This research studying the effect of the most important analytical and technical conditions on the voltammetric curves of lead and cadmium in order to choose the optimal conditions for the simultaneous determination of these two elements by Differential pulse anodic stripping voltammetry (DPASV) using Graphite mercury film electrode(GMFE) as a working electrode. The results showed that the optimum analytical conditions were when using Sodium acetate - acetic acid (0.05M) electrolyte, where pH= 4.6, and a concentration (25mg/l) of Hg2+, CCd:CPb ratio up to 1:10 and conversely, and the optimum technical conditions were when applying scanning field from -1200 to -100mV, accumulation potential Eacc= -1200mV, accumulation time tacc= 120sec, speed rate υ= 120mV/sec, and amplitude pulse ΔE= 50mV. The previous conditions gave ideal voltammetric curves, Ip(Cd)= 6.134µA, Ip(Pb)= 4.966µA, Ep(Cd) = -647 mV, Ep(Pb)= -473 mV. The previous conditions were applied on a standard sample and the limit of detection was (Cd) 0.100µg/l, (Pb) 1.000µg/l, retrieval coefficient R%(Cd)= 100.5%, R%(Pb)= 97.2%, standard deviation SD(Cd)= 0.020mg/l, SD(Pb)= 0.021mg/l; Therefore, that shows the accuracy and precision of the method. The validity of the method under its new conditions was examined on a number of environmental samples and showed success and high efficiency.