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While recording the voltammograms of [Fe(CN)6]3– and [Fe(CN)6]4– shown in Figure 4.5 and 4.6, the current was simultaneously recorded on a gold ring WE at a constant potential. These results are presented in Figure C.2 and C.3 in Appendix C and in both cases show collection efficiencies higher than the theoretical value of 38.3%. The discrepancy could be caused by the gold ring not being a perfectly flat surface and therefore achieving higher current densities, or by parts of the GC disk surface being blocked, leading to lower current densities. Lastly, a bulk electrolysis experiment was conducted on a solution of 50mL 10mM [Fe(CN)6]4– dissolved in 1M KOH, equalling a theoretical capacity of 13.4mAh. The solution was cycled galvanostatically at ±25 mA between 0.19 V and 0.84 V vs. SHE, with each half-cycle followed by a potentiostatic hold at the limit until the current had dropped to 6 mA during charge and 1 mA during discharge. These cut-off currents were chosen based on the stabilisation currents observed during the first cycle. The results are presented as curves of potential against capacity in Figure 4.8. The 10 recorded cycles overlap closely and show no signs of degradation, reaching the theoretical capacity on all 10 cycles. These results give an initial indication that the ferri-/ferrocyanide couple can be cycled in a stable manner in alkaline media. The cycling stability was later tested in a symmetric single cell configuration closer to the conditions where the redox couple is used as a posolyte material; these results are presented in Chapter 5. Figure 4.8: Bulk electrolysis of 50 mL 10 mM [Fe(CN)6 ]4 – in 1 M KOH recorded on a carbon mesh WE. The solution was cycled galvanostatically at ±25 mA with a potentio- static hold at the potential limit after each half-cycle. The insets show the curves offset by 10 mV from each other to ease comparison (the Cycle 1 curves are unchanged). 4.2. Results and Discussion 53PDF Image | Organic Redox Flow Batteries 2023
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