Abstract Due to the considerable risks of heavy metal to the humans' health, it is very necessary to provide an efficient determination technique. The present research procured a modified carbon paste electrode (CPE) with Eu3+ doped NiO and utilized it for sensitively detecting the Pb (II) and Cd (II). In addition, electrochemical behavior of Pb (II) and Cd (II) on the introduced electrode have been investigated via square wave anodic stripping voltammetry (SWASV). Moreover, experimental variables like modifier%, pH of the buffer solution, deposition time and potential have been optimized. Based on optimal condition, the linear range was 0.8 to 165 μg /L and limit of detection (LOD) was calculated 0.1 and 0.4 μg/L for Pb (II) and Cd (II), respectively. Therefore, analyzing multiple real samples like tap water, apple juice, raw milk, honey and black tea, demonstrated appropriateness, sensitivity, and accuracy of the mentioned technique to determine Pb (II) and Cd (II) in diverse real samples with good recovery.