Abstract: The determinations of rhenium in molybdenum and copper ores were performed by inductively coupled plasmaatomic emission spectrometry (ICP-AES) with sample pretreatment using magnesium oxidesodium nitratehydrogen peroxide. The sample pretreatment parameters and instrument operating conditions were optimized. The detection limit of the method for Re was 0.014 μg/g. The method has been verified by determination of Re in molybdenum ore and copper ore National Standard References and the results are in agreement with certified values with precision of less than 5.00%RSD (n=11).