Synthesis of new molybdenum perfluoropinacolate complexes and investigation of CuSn alloys for nitrate reduction
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Fluorinated alkoxide ligands, including perfluoropinacol (H2pinF), have been investigated for their ability to support high oxidation status for 3d transition metals. Molybdenum is a 4d transition metal used for its catalytic effect in nature as well as in industry. Three new Mo pinF -containing anions [MoO3(pinF)]2-, [Mo2O4(μ2-O)(pinF)2]2-, [Mo2O2(μ-O)2(pinF)2]2- have been synthesized and structurally characterized. The pinF ligands have been found to stabilize both monomeric and dimeric Mo(V) complexes and a dimeric Mo(VI) complex. These compounds can be further studied to look for catalytic redox reactions, and for potential understanding of the rates and mechanism of catalysis. Algal blooms are environmentally hazardous phenomena that cause major damage to aquatic ecosystems. One factor responsible for this effect is the overuse of nitrogen-based fertilizers that has led to accumulation of nitrate (NO3-) in open waters. Nitrate is a nutrient for algae, and when algae proliferate too quickly it causes hypoxia of water. Cu is a well-known catalyst for the electrocatalytic reduction of NO3- and Sn is known to promote selectivity for N2 as the final product of NO3- reduction. The catalytic effect of CuSn alloys for the reduction of nitrate and nitrite have been studied to find the optimum Cu to Sn ratio for this application. It was found that a ratio of 1:1 resulted in the highest peak catalytic current but still less than pure Cu. Additionally, deposition methods on a glassy carbon electrode (GCE) were optimized. It was found that Cu-Sn co-deposition on GCE by controlled potential electrolysis (CPE) was found to be most stable when surfactant K3citrate was added to the deposition solution. Analysis of the final products of NO3- reduction through a microcolorimetric assay was inconclusive and requires further optimization to obtain meaningful data.