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The polargraphic behavior of Bi(III)-NOTP complex has been investigated in aqueous solution. It was found that under the conditions of pH 3.0 and of 0.02 mol/L NH4Cl, the Bi(III)-NOTP system gives a sensitive second order derivative wave at (0.340 V(vs SCE), which is proved to be an adsorptive complex wave. The composition of the complex is Bi(III):NOTP. Furthermore, the peak current is linear to the concentration of Bi(III) in the range from 3.0×10(8 to 5.0×10(6 mol/L. Artificial and practical samples have been detected with high sensitivity and receptivity.