大学化学 >> 2016, Vol. 31 >> Issue (9): 56-61.doi: 10.3866/PKU.DXHX201602015

化学实验 上一篇    下一篇

多种方法分析与评价乙酸乙酯合成实验中产物之纯度

赵华绒*(),蔡黄菊,秦敏锐,余利明,邵东贝   

  • 发布日期:2016-09-30
  • 通讯作者: 赵华绒 E-mail:zhr0103@zju.edu.cn
  • 基金资助:
    国家基础科学人才培养基金(J1210042);2015年浙江大学探究性实验教学研究项目

Analysis and Evaluation of Purity of Ethyl Acetate in the Esterification Reaction of Ethanol and Acetic Acid

Hua-Rong ZHAO*(),Huang-Ju CAI,Min-Rui QIN,Li-Ming YU,Dong-Bei SHAO   

  • Published:2016-09-30
  • Contact: Hua-Rong ZHAO E-mail:zhr0103@zju.edu.cn
  • Supported by:
    国家基础科学人才培养基金(J1210042);2015年浙江大学探究性实验教学研究项目

摘要:

采用气相色谱内标法、面积归一化法及NMR内标法3种方法对乙酸乙酯合成反应中的产物进行纯度分析。GC内标法可抵消由于操作条件的波动而带来的误差,只需内标物与待测组分在同样条件下出峰且分离度较好,定量精度高,测出的乙酸乙酯纯度最低;应用NMR内标法可同步完成纯度分析和结构鉴定,且无需引入校正因子,操作简便。

关键词: 微型核磁共振波谱仪, 气相色谱仪, 纯度, 内标法, 面积归一化法

Abstract:

The gas chromatography method using internal standard and area normalization calibration and the NMR method using internal standard calibration are adopted for the determination of product purity in the synthesis of ethyl acetate. The purity of ethyl acetate detected by the GC internal standard method was the lowest. In contrast, the purity detected by the NMR internal standard method was the highest. The NMR internal standard method has more advantages, for this method can be used to complete the quantitative analysis and structural identification simultaneously, without the need to measure the correction factor.

Key words: Portable nuclear magnetic resonance spectrometer, Gas chromatography, Purity, Internal standard method, Area normalization calibration

MSC2000: 

  • O6-3