摘要
采用差示扫描量热单峰法对邻氯代苯亚甲基丙二腈(西埃斯)的纯度进行了测定,通过对升温速率的优化,采用密闭不锈钢耐压池,降低了西埃斯本身挥发性的影响,获得了不同质量样品的纯度值,并与高效液相色谱、气相色谱-质谱和核磁共振等方法的测定结果进行了比较。结果表明:差示扫描量热单峰法、高效液相色谱法、气相色谱质谱法和核磁共振法测定的纯度值分别为99.89%、99.92%、99.25%和95.0%,测定结果最大相差4.92%。并讨论了不同分析方法产生偏差的原因。
The purity of o-chlorobenzylidene malononitrile(CS)was measured by differential scanning calorimeter(DSC)using the monopeak method.Considering the volatility of CS,the experiment was conducted by optimization of different heating rates and different qualities.Meanwhile,the purity of CS was also tested by high performance liquid chromatography(HPLC),gas chromatography-mass spectrometry(GC-MS)and nuclear magnetic resonance spectroscopy(NMR).We compared their difference.The purities of CS are 99.89%,99.92%,99.25%,and 94.0%by DSC,HPLC,GC-MS and NMR,respectively,and the maximum discrepancy is 4.92%.We also discuss the reason for the differences.
作者
汪海涛
刘海锋
刘艳
赵文博
高润利
段晶钟
张远鹏
WANG Haitao;LIU Haifeng;LIU Yan;ZHAO Wenbo;GAO Runli;DUAN Jingzhong;ZHANG Yuanpeng(State Key Laboratory of NBC Protection for Civilian,Beijing 102205,China)
出处
《应用化学》
CAS
CSCD
北大核心
2020年第7期810-815,共6页
Chinese Journal of Applied Chemistry
基金
国家自然科学基金资助项目(21876202)
国家重大科学仪器设备开发专项(2013YQ060615)。
关键词
西埃斯
差示扫描量热
高效液相色谱
核磁共振
纯度
2-chlorobenzalmalononitrile
differential scanning calorimeter
high performance liquid chromatography
nuclear magnetic resonance
purity
