毛细管色谱法同时测定异戊二烯中环戊二烯、甲基吡咯烷酮和二甲基甲酰胺

Simultaneous determination of cyclopentadiene,dimethylformamide and N-methylpyrrolidone in isoprene by capillary column gas chromatography

用毛细色谱法建立异戊二烯中各组分定性分析方法及环戊二烯,N-甲基吡咯烷酮,N,N-二甲基甲酰胺的测定方法.气相色谱条件：采用OV-1701毛细管气相色谱柱,50 m×0.32 mm×0.53 μm.程序升温60 ℃保持5 min后,以10 ℃/min升至190 ℃,保持3 min.氮气（纯度99.999%）为载气,柱前压为69 kPa.分流进样,分流比1∶100.进样口温度200 ℃,FID检测器,检测器温度为200 ℃.结果表明,异戊二烯中各组分均达到良好分离.环戊二烯、N-甲基吡咯烷酮、N,N-二甲基甲酰胺的线性范围均为0.5～1 200 μg/mL;回收率分别为96.0%～98.5%,95.0%～102%,96.0%～99.6%;检出限均达到0.5 μg/mL.其方法简单、快捷且灵敏度高,可以用于异戊二烯中杂质含量的控制.

To establish a method for determination of eyelopentadiene, dimethylformamide and N-methylpyrrolidone simultaneously in isoprene by GC. Qualitative analysis on GC-MS;Quantitative analysis on GC. All components were separated and identified by OV-1701 capillary column （50 m×0.32 mm×0.53 μm）. A temperature program was also applied, the temperature was initialized at 60 ℃ for 5 min, then raised to 190 ℃ at a rate of 10 ℃/min and finally kept for 3 min. Split injection,split ratio 1 ： 100, injector temperature 200 ℃. Deteetor：FID, temperature 200 ℃. N2 （99. 999% ） was used as carrier gas, column press was 69 kPa. All components were well resolved. The linear ranges of eyelopentadiene, dimethylformamide and N-methylpyrrolidone were 0.5 - 1 200 μg/mL, the average recoveries of these components were 96.0% -98.5% ,95.0% - 102% ,96.0% - 99.6% respectively. The detect limits of them were 0.5 μg/mL. This method is simple, rapid and has good sensitivity.