The construction and performance characteristics of polymeric membrane electrodes based on two newly synthesized macrocyclic ligands 6,7:14,15-Bzo 2-10,11-(4-methylbenzene)-[15]-6,8,12,14-tetraene-9,12-N 2-1,5-O 2 (L 1) and 6,7:14,15-Bzo 2-10,11-(4-methylbenzene)-[15]-6,14-diene-9,12-dimethylacrylate-9,12-N 2-1,5-O 2 (L 2) for the quantification of Zn 2+ ions are described here. Several membranes having different compositions of PVC, plasticizers, ionic additives and ionophores were fabricated and the best response was observed for the membrane having composition L 2:PVC:TBP:NaTPB in the ratio of 4:37:57:2 (w/w; mg). The response characteristics of the membrane based on L 2 were compared with polymeric membrane electrode (PME) as well as with coated graphite electrode (CGE). The electrode exhibits Nernstian slope for Zn 2+ ions with limits of detection of 3.3 × 10 −7 mol L −1 for PME and 7.9 × 10 −8 mol L −1 for CGE with response time of 12 s and 10 s for PME and CGE respectively. Furthermore, the electrodes generated constant potentials in the pH range of 3.0–8.0 for PME and 2.5–9.0 for CGE. The practical utility of the CGE has been demonstrated by its usage as an indicator electrode in potentiometric titration of EDTA with Zn 2+ ion solution. The high selectivity of CGE also permits their use in the determination of Zn 2+ ions in water, biological, milk and tea samples.