摘要
目的:建立测定N,N'-羰基二咪唑(CDI)含量的GC方法。采用先把CDI用甲醇衍生成碳酸二甲酯,再以碳酸二甲酯为对照品,用GC测定其含量。方法:采用DB-624毛细管柱为色谱柱;检测器为火焰离子化检测器(FID);程序升温:起始温度40℃,维持3分钟,以每分钟10℃的速率升温至240℃,维持5分钟;柱流速为2 ml/min;进样口温度为150℃;检测器温度为280℃;进样量为0.5μL。结果:碳酸二甲酯在浓度2～24 mg/mL范围内线性关系良好。CDI衍生回收率为103.4%。结论:该方法专属性强、线性好、灵敏度高、操作简便。
Objective: To establish a GC method for Quantitative Analysis of N,N’-carbonyldiimidazole(CDI). A rapid derivatization of CDI to dimethyl carbonate and subsequent GC-FID analysis has been demonstrated here.Methods: All separations were performed on the DB-624 column. The oven temperature program was set as follows: 40 ℃ for 3 min, ramp at 10 ℃/min to 240 ℃, hold at 240 ℃ for 5 min. Inlet temperature was 150 ℃. injection volume was 0.5 μL. FID temperatures were set at 280 ℃. Flow rate was set at 2 mL/min in constant flow mode.Results: The chromatographic peak area and dimethyl carbonate concentration showed a good linear relationship at the range of 2~24 mg/mL. The recovery of derivatization of CDI was 103.4 %. Conclusion: This procedurally simple method is specific, linear, precise, and accurate.
作者
王倩倩
顾铭盼
沈志超
Wang Qianqian;Gu Mingpan;Shen Zhichao(Synthetic Laboratory,Changzhou Pharmaceutical Factory,Changzhou 213018,China)
出处
《广东化工》
CAS
2019年第2期183-184,共2页
Guangdong Chemical Industry
