The potentiometric response behavior of an electrode, which consists of a non-plasticized carboxyl-modified polyacrylamide polymer (PAA) coupled to benzo-12-crown-4 (PAA–B12C4) to Li+, Mg2+, and Ca2+ in such aprotic solvents as acetonitrile (AN), propylene carbonate (PC), and γ-butyrolactone (GBL), were examined. The electrode showed a Nernstian response to Li+ and Ca2+ in AN, and Li+, Mg2+, and Ca2+ in PC and a near-Nernstian response to Mg2+ in GBL. From the response to Ca2+ it could be confirmed that the membrane potential was mainly established at the polymer membrane–solution interface. The electrode was applied to a study of their complexing with such other basic aprotic solvent molecules (D) as N,N-dimethylformamide, dimethyl sulfoxide, and hexamethylphosphoric triamide. The successive complex formation constants (βi) and Gibbs energies of transfer (ΔGtr(j)) of Li+ in AN and Mg2+ in PC in relation to such D were obtained.
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