Abstract: The ferromolybdenum alloy (molybdenum content 55%~65%) was determined by inductively coupled plasma atomic emission spectrometry (ICP-OES), and good linearity was obtained using the single point calibration. The sample was acidified and microwave digestion was carried out, yttrium was added as the internal standard element to reduce the influence of instrument fluctuation and the optimum emission intensity of molybdenum was measured at the analytical line of 202.030 nm. The results showed that the microwave digestion can reduce the dissolution time of the sample to 14% of the weight method, and the relative standard deviation was 0.17%~0.22%. The accuracy of the validation results for standard samples was equaled to that of the gravimetric method, which provides a reference for the ICP-OES method to detect high content components.