Determination of the Purity of o-Chlorobenzylidene Malononitrile  by Multiple Analysis Methods

doi:10.11944/j.issn.1000-0518.2020.07.200008

Chinese Journal of Applied Chemistry ›› 2020, Vol. 37 ›› Issue (7): 810-815.DOI: 10.11944/j.issn.1000-0518.2020.07.200008

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Determination of the Purity of o-Chlorobenzylidene Malononitrile by Multiple Analysis Methods

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

Received:2020-01-06 Published:2020-07-01 Online:2020-07-07
Contact: WANG Haitao, professor; Tel:010-66758548; E-mail:dr_wht@163.com; Research interests:detection and harmless disposition of hazard chemicals
Supported by:
Supported by the National Natural Science Foundation of China(No.21876202), the National Major Scientific Instrument and Equipment Development Project (No.2013YQ060615)

Abstract

Abstract: 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.

Key words: 2-chlorobenzalmalononitrile, differential scanning calorimeter, high performance liquid chromatography, nuclear magnetic resonance, purity

WANG Haitao, LIU Haifeng, LIU Yan, ZHAO Wenbo, GAO Runli, DUAN Jingzhong, ZHANG Yuanpeng. Determination of the Purity of o-Chlorobenzylidene Malononitrile by Multiple Analysis Methods[J]. Chinese Journal of Applied Chemistry, 2020, 37(7): 810-815.

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Determination of the Purity of o-Chlorobenzylidene Malononitrile by Multiple Analysis Methods

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