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28 Chapter 5. Electrochemical Studies of Non-Aqueous-based CO2 Reduction below focuses on characterizing both reactions in solvents of interest (MeCN, ionic liquids) and conditions relevant to Mars operation. 5.2 Experimental Approach CO2 reduction (Process A) and O2-evolution (Process B) reactions were evaluated separately using pressurized stainless steel Swagelok cells fitted with pressure sensors (see Figure 5.1 for their configuration). All manipulations were carried out under anhydrous conditions, using anhydrous materials. Coated electrodes were prepared at JPL or obtained from commercial partners. Mg metal, magnesium triflate (Mg(OTf)2), lithium carbonate, sodium carbonate, cesium carbonate, trimethylneo-pentylammonium fluoride, lithium peroxide, tetrabutylammonium hexafluorophosphate, acetonitrile (MeCN) and N,N’-dimethylacetamide (DMA) were supplied by Aldrich. 1-Ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium triflate, 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, butyltrimethylammonium bis(trifluoromethylsulfonyl)imide (BTMA-TFSI), diethylmethylammonium triflate (DEMA-OTf), and choline bis(trifluoromethylsulfonyl)imide ionic liquids were supplied by Iolitec. Mn(6,6’- dimesityl-2,2’-bipyridine)(CO)3(MeCN)(OTf) catalyst was supplied by the Kubiak group at UCSD. Differential electrochemical mass spectrometry (DEMS) was performed using an SRS Residual Gas Analyzer connected to a Pfeiffer turbomolecular pump, for which access was generously provided by Liox Power, Pasadena, CA. Electrochemical experiments were carried out using a BioLogic system. Experiments were carried out in a Tenney thermal chamber (Process A) or in a Binder oven at 30◦C (Process B), after at least 2 hours of thermal equilibration. Figure 5.1: Stainless steel Swagelok cells fitted with pressure sensors (left) used for electrochem- ical experiments, shown with cell components for CO2 reduction (right). For Process A, the electrodes used were either Pt/Teflonized carbon paper or Mg metal. The electrolyte (100 μL per cell) comprised 0.1 M Mg(OTf)2 and 0.5 mM Mn(6,6’-dimesityl- 2,2’-bipyridine)(CO)3(MeCN)(OTf) catalyst dissolved in MeCN/0.1 M tetrabutylammoniumPDF Image | ISRU Challenge Production of O2 and Fuel from CO2
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