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Y with several A1C13 samples obtained from different manufacturers: Mallinckrodt lot RTY and TJB; Fisher lot 780679; MCB lot 25; Baker and Adamson lot B128; J. T. Baker lot 33025 and 33.824; BDH ( Gallard-Schlesinger, N. Y. ) lot 0564110; Fluka (Buchs, Switzerland) lot 461085; Koch-Light Labs (Colnbrook, Buckinghamshire, England) In all cased at 120 "C, the eutectic showed the brownish dis- coloration, which was lightest in the case of the Fluka material. There- fore, it was decided to use this material when attempting to develop a standard purification technique. Partial success in the purification of this material has been seen in previous work after treatment of the final eutectic with aluminum turnings. "he success is not complete, since the effectiveness of this treatment varied fromcase to case. Assummg tnar:analuminumoxide layer is responsible for the lack of consistency in the degree of purification, we attempted to solvethis problem by using an amalgamated aluminum plate which was kept under stirring in the eutectic for 6 hr. This treat- ment succeeded in removingthe coloration and in substantially decreasing the iron peaks of the cyclic voltammetric curves. However, a small peak at a potential of about 1.5 V was introduced which can be attributedto the presence of ~ g in~sol+ution. Pre-electrolysis of the eutectic at 120 "C for 24 hr using Ultra Carbon U-5grade carbon electrodes was successful in decreasing the iron peaks, but did not improve the coloration sufficiently. After these preliminary purification attempts, the following pro- cedure was found to yield satisfactory results. AlC13 (Fluka) was mixed with NaCl and KC1 in the ratio of =bout 1.0 molKC1, 1.5 mol NaC1, and 9. 8 mol A1C13, giving a liquid at % 130 "C with a high A1C13 vapor pressure. This liquid was treated with mamesium turnings to ensure the precipitation of such impurities as iron chloride which show an appreciable vapor pressure. From this melt, aluminum chloride was evaporataedta constant temperature of 215 "Cand condensed a s large crystals in the cold part of the apparatus. Byusingtwo.l-B resinreactionkettlesasshowninFig. 6,about70g of pure AlC13 can be obtained overnight. Fig. 7 shows the crystallized 15PDF Image | ALUMINUM CHLORINE BATTERY
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