气相色谱法分析环己烷氧化液中组分研究

Determination of components in cyclohexane oxidation solution by gas chromatography

采用气相色谱法,通过筛选色谱柱,优化气相色谱分析条件,对环己烷空气氧化液中的组分进行分析研究。结果表明:选用中极性色谱柱D(60 m×0.25 mm×0.25μm),在柱箱起始温度80℃,保持2 min,然后以10℃/min的速率升至260℃,保持20 min,氢火焰离子化检测器温度280℃,进样口温度200℃,分流比501,进样量0.5μL,氮气流速1.6 mL/min,氢气流速35 mL/min,空气流速400 mL/min的条件下,以校正面积归一化法定量,分析环己烷氧化液中的组分含量,环己烷氧化液中各组分能较好地分离,其中环己烷的质量分数为95.2883%,主要组分环己醇、环己酮和环己基过氧化氢(CHHP)的质量分数分别为0.9630%,0.4210%,2.9369%,其相对标准偏差分别为0.44%,0.38%,0.32%;环己醇、环己酮的加标回收率分别为99.1%~100.7%,99.3%~100.4%,CHHP的加标回收率为98.1%~98.9%。

The components in cyclohexane air oxidation solution were analyzed by gas chromatography through selecting chromatographic columns and optimizing gas chromatographic analysis conditions.The results showed that the contents of components in cyclohexane oxidation solution can be quantitatively analyzed by calibration area normalization method and the components can be efficiently separated under the conditions as followed:a medium-polarity chromatographic column D(60 m×0.25 mm×0.25μm),a column box keeping the initial temperature at 80℃for 2 min and then heating to 260℃at a rate of 10℃/min and keeping for 20 min,hydrogen flame ionization detector temperature 280℃,injection temperature 200℃,split ratio 501,injection volume 0.5μL,nitrogen flow rate 1.6 mL/min,and hydrogen flow rate 35 mL/min,air flow rate 400 mL/min;the mass fraction of cyclohexane was determined as 95.2883%and the mass fractions of cyclohexanol,cyclohexanone and cyclohexyl hydrogen peroxide(CHHP)as 0.9630%,0.4210%and 2.9369%,with the relative standard deviations of 0.44%,0.38%and 0.32%,respectively;and the recovery of standard addition of cyclohexanol,cyclohexanone and CHHP were 99.1%-100.7%,99.3%-100.4%and 98.1%-98.9%,respectively.