Gas-Chromatographic Separation of Inorganic Chlorides and its Application to Metal Analysis: I. Qualitative and Quantitative Aspects of the Gas-Chromatographic Separation Procedure

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Abstract
A study has been made of the potentialities of gas chromatography as a tool for the analysis of metals and alloys. As is demonstrated in the present paper, gas chromatography can be used for the separation and the quantitative determination of inorganic chlorides. With proper adaptation of the apparatus and technique to the reactivity of these compounds, satisfactory chromatograms were obtained, showing good peak symmetry, stable baselines, and absence of artefact peaks. Of nineteen substances studied, having boiling points between 50 and 250°C, all but a few were determined accurately in mixtures. The exceptions are the very unstable vanadium tetrachloride and antimony pentachloride (dissociating readily even at relatively low temperatures) as well as an oxychloride of molybdenum, of which the identity was uncertain. A number of determinations carried out on a mixture of the tetrachlorides of silicon and tin under various conditions showed a good reproducibility: standard deviations of 0.2 to 0.6 wt % were found. The analysis of metals and alloys will be reported in a subsequent paper.