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The electrochemical properties of La _9.33 Si _6 O _26 (LSO)–La _0.8 Sr _0.2 Ga _0.8 Mg _0.2 O _2.55 (LSGM) electrolyte composites have been evaluated over NiO and La _0.1 Ca _0.9 MnO _3 (LCM) electrodes using symmetric and asymmetrical cells of NiO/LSO–LSGM/NiO and NiO/LSO–LSGM/LCM, respectively. The Nyquist plot obtained from this study suggested that the new electrolyte system exhibits excellent performance over the NiO and LCM electrodes and shows an ideal Randel cell electrical circuit characteristic in both NiO/LSO–LSGM/NiO and NiO/LSO–LSGM/LCM cells. The area-specific resistance (ASR) and, the activation energy (Ea) of NiO/LSO–LSGM/NiO from the Arrhenius plot are lower than the NiO/LSO–LSGM/LCM, which is 0.30 Ω cm ^−2 and of 0.74 eV vs 0.40 Ω cm ^−2 with Ea of 0.76 eV, respectively.