Citation: 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. doi: 10.11944/j.issn.1000-0518.2020.07.200008 shu

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

State Key Laboratory of NBC Protection for Civilian, Beijing 102205, China

Corresponding author: WANG Haitao, dr_wht@163.com
Received Date: 6 January 2020
Revised Date: 21 February 2020
Accepted Date: 30 March 2020

Fund Project: the National Natural Science Foundation of China 21876202Supported by the National Natural Science Foundation of China(No.21876202), the National Major Scientific Instrument and Equipment Development Project (No.2013YQ060615)the National Major Scientific Instrument and Equipment Development Project 2013YQ060615

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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.
- 2-chlorobenzalmalononitrile,
- differential scanning calorimeter,
- high performance liquid chromatography,
- nuclear magnetic resonance,
- purity
1. [1]
  Olajos E J, Salem H. Riot Control Agents:Pharmacology, Toxicology, Biochemistry and Chemistry[J]. J Appl Toxicol, 2001,21:355-391. doi: 10.1002/jat.767
2. [2]
  QU Ganglian, PAN Rongrong, MA Guohua. Application of Orthogonal Experimental Design in Optimizing the Desorption Condition of o-Chlorobenzylidene Malononitrile[J]. Chem Anal Meterage, 2007,27(3):47-49. doi: 10.3969/j.issn.1008-6145.2007.03.015
3. [3]
  HUANG Chaoqun, SHI Hongxing, PENG Wenlian. Formation Condition of Hazardous Products in the Pyrolysis and Combustion Progress of CS by TOF-MS[J]. Safety Environ Eng, 2017,24(3):97-102.
4. [4]
  HUANG Chaoqun, SHI Hongxing, PENG Wenlian. On line Analysis Research of the Pyrolysis Products in the Combustion Progress of CS Based on PET-TOF-MS[J]. Mod Sci Instrum, 2017(2):67-71.
5. [5]
  WANG Geng, LI Yanli, WANG Xuhong. Determination of CS by Ultraviolet Spectrophotometry[J]. Chinese J Spectrosc Lab, 2013,30(3):1029-1031. doi: 10.3969/j.issn.1004-8138.2013.03.002
6. [6]
  WANG Hongying, HAO Huanming, MU Yinglin. Determination of Irritang Agents in Lachrymator by Gas Chromatorgraphy[J]. Anal Instrum, 2012,30(4):30-32. doi: 10.3969/j.issn.1001-232X.2012.04.007
7. [7]
  CHEN Qing, WEI Borong, BAO Dejun. Determination of Purity of Samples by Monopeak Method of Differential Scanning Calorimetry[J]. Anal Instrum, 2005,30(3):42-46. doi: 10.3969/j.issn.1001-232X.2005.03.012
8. [8]
  DING Enyong, LIANG Xuehai. The Criticism of the MonoPeak Method of DSC to Determine the Purity of Samples[J]. J Instrum Anal, 1993,12(4):52-55.
9. [9]
  SONG Yinqing, WANG Min, WANG Tongtong. Application of Inverse Gated Decoupling Technique in Quantitative ¹H NMR Determination of Purity of Phenylethanolamine A[J]. J Instrum Anal, 2017,36(7):933-936. doi: 10.3969/j.issn.1004-4957.2017.07.018
10. [10]
  JIANG Xiangdong, SU Keman, CAI Shuihong. Determination of Enantiomeric Purity of (S)-(-)-α-Phenylethylamine by NMR[J]. Spectrosc Spectr Anal, 2001,21(3):404-405.
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