Electrochemical polarization and reduction experiments are reported which were performed with a three-terminal cell and a molten salt electrolyte consisting of calcium chloride with additions of calcium oxide. Employing a metal cathode, a graphite anode and a pseudo-reference electrode also made from graphite, polarization measurements were carried out with the aim to validate the performance of the pseudo-reference electrode and to assess the stability of the electrolyte. Using a chromium sesquioxide cathode in conjunction with a graphite anode and a graphite pseudo-reference electrode, electrochemical reduction experiments were conducted under potentiostatic control. The key results are: a graphite pseudo-reference electrode has been shown to be appropriate in the present type of molten salt electrochemical experiments that take place on a time scale of many hours; the conversion of chromium oxide into chromium metal has been accomplished under cathodic potential control and in the absence of calcium metal deposition; a significant amount of calcium oxide in the calcium chloride has been found necessary to preclude anodic chlorine formation throughout the entire experiment; a considerable overpotential has been identified at the anode.
Copper has been separated from iron and steel by chlorine-air mixtures at 800uC. It was found that, contrary to predictions based upon thermodynamics, cupric chloride was the favoured copper product rather than cuprous chloride. This was due to the high vapour pressure of cupric chloride. It was found that in order to prevent the reaction between iron and cupric chloride it was necessary to preoxidise the iron to form an impervious oxide film. Copper contents lower than 0 . 05 wt-% were readily obtained after 10 min exposure to the gas, even when starting with several per cent of copper mixed with the iron or steel.
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