过氧化新戊酸叔丁酯的气相色谱分析法

Gas Chromatography of Tert-Butyl Peroxypivalate

通过气相色谱法研究了过氧化新戊酸叔丁酯，进而研究了部分其它过氧化物。这些不耐热的过氧化物不能在高温下分析。在低温下，由于有较低的蒸汽压，满意的色谱图也不易获得。因此，利用气相色谱分析时必需严格的控制相关温度。经研究得出，用PEG6000、DNP and Silicone SE-30做固定相，载气流速设为10～100mL／min，对于过氧化物的分解没有影响。过氧化新戊酸叔丁酯的分析条件：Silicone SE-30（固定液），80℃（柱温），10mL／min（载气流速），萘嵌戊烷（内标物）。标准偏差0.84％，回收率99．49％。有些蒸发后立即分解的过氧化物，不能用这个方法检测。

This text passed gas chromatography of tert - Butyl peroxypivalate to study, then studied parts of others over oxide. These heat- labile 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 packing 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. The condition to t - butyl peroxypivalate ： Silicone SE - 30（stationary liquid）, 80 ℃ （column temp. ）, 10-ml/min（flow rate）, t - butanol （in- ternal standard）. Standard deviation（ ± 3δ）0.85 % , Recovery（ % ）99.49 %. Some organicperoxides which decomposed immediately after vaporization could not be determined by this method.