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The degradation of methylene blue (MB) in an aqueous solution by nano-metallic particles (NMPs) was studied to evaluate the possibility of applying NMPs to remove MB from the wastewater. Scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS) were used to characterize the synthesized NMPs before and after the reaction. The effects of the NMP dosage, the initial pH, the initial concentration of MB and the amount of H2O2 on the MB degradation outcomes were studied. The highest removal rate of MB was achieved to be 100% with an initial MB concentration of 5 mg/L, followed by 99.6% with an initial concentration of 10 mg/L under the following treatment conditions: dose of NMP of 0.15 g/L, concentration of H2O2-100 mM and a temperature of 25oC. The SEM analysis revealed that the nano particles were not spherical in shape. FTIR spectra shows occurrence of metal oxides on the surfaces of the NMPs. The XPS analyses results represent that Fe, Zn, N, Ca, C and O were occurred on the surfaces of the NMPs. The degradation of MB was suitable for the pseudo-first-order kinetics. KCI Citation Count: 4