The chemistry of tungsten hexachloride in an acidic sodium chloroaluminate melt (63 mole percent A1C13) has been investigated by electrochemical and spectroscopic techniques at temperatures of 150 ~ and 175~ WC16 undergoes several reduction steps in the melt, the first of which is sensitive to the presence of oxide impurities. UV-visible and infrared absorption measurements indicate that tungsten hexachloride reacts with oxide to produce WOC14. Comparison of spectroscopic and electrochemical data indicates that the first voltammetric wave is due to the reduction of the hexachloride to WC15 (E1/2 = +1.665V vs. A13 § in the same melt) and that WOC14 is electroactive only below + 1.5V. The equilibrium constant for the formation of WOC14 and the initial amount of oxide in the melt are derived from voltammetric data and compared to values obtained from infrared measurements.
ChemInform Abstract In an acidic sodium chloroaluminate melt (63 mol% AlCl3), WCl6 undergoes several reduction steps, the first of which is sensitive to oxide impurities and possibly can be used for the quantitative determination of oxide in such melts. UV/VIS and IR absorption measurements indicate that WCl6 reacts with oxide to produce WOCl4. Comparison with the electrochemical data indicates that the first voltammetric wave is caused by the reduction of WCl6 to WCl5 (E1/2 = 1.665 V vs. Al/Al3+ in the same melt) and that WOCl4 is electroactive only below +1.5 V.
Various metal oxides (MOx's), formed either as composites or films, were studied as possible materials for the fabrication of a faradaic pseudo reference electrode ( FPRE ). The basis of the reference was the constant current electrolysis of water to oxygen where the potential depended logarithmically on the current due to the irreversibility of the electrode reaction. It was anticipated, that with judicious choice of the MOx and the current level, that interferences could be minimized in comparison with a reversible, potentiometric reference electrode, particularly for in-vivo application. The properties of Ru02 on Ti substrate or as a composite (graphite/Kel-F), Pt, and Pt particles dispersed in a polymer film on glassy carbon were investigated as possible FPRE. In the case of Pt, the surface of the electrode is assumed to be platinum oxide at anodic potentials.
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