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eDAQ was used. A list of the reference potentials vs. SHE of these electrodes is given in Table A.2 in Appendix A. Solutions were purged with nitrogen or argon for 15 min before starting measurements. CV was usually carried out at a potential scan rate of 50 mV s−1, or in a range from 50–500 mV s−1 when a Randles-Ševčík analysis was carried out. The voltammograms were recorded on either a CH Instruments CHI760E bipotentiostat or a BioLogic SP-200 potentiostat and will be presented versus the SHE. For voltammetry experiments with RDEs, the setup consisted of an RDE glass vessel, a 5.0 mm or 5.5 mm diameter GC disk shrouded in PEEK from Pine Research Instrumen- tation as WE, and counter and reference electrodes as described for the experiments with stationary WEs. In the cases where RRDE voltammetry was carried out, a GC disk/gold ring shrouded in PEEK from Pine Research Instrumentation was used (5.5 mm diameter GC disk, 6.5 mm inner and 8.5 mm outer diameter gold ring). The solutions were purged with nitrogen or argon for 30min before starting measurements. A gas-purged bearing assembly from Pine Research Instrumentation was added to the setup when recording voltammetry on DBEAQ, as the oxygen-sensitivity of the compound [24] necessitates ex- tra oxygen shielding. Linear sweep voltammetry (LSV) was performed at 5 mV s−1 with the WE rotated at speeds ranging from 100–2500 rpm controlled by a Pine Research In- strumentation MSR Rotator. The voltammograms were recorded on a CH Instruments CHI760E bipotentiostat and will be presented versus the SHE. Bulk electrolysis was carried out in a 100 mL glass cell fitted with a PTFE cap, a carbon mesh WE, a Ag/AgCl RE with 3 M NaCl filling solution, and a platinum wire CE. The CE was separated from the bulk solution by a glass vial fitted with a ceramic junction and filled with blank supporting electrolyte solution. The cell was filled with approximately 50 mL solution, which was degassed for 30 min before starting measurements. The measurements were carried out galvanostatically on a BioLogic SP-200 potentiostat. 4.2 Results and Discussion The experimental results obtained from three-electrode configurations of stationary and rotating electrodes are presented and discussed in the following. To give an initial com- parison of the molecular electrochemistry of the investigated compounds, a cyclic voltam- mogram recorded for each is presented in Figure 4.2. The last voltammogram of a series of two or three cycles is shown, grouped into four subplots after the structure of the parent molecule, and normalised to an electron concentration of 5 mM. Electron concentration here means the molar concentration multiplied by the number of electrons a compound was expected to exchange. The four subplots of Figure 4.2 are furthermore shown with the same potential range to facilitate comparison of the redox potentials. The voltam- mograms were recorded with mainly GC as the WE material over a range of pH values (0, 7, 12, and 14), which was selected depending on the expected solubility and stability of the materials in different supporting electrolyte systems. In some cases, CV was also conducted on a gold WE to study the behaviour on another WE material. The remaining results are divided into subsections corresponding to each of the investi- gated compounds, where the cyclic voltammograms will also be described in more detail. The redox potential (in the form of the half-wave potential) determined from CV and diffusion and kinetic parameters obtained from the various experiments are summarised 4.2. Results and Discussion 47PDF Image | Organic Redox Flow Batteries 2023
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