Ag NTf2 salt, identical in composition to the previously described solution, was introduced into the reference capillary. This was followed by the recording of a single linear sweep voltammogram (LSV) using a three-electrode configuration. The setup involved an Ag wire as the pseudo-reference electrode, graphite as the counter electrode, and the working electrode being the Au foil (Figure 2.6b). Importantly, a four-electrode connection was utilized to measure the potentials of both the working electrode and the counter electrode relative to Ag/Ag+. Subsequently, the Ag solution was withdrawn from the capillary to minimize the potential impact of Ag-imidazolium deposition on the working electrode. In the third step, the potential recorded versus Ag/Ag+ in the second step is contrasted with the potential recorded versus graphite in the first step (Figure 2.7a). This comparison allows for the alignment of the previously recorded potential versus graphite with respect to the Ag/Ag+ reference using the following equation: This alignment step ensures the accurate calibration of the potential recorded versus graphite as a function of potential ( with respect to the Ag/Ag+ reference, enabling reliable comparison and analysis of the electrochemical data. Finally, in the last step, the cell potential recorded in the three-electrode configuration was compared to that of the two-electrode configuration to examine the overlap between the two profiles obtained in steps 1 and 2 (Figure 2.7b). This comparison aimed to ensure the absence of any artifacts or anomalous effects arising from the presence of the Ag salt reference solution. By assessing the consistency and agreement between the cell potentials obtained from both configurations, the reliability and validity of the experimental data were verified, further confirming the effectiveness of the developed protocol in mitigating potential issues associated with reductive Ag deposition during electrolysis experiments. Furthermore, Figure 2.7c presents the scanning electron microscopy (SEM) results along with energy-dispersive X-ray spectroscopy (EDX) analysis of the Au foil used as
RkJQdWJsaXNoZXIy MTk4NDMw