环己烷中痕量组分的测定

Determination of trace components in cyclohexane

采用GC-2030气相色谱仪、介质阻挡放电离子化(BID)检测器、InertCap 1非极性气相色谱柱,建立了环己烷中痕量环己酮、环己醇组分的定量检测方法。结果表明:该方法合适色谱分析条件为采用程序升温,载气流速为1 mL/min,进样量为1.0μL,分流比为201;该方法测定环己烷中痕量环己酮、环己醇时,环己醇的加标回收率为96.7%~104.8%、相对标准偏差(RSD)为0.25%~1.00%、检出限为0.06 mg/kg,环己酮的加标回收率为97.1%~104.1%、RSD为0.03%~1.04%、检出限为0.09 mg/kg;该方法精密度、准确度高,重现性好,分析时间短,有助于聚合溶剂用环己烷生产工艺的精准调控。

The quantitative method of trace cyclohexanone and cyclohexanol in cyclohexane was established by using GC-2030 gas chromatograph,dielectric barrier discharge ionization(BID)detector and InertCap 1 non-polar gas chromatographic column.The results showed that the suitable chromatographic analysis conditions for this method were as followed:programmed heating,carrier gas flow rate of 1 mL/min,injection volume of 1.0μL and split ratio of 201;the standard addition recovery rate of cyclohexanol was 96.7%-104.8%,the relative standard deviation(RSD)0.25%-1.00%,the detection limit 0.06 mg/kg,the standard addition recovery rate of cyclohexanone 97.1%-104.1%,RSD 0.03%-1.04%,and the detection limit 0.09 mg/kg when this method was used to determine the trace cyclohexanone and cyclohexanol in cyclohexane;the method had high precision and accuracy,good reproducibility and short analysis time,which was conducive to the precise control of the production process for cyclohexane as polymerization solvent.