Gas Chromatographic Behavior of the Stationary Phase Near the Freezing Point

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Abstract
The effect of decreasing the column temperature below the freezing point of the stationary phase was investigated with four polymeric and one single compound stationary phases. Column efficiencies, polarity, and retention volumes were studied using a polarity mixture introduced by Averill. Log Vg vs 1/T plots were constructed for each solute on Carbowax 1540 and 20M, ethylene glycol succinate, Halocarbon 6-00, and cetyl alcohol columns. Carbowax 1540 and 20M, ethylene glycol succinate, and cetyl alcohol showed sharp discontinuities at the freezing point. Changes in the elution order of the components in the polarity mixture occurred at the freezing point with Carbowax 1540 and 20M, Halocarbon 6-00, and cetyl alcohol. Column efficiencies decreased abruptly where large discontinuities in the log Vg vs 1/T plots were observed and generally improved again at temperatures below the freezing point of stationary phase. Apparent oxidation of Carbowax 1540 occurred during either the preparation of column packing by the steam bath evaporation technique or drying of the packing.

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