CrHCF) modified glassy carbon electrode (GC) indifferent electrolytes was studied by cyclic voltammetry and in situ FTIR spectroelectrochemistry.The results indicate that the behavior of CrHCF film can be understood in term of two structures:Cr1/3Cr(III)Fe(II)(CN)6 and MCr(III)Fe(II)(CN)6. Besides, the film exists in amorphous state: theouter layer is porous film, while the inner layer is relatively compact. According to theelectrochemical reaction of CrHCF, the lattice can contract and expand with the cations’ diffusion.