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This paper studies the effect of addition of Zn and ultrasound-assisted co-precipitation on Cu-Mn oxide catalysts for the oxidation of CO. Cu-Mn-Zn oxide catalysts were synthesised at different molar ratios and characterised and evaluated for CO oxidation performance. Scanning electron microscopy (SEM) imaging showed that the morphologies and textural properties of the catalysts were markedly affected by the different synthesis conditions, notably the formation of different geometries of various sizes depending on the Zn loading used. Characterisation results also revealed that both the addition of Zn and the use of ultrasound-assisted synthesis improved the dispersion of metal constituents in the mixed oxide phase, evident from the lower peak intensity and smaller crystallite sizes and more dispersed particles as seen in SEM imaging. Gas adsorption results revealed that Zn loading influences the porosity and adsorption capability of the catalyst. Zn-loaded samples exhibited a H3 hysteresis loop, which suggests the presence of slit-like pores. Temperature-programmed reduction results indicate that sonicated samples exhibit improved reduction capabilities which can increase overall catalytic activity. Results showed that Cu/Mn/Zn = 2:1:0.5 displayed the highest activity, showing 76.0% and 82.8% for CO and SO2 at 130 °C, respectively. This work has confirmed that the addition of 0.5 molar ratio of Zn and the presence of ultrasonic treatment during the catalyst synthesis have improved the overall catalytic performance, while further addition in Zn concentrations resulted in an adverse effect on the catalyst. [ABSTRACT FROM AUTHOR]