The goal of this study was to demonstrate a novel potentiometric technique for the measurement of Cd(II) ion. A new ionophore called [5′‐(ethane‐1,2‐diylbis(sulfanediyl))bis(3‐phenyl‐4H‐1,2,4‐triazol‐4‐amine) (ESPTA)] was prepared and used as an electroactive material in the fabrication of new carbon paste electrode (CPE) for the quantification of Cd(II) ion. The paste was prepared by mixing ESPTA, graphite, graphene, and TCP or o‐NPOE as a plasticizer in different weight percent ratios. The developed electrodes I, II, III, and IV showed divalent Nernstian response of 29.80±0.05, 29.80±0.08, 29.86±±0.04 and 29.75±0.33 mV decade−1 over the concentration ranges of 1.0×10−5–1.0×10−1, 1.0×10−8–1.0×10−1, 1.0×10−6–1.0×10−1 and 1.0×10−7–1.0×10−1 mol L−1 with percentage of (2.65 ESPTA: 66.32 graphite: 31.03 TCP), (2.65 ESPTA: 13.27 graphite : 53.05 graphene : 31.03 TCP), (2.75 ESPTA: 68.68 graphite: 28.57 o‐NPOE) and (2.75 ESPTA: 13.74 graphite : 54.94 graphene : 28.57 o‐NPOE), for electrodes I, II, III, and IV, respectively. In order to improve the performance characteristics of electrodes I, II, III, and IV, response time, the effect of temperature, and pH were examined. The electrodes showed high selectivity for Cd(II) over different mono‐, di‐ or trivalent cations. These modified electrodes were applied for the determination of the concentration of Cd(II) in different real samples like Nido Milk, juice extractions and tap water samples with high percentage recovery. The F‐ and t‐test values showed that there is no statistically significant difference between the results obtained and those from the stated method of inductively coupled plasma. Low standard and relative standard deviation values, good percentage recovery, and modest detection and quantification limitations were all displayed by the electrodes. The outcomes showed the potentiometric method‘s effectiveness in detecting Cd(II) in actual samples and its potential for use in routine analysis.
