A highly electroactive material Mo2[(OAc)2(H2-calix[4]arene)] is used as a neutral carrier for Cd2 +  ions in this paper. The membrane is fabricated by using ionophore [Mo2(OAc)2(H2-calix[4]arene)]:poly(vinyl chloride) (PVC): dibutylphthalate(DBP):sodium tetraphenyl borate (NaTPB) in the ratio of 40:300:470:5 respectively and tetrahydrofuran (THF) used as a solvent. The membrane electrode performed in the concentration range of 9.9 × 10−8–1.0 × 10−1 M (2.34 × 10−5–23.64 mg/mL) having the Nernstian slope of 30.0±1.0 mV and the best detection limit was observed at 9.8 × 10−8 M (2.31 × 10−5 mg/mL). The proposed membrane electrode has the response time of 12 s and a useful working pH range of 1.0–7.0, and used over a period of 10 months and work satisfactorily in the test solution having 30% (v/v) non-aqueous content. Electrode sensor has distinguishable ability for Cd2 +  ion with regard to several alkali, alkaline earth, transition and heavy metal ions. It was used in direct potentiometry as an indicator electrode, in the potentiometric titration of 10−3 M Cd2 +  solution against 10−2 M of ethylenediaminetetraacetic acid (EDTA).

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