Abstract: This article presents a new method for determining zinc, arsenic and manganese in iron ore samples using X-ray fluorescence spectrometry with pressed-powder pellets. Working curves are established under the best preparation condition for samples and optimum measurement parameters. The results of this method have been compared with the values in the national standard reference for iron ore samples and are consistent with certified values. The relative error of accuracy is ±0.007%, and the relative standard deviation RSD (n=10) of the method is less than 2.80% for all three elements. The reported high precision and accuracy of the experimental results demonstrate that the method is suitable to manufacturing requirements with high accuracy and fast detection.