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Here, we prepared two kinds of nanocomposites (MCT#1 and MCT#2) involving MWCNTs and TiO2 nanoparticles. The characterisation of the samples is carried out based on FTIR spectroscopy and TEM. The Ti-O groups that is attributed to the TiO2 nanoparticles can be confirmed according to the FTIR analysis. TEM images show that the average particle size of TiO2 nanoparticles in prepare MCT#1 and MCT#2 is equal to 13 nm and 15 nm, respectively. The influences of nanocomposites weight fraction and illumination time are investigated on the decomposition rate of methyl orange (MO) as pollutant. The photocatalytic results exhibit that the decomposition rate of MO is increased with respect to the weight fraction and illumination time. Meanwhile, higher decomposition rate can be observed using MCT#2 compared to MCT#1. Statistical analysis of the results based on Duncan's multiple range test at α = 0.05 reveals that all of the applied levels of the factors have a significant effect on the decomposition rate. The response surface results confirm that the effect of illumination time is high that that of weight fraction of MCT#1 and MCT#2. [ABSTRACT FROM AUTHOR]