Objectives: In this study, the polarographic behaviour of methimazole was studied using cyclic, square wave and differential pulse polarographic methods. Methods: The influence of several variables (including nature of the buffer, concentration, scan rate, drop size, etc.) was examined in square wave and differential pulse polarographic methods for methimazole. The best square wave and differential pulse polarographic responses were obtained in 0.1 M sulfuric acid. The peak currents were measured with a static mercury drop electrode at 0.10 V versus Ag/AgCl. Results: The linearity was established over the concentration range of 5-80 mg/mLfor both methods in supporting electrolyte and human serum. The methods were validated and applied to the determination of methimazole in a commercial tablet. There was no significant differences between the results obtained by square wave and differential pulse polarographic methods. Square wave and differential pulse polarographic methods are also available and applicable for the determination of mentioned substance in human serum. No electroactive interferences from the endogenous substances were found in the serum samples. Mean recovery was 99.9%. Conclusion: They were concluded that the developed methods were accurate, sensitive, precise, reproducible and useful for the quality control of methimazole in pharmaceuticals and spiked serum.