Zirconium hexacyanoferrate (ZrHCF), a new Prussian blue analog with electroactivity, was immobilized on the surface of a gold electrode by electrochemical sweeps and characterized by infrared spectroscopy, X-ray photoelectron energy and voltammetry. The results show that the electroactive white deposit attached to the gold substrate is actually composed of zirconium hexacyanoferrate(II). The electrochemical behavior of the ZrHCF modified electrode was studied by cyclic voltammetry; the peak current is proportional to the sweep rate up to 200 mV s(-1). Under optimized conditions the peak-to-peak separation is only 3 mV, showing the characteristics of the surface reaction. Ion effects of the supporting electrolyte suggest that cations have a considerable effect on the electrochemical behavior of the modified electrode.