The polarographic and voltammetric behaviors of ［Cd(CHZ)₃］(NO₃)₂ were studied. The results show that optimized conditions are as follows: purging time 300 s,equilibration time 10 s, 30% HCl 2.4 mL, start potential －０．８ V, end potential －0.45 V, voltage step time 0.8 s, scaning rate 7.4 mV·s^－１, peak potential of Cd²⁺ －0.58 V,deviation ±0.05V. And lots of data show that ten times of K⁺、Ni⁺、Zn²⁺ and Fe³⁺ have no effect on the determining results. Furthermore, the voltaic property of deoxidize peak and oxidation peak was studied by using cyclic voltammetry. Experiments indicate that the electrode reaction is not reversible, but adsorptivity on the surface of the electrode exists.