<span lang="EN-US">Glassy carbon electrode (GCE) modified by 2-mercaptobenzothiazole (MBT), mesoporous silica (Meso) and bismuth was developed to determine Cd(II) and Pb(II) simultaneously by square wave anodic stripping voltammetry (SWASV). In-situ preparation was found to work best in optimum conditions of acetate buffer pH 6, accumulation potential of <br /> -1.1 V, deposition time of 300 s and scan rate of 200 mV/s. SW peaks revealed the linear range of 5-50 µg/L Cd(II) and 5-50 µg/L Pb(II). LOD and LOQ for Cd(II) and Pb(II) were determined as 0.56, 0.80, 1.87 and 2.66 µg/L, respectively. The interaction of metals with bismuth and MBT, as well as higher surface area due to mesoporous silica, support beneficial performance of the modified electrode. Insignificant interferences from other regularly present metal ions were found. With SRM1640 standard, the SWASV results are found comparable to those obtained by inductive coupled plasma optical emission spectrometry (ICP-OES). The method was used to analyze the metals in tap water by standard addition method with the satisfactory recovery of 100.7 % for Cd(II) and 100.8 % for Pb(II).</span>