Gas chromatography of metal halides Public Deposited

http://ir.library.oregonstate.edu/concern/graduate_thesis_or_dissertations/zg64tp699

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  • An all-glass gas chromatograph was developed for the analysis of corrosive metal halides. Included in the apparatus is a new liquid sampling system designed for fast repetitive sampling of corrosive liquids in an inert atmosphere. A flame photometer detector was developed to permit the detection of corrosive solutes in the gas stream without exposing the sensing element to chemical attack. Several materials were evaluated to determine their applicability as column materials for the analysis of metal chlorides. All the materials failed to separate the metal chlorides completely, except for Halocarbon 6-00. However, polytetrafluoroethylene, FX-45 and Teflon, gave promising results. Chromatograms of metal chlorides on porous glass showed an inordinate amount of tailing. Niobium pentachloride and niobium oxytrichloride failed to elute from a column where a LiCl-KC1 eutectic was used as a liquid phase, except when the temperature was very high and the column very short. Halocarbon 6-00 on Chromosorb W was used to separate mixtures of metal chlorides. Several metal chlorides, including GeC1₄, SnC1₄, AsC1₃ and TiC1₄ gave almost symmetrical peaks. No evidence of reactions between the metal chlorides and the column materials was observed, even at temperatures up to 185°C. Log V[subscript g] versus 1/T plots give straight lines for the four metal chlorides listed above, indicating a normal distribution between the stationary and mobile phases. The reproducibility of peak areas for samples of AsC1₃ and SnC1₄ was very good. Three mixtures of AsC1₃ and SnC1₄ were analyzed and the results are also considered to be quite good. Chromatograms of a mixture of AsBr₃ and AsC1₃ indicate that an exchange may take place between the two compounds. The same results were obtained for a mixture of SnC1₄ and SnBr₄.
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