毛细管气相色谱法检测环氧氯丙烷及其微量组分  

Determination of epichlorohydrin and its trace components by capillary gas chromatography

作　　者：胡芳 于旺堂 张卫东 HU Fang;YU Wangtang;ZHANG Weidong(Henan Bilions Advanced Material Co.Ltd.,Jiaozuo 454191,China;Public Inspection and Testing Centre of Yuanyang County,Xinxiang 453500,China)

机构地区：[1]河南佰利联新材料有限公司,河南焦作454191 [2]原阳县公共检验检测中心,河南新乡453500

出　　处：《精细石油化工进展》2022年第4期50-54,共5页Advances in Fine Petrochemicals

摘　　要：根据甘油法生产环氧氯丙烷(ECH)中控及产品分析的需求,建立一种毛细管气相色谱法测定二氯丙醇、ECH及其微量组分的方法。采用OV-1701(30.0 m×0.25 mm,1.00μm)7%氰丙基-7%苯基-86%甲基聚硅氧烷色谱柱,程序升温,起始温度100℃,保持1 min,以15℃/min升到180℃并保持5 min,进样口温度220℃,分流进样,分流比为50∶1,氢火焰离子化(FID)检测器,检测器温度350℃,进样量0.2μL的检测条件,先根据ECH、1-氯-2-丙醇、缩水甘油、1,3-二氯丙醇、2,3-二氯丙醇和3-氯-1,2-丙二醇单标的保留时间进行定性分析,再采用校正面积归一法对ECH中控及产品进行定量分析。结果表明:毛细管气相色谱法可准确测定反应体系中6种物质的含量,ECH、1-氯-2-丙醇、缩水甘油、1,3-二氯丙醇、2,3-二氯丙醇和3-氯-1,2-丙二醇的保留时间分别为3.754、4.017、4.205、6.477、7.076和7.775 min;经检测,2022年3月28日某公司某批次的氯化样品含1,3-二氯丙醇和2,3-二氯丙醇的总质量分数为95.52%,ECH样品含ECH的质量分数为99.64%。该方法操作简单、相对标准偏差为0.01%~0.05%、加标回收率为98.7%~100.3%,可作为甘油法生产ECH的过程及产品质量监控。A method for the determination of dichloropropanol,epichlorohydrin and their trace components by capillary gas chromatography had been developed to take central control and final products for analysis in the production process of epichlorohydrin by glycerol method. The analytical condition was based on OV-1701(30.0 m×0.25 mm,1.00 μm)7% cyanopropyl-7% phenyl-86% methyl polysiloxane column with programmed temperature steps,the initial column temperature was 100 ℃,maintained 1 min,then rised to 180 ℃ with the speed of 15 ℃/min,maintained 5 min. The inlet temperature was 220 ℃ with the split ratio 50∶1. The detector was hydrogen flame ionization(FID)with temperature of 350 ℃ and the injection volume was 0.2 μL. Firstly,the retention time of epichlorohydrin(ECH),1-chloro-2-propanol,glycidyl,1,3-dichloropropanol,2,3-dichloropropanol and 3-chloro-1,2-propanediol was analyzed qualitatively,and then the calibration area normalization method was applied to the quantitative analysis of the central control and final products. Results showed that the content of 6 substances in the reaction system could be accurately determined by the capillary gas chromatography,such as the retention time of epichlorohydrin,1-chloro-2-propanol,glycidyl,1,3-dichloropropanol,2,3-dichloropropanol and 3-chloro-1,2-propanediol of was 3.754,4.017,4.205,6.477,7.076 and 7.775 min respectively,after testing,the total mass fraction of 1,3-dichloropropanol and 2,3-dichloropropanol was 95.52% in the chlorination sample,and the mass fraction of epichlorohydrin was 99.64% in the ECH sample from some company respectively,on March 28,2022,which could be used for monitoring the production process and product quality of epichlorohydrin by glycerol method. The relative standard deviation about the components of each impurity and recovery rate were 0.01%-0.05% and 98.7%-100.3% seperatively by this simple method.

关 键 词：毛细管气相色谱法 氢火焰离子化检测器 环氧氯丙烷 二氯丙醇 

分 类 号：O657.71[理学—分析化学] TQ222.2[理学—化学]