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The electrochemical pre-treatment method was applied for the activation of glassy carbon electrode for the detection of catechol (CC) and hydroquinone (HQ) by using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques. The influence of concentration, pH and scan rate was studied at nitric acid pre-treated glassy carbon electrode (NAPGCE) for both CC and HQ. The NAPGCE depicts the adsorption controlled process and it exhibits a good limit of detection for CC and HQ was found at 0.99 and 1.2 μM respectively. The suggested electrode exhibited good sensitivity and reliability in the simultaneous electroanalysis of CC and HQ. Moreover, the recovery of CC and HQ was developed by a simple method in tap water.