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Heavy metals do great harm to human body. Usually it is concluded that Pb and Cd ion selective electrodes are not abele be used simultaneously because of international interference of Pb2+ and Cd2+ ion. In this paper, multiple linear regression analysis method is proposed for the determination of Pb2+ and Cd2+ ion based on the two ion selective electrodes. Meanwhile, the regression equations of Pb2+ ion and Cd2+ ion are established separately. The regression coefficient was R2=0.9999 and the experimental data were fitted well. This measure method is simply and the experimental results are satisfying.