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The reduction of the nitrobenzene compounds (NBCs) by the catalyzed Fe-Cu process and the relationship between the electrochemical reduction characteristics of NBCs at copper electrode and reduction rate were studied in alkaline medium(pH=11).The catalyzed Fe-Cu process was found more effective on degradation of NBCs compared to Master Builder’s iron. The reduction rate by the catalyzed Fe-Cu process decreased in the following order: nitrobenzene ＞4-chloro-nitrobenzene ≥m-dinitrobenzene ＞4-nitrophenol ≥2,4-dinitrotoluene ＞2-nitrophenol. The reduction rate by Master Builder’s iron decreased in the following order:m-dinitrobenzene ≥4-chloro-nitrobenzene ＞4-nitrophenol ＞2,4-dinitrotoluene ≈nitrobenzene ＞2-nitrophenol. NBCs were reduced directly on the surface of copper rather than by the hydrogen produced at cathode in the catalyzed Fe-Cu process. The reduction was realized by the hydrogen produced at cathode and Fe(OH)2 in Master Builder’s iron. It is an essential difference in reaction mechanisms between these two technologies. For this reason, the reduction by the catalyzed Fe-Cu depended greatly on NBC’s electron withdrawing ability.