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The orthogonal perovskite EuFe0.9Co0.1O3 oxides with uniform particle size distribution were prepared by a sol–gel method. The samples were calcined at the different temperatures and the results showed that the mean grain size increased from 31 to 38 nm when the calcinations temperature increased from 600 to 900 °C. The investigation of sensing properties exhibited that the sensor based on EuFe0.9Co0.1O3 calcined at 800 °C has good gas sensing properties to acetone gas at the operating temperature of 280 °C.