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C 2020, 6, x FOR PEER REVIEW 6 of 21 C 2020, 6, 34 6 of 21 2.2.3. Determination of CO2 Concentration 2.2.3. Determination of CO2 Concentration A thermal mass flowmeter of modular construction with a ‘laboratory style’ pc-board housing A®thermal mass flowmeter of modular construction with a ‘laboratory style’ pc-board housing (EL-FLOW Mass Flow Meter/Controller) from Bronkhorst Hi-Tec (Ruurlo, Netherlands), was used to (EL-FLOW® Mass Flow Meter/Controller) from Bronkhorst Hi-Tec (Ruurlo, Netherlands), was used monitor the CO2 concentrations in the solution. Control valves were integrated to measure and control to monitor the CO2 concentrations in the solution. Control valves were integrated to measure and a gas flow from the lowest range of 0.2 up to 10 mL·min−1. control a gas flow from the lowest range of 0.2 up to 10 mL·min−1. 3. Results and Discussion 3. Results and Discussion 3.1. Electrochemical Behaviour of Nitro-Compounds under Inert Atmposphere 3.1. Electrochemical Behaviour of Nitro-Compounds under Inert Atmposphere The electrochemical behavior of a sequence of four p-nitro-compounds was studied in different The electrochemical behavior of a sequence of four p-nitro-compounds was studied in different solvents, and electrodes under inert atmosphere. solvents, and electrodes under inert atmosphere. Cyclic voltammograms (CVs) of a 3–10 mL solution of 1-4 in DMF using 0.10 M Cyclic voltammograms (CVs) of a 3–10 mL solution of 1-4 in DMF using 0.10 M of of tetrabutylammonium tetrafluoroborate (TBA BF4), and 1-methyl-1-ethylimidazolium tetrabutylammonium tetrafluoroborate (TBA BF4), and 1-methyl-1-ethylimidazolium bis(trifluoro- bis(trifluoro-methanesulfonyl)imide (EMIM TFSI) were recorded at different scan rates (from 0.10 a methanesulfonyl)imide (EMIM TFSI) were recorded at different scan rates (from 0.10 a 1.0 V s−1) using 1.0 V s−1) using glassy carbon (C, blue lines), Ag (black lines) and copper, Cu (red lines) as working glassy carbon (C, blue lines), Ag (black lines) and copper, Cu (red lines) as working electrodes under electrodes under a N2 atmosphere (Figure 2). Focusing in the first wave, the same general trend was a N2 atmosphere (Figure 2). Focusing in the first wave, the same general trend was observed in all observed in all electrodes and both solvents. Compounds 1-3 shows a monoelectronic fast reversible electrodes and both solvents. Compounds 1-3 shows a monoelectronic fast reversible electron electron transfer, whereas compound 4 has an irreversible electron transfer (Table 1). transfer, whereas compound 4 has an irreversible electron transfer (Table 1). Figure 2. Cyclic voltammetry of 10 mM p-nitro compounds 1-4 with Ag (black line), Cu (red line) and C (blue line), under nitrogen atmosphere. Scan rate: 0.5 V·s−1. Solution of DMF/0.1M TBA BF4 (left) and solution of 3 mL EMIM TFSI (right).PDF Image | Electrochemical Tuning of CO2 Reactivity in Ionic Liquids
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