Chinese Journal of Chromatography

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Preparation and Quantitative Analysis of Methyl Phenyl Carbonate Standard Sample

XING Aihua1,2, ZHANG Minqing1, HE Zhimin1, ZHANG Jianping1

  

  1. 1.School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China;
    2.Department of Chemical Engineering, Tsinghua University, Beijing 100084, China

  • Received:2005-06-21 Revised:2006-03-09 Online:2006-05-30 Published:1987-03-25
  • Contact: Xing Aihua

Abstract:

The preparation and quantitative analytical method for high-purity methyl phenyl carbonate (MPC) was developed. Dimethyl carbonate(DMC) and diphenyl carbonate (DPC) were firstly used as reactants to synthesize MPC catalyzed by TiO2/SiO2 because the disproportionation of MPC is reversible and the reverse reaction is thermodynamically favorable. The high-purity MPC standard sample was obtained by reduced pressure distillation and the removal of minor phenol with dilute sodium hydroxide solution. The qualitative analysis by gas chromatography-mass spectrometry (GC-MS) showed there were minor phenol and diphenyl carbonate in the MPC sample. The mass percent concentration of water in the MPC sample was 0.26%, which was determined by Karl Fischer titration. A gas chromatographic method with an OV-101 capillary column was established for quantifying the minor phenol and DPC in the MPC sample. The quantitative results showed the mass concentrations of phenol and DPC were 2.04% and 1.59%, respectively. The difficulty to analyze MPC, the intermediate product of the transesterification of DMC and phenol, was solved with the self-made MPC standard sample.

Key words: methyl phenyl carbonate, preparation , standard sample, gas chromatography-mass spectrometry (GC-MS)