The differential pulse adsorptive cathodic stripping voltammetry (DP-AdsCSV) employing the hanging mercury drop electrode (HMDE) was used towards the determination of two psychotropic drugs in environmental samples. Voltammetric and experimental conditions to Clonazepam (CLO) and diazepam (DIAZ) were optimized and the methods were in-house validated. Accumulation potentials were À0.3 V to CLO and À0.6 V to DIAZ at 120 s of accumulation time. Pulse amplitude, pulse time and scan rate were 80 mV, 20 ms and 25 mV s
À1to CLO and 100 mV, 20 ms and 40 mV s À1 to DIAZ, respectively. Recovery tests were done in three different concentrations to evaluate methods' accuracy and the results were from 88 AE 6 to 120 AE 13 %. In precision tests, standard deviations were lower than 15 % for both methods. Goods limits of quantification 0.65 and 0.27 mg L À1 to CLO and DIAZ respectively were achieved without pre-concentration steps such as SPE, etc. Voltammetry employing HMDE was first used for the determination of CLO and DIAZ in natural water. Natural samples were spiked and recovery tests confirmed the applicability of the methods developed. Nine samples from Parana state, Brazil, were analyzed and CLO and DIAZ values were below the limits of detection in all samples.