Abstract: In this study, we reported an X-ray fluorescence spectrometric method for the determination of molybdenum in geological samples. Empirical coefficients are used to correct the interference of strontium, uranium and other elements. Segmented calibration curves are used to lead to more precise results. And the influence of sample preparation has been discussed. The method is simple and fast, and a high precision (RSD=7.91%, n=11) with a detection limit of 0.48 μg/g can be obtained, and the test results agree with the chemical value. It is very suitable for the batch measurement of geological samples.