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A metal‐organic framework MIL‐53(Fe) was successfully synthesized by a simple hydrothermal method. A synthesized MIL‐53(Fe) sample was characterized, and results indicated that the formed MIL‐53(Fe) was a single phase with small particle size of 0.8 μm and homogeneous particle size distribution was obtained. The synthesized MIL‐53(Fe) has been used to modify a glassy carbon electrode (GCE) by a drop‐casting technique. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements of the MIL‐53(Fe)‐modified GCE showed that the MIL‐53(Fe) was successfully immobilized onto the GCE electrode surface and the electrochemical behavior of the GCE/MIL‐53(Fe) electrode was stable. In addition, several electrochemical parameters of MIL‐53(Fe)‐modified GCE (GCE/MIL‐53(Fe)) including the heterogeneous standard rate constant (k⁰) and the electrochemically effective …