The influence of preparation methods on structural and catalytic properties of the Fe2O3-Cr2O3-CuO catalyst during the high-temperature water-gas shift reaction was determined. The prepared samples were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller method (BET), and temperature-programmed reduction (TPR). The results revealed that the type of coprecipitation, i.e., simple, inverse, and differential, had a significant effect on both structural and catalytic properties. The catalyst prepared by the simple precipitation method exhibited higher activity than the catalysts generated by inverse and differential coprecipitation and the commercial catalyst. The types of precipitation agent and iron and chromium precursors were found to have a significant impact on the structural and catalytic features.