Characterization of home-made silver sulphide based iodide selective electrode

Abstract

Polycrystalline silver sulphide/silver iodide ion selective electrodes (ISEs) with four different compositions, 9:1, 2:1, 1:1, 1:9 Ag 2S–AgI mole ratios, have been fabricated in the laboratory and characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). X-ray diffraction studies show the presence of Ag 3SI, Ag 2S and AgI crystalline phases in the electrode material. The electrode surfaces have been found to become smoother and lustrous with increasing percentage of silver sulphide in silver iodide. ISE 1:1, ISE 2:1 and ISE 9:1 all responded in Nernstian manner with slopes of about 60 mV/decade change in iodide ion concentration in the linear range of 1 × 10 −1 to 1 × 10 −6 M while ISE 1:9 showed sub-Nernstian behavior with slope of about 45 mV up to the concentration 1 × 10 −5 M. Two capacitive loops, one corresponding to the charge transfer process at metal electrode and the back contact and a second loop corresponding to the charge transfer process at membrane–electrolyte interface have been observed at high and low frequency ranges, respectively. Mott–Schottky analysis shows that the materials are n-type semiconductors with donor defect concentrations in the range of 5.1 × 10 14 to 2.4 × 10 19/cm 3.