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In this study, MFe 2 O 4 (M= Zn, Cu, Co and Ni) nanoparticles were prepared to use a modified chemistry co-precipitation methods followed by annealing, respectively.Then, Ag/MFe 2 O 4 nanoparticles were synthesised via a wetness impregnation method. The structural properties of the samples were systematically investigated by XRD, SEM, TEM, EDX, DRS, BET, SPV and FT-IR techniques. The photocatalytic performances of the prepared MFe 2 O 4 and Ag/MFe 2 O 4 samples were comparatively studied by the photodegradation of 4-Chlorophenol under xenon lamp illumination in FTIR reaction cell. The photodegradation rate of 4-Chlorophenol in photocatalytic process was 90% on Ag/CoFe 2 O 4 sample. The cheap cost and easy synthesized process of the photocatalysts indicate a better potential for the thermal disposal of chlorophenols pollutants at lower temperatures.