Abstract: In this work, the analysis of copper and nickel in highcalcium geological samples was carried out with inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasmaatomic emission spectrometry (ICPAES). The results indicated that calcium interfered with the determination of copper and nickel. Through the experiments, the interference factors were determined and applied to interference correction. The method has been tested by determination of copper and nickel in geological standard reference materials and the results are in good agreement with certified values with precision of <2%RSD (n=10).