有機過酸化物のガスクロマトグラフィー

概要

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Organic peroxides are widely used in industry and known to be evolved in autoxidation and combustion reactions. The peroxides have been generally determined by iodometric method, although the method could not exclude analytical errors caused by incomplete reaction and formation of iodine by dissolved oxygen. The present study has been undertaken to measure dialkylperoxide, hydroperoxide, peroxyester and diacylperoxide by gas chromatography. These heatlabile peroxides were unable to be analyzed at a high temperature, while satisfiable chromatogram was not obtained at a low temperature because of their low vapor pressure. Therefore, this method required a strictly established temperature. Column packings of PEG 6000, DNP and Silicone SE-30 and the flow rate of carrier gas in (10〜100) ml/min had no effect on decomposition of the peroxides. Analysis conditions for typical peroxides were summarized as follows; t-butyl cumyl peroxide: PEG 6000, 100℃ (column temp.), 20 ml/min (flow rate), 2-phenyl-2-propanol (internal standard), i-butyl hydroperoxide: Silicone-SE-30, 80℃, 1Oml/min, t-butanol, t-butyl peroxy benzoate: Silicone SE-30, 100℃, 100 ml/min, acenaphthene. Their percentage errors of determination were in the range of 0.11 to 0.85%. Some organic peroxides which decomposed immediately after vaporization. e.g. benzoyl peroxide, could not be determined by this method.
1976-12-10