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An inductively coupled plasma atomic emission spectrometry (ICP - AES) method was developed for the determination of 12 impurity elements (Cd, Mn, Cr, Cu, Fe, Ca, Zn, Al, Co, Nd, Pr and Ce) in nickel plating solution for Nd - Fe - B. The optimum working parameters of the instrument and the analytical spectral lines of each element were determined. By using matrix matching and simple bath dilution, the spectral interference to the elements to be detected caused by a large number of matrix substances in the bath was eliminated. Results showed that the linear relationship of these 12 elements was good, the linear correlation coefficient R > 0.999, the detection limit was 0.005～0.690 μg/mL, the results of experiments of precision and recovery showed that this method had the advantages of simple, rapid and accurate, meeting the requirements of daily detection of impurity elements in Nd - Fe - B nickel plating solution.