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In this study, metal oxides nanoparticles heterogeneous photocatalysts prepared by coprecipitation and ultrasonic techniques were used for diesel desulfurization. They were characterized by scanning electron microscope, powder X-ray diffraction, energy dispersive analysis, diffused reflectance spectra, photoluminescence analysis and BET surface area. The surface area of catalyst B is larger than catalyst A confirming its higher reactivity. X-ray reflectance spectroscopy was used to analyze the sulfur contents in feed. Thiophene was used as a model fuel to evaluate the photocatalytic activity of catalysts A and B. Using the Scherrer equation, sharp and intense signals suggesting their higher degrees of crystallinity, with average crystal sizes for ZnO, Bi2O3, catalysts A and B, respectively; of 18, 14.3, 29.7, and 23.8 nm. The operational parameters of the desulfurization process were optimized and have been studied and the maximum sulfur removal was achieved via a further solvent extraction step. A diesel fuel with a 24 and 19 ppm sulfur content and hence a total sulfur removal of 94.6% and 95.7% was acquired for catalysts A and B, respectively (sulfur compounds concentration in diesel fuel feedstock was 450 ppm). These findings demonstrated that photocatalysts A and B are good and effective catalysts for desulfurization of diesel fuel. [ABSTRACT FROM AUTHOR]