色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 116-120.DOI: 10.3724/SP.J.1123.2018.08030

• 研究论文 • 上一篇    

气相色谱法检测工业用乙二醇纯度及杂质

范晨亮, 张育红, 王川, 彭振磊, 高枝荣   

  1. 中国石化上海石油化工研究院, 上海 201208
  • 收稿日期:2018-08-21 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 范晨亮,Tel:(021)68462197,E-mail:fancl.sshy@sinopec.com.

Determination of purity and impurities of ethylene glycol for industrial use by gas chromatography

FAN Chenliang, ZHANG Yuhong, WANG Chuan, PENG Zhenlei, GAO Zhirong   

  1. Shanghai Research Institute of Petrochemical Technology, SINOPEC, Shanghai 201208, China
  • Received:2018-08-21 Online:2019-01-08 Published:2014-11-29

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摘要：

以Rtx-624色谱柱（30 m×0.32 mm×1.8 μm）为分析柱进行分析，采用校正面积归一化法，建立了检测工业用乙二醇纯度及其中有机杂质的气相色谱分析法。该法可检测传统乙烯法制得的乙二醇中固有杂质二乙二醇、三乙二醇和1，3-二氧杂烷-2-甲醇，同时也适用于检测草酸酯加氢法制得的乙二醇中的新杂质（1，2-丁二醇、1，4-丁二醇、1，2-己二醇、碳酸乙烯酯等）。结果表明，该法具有良好的重复性和较高的检测灵敏度，检出限最低可达0.0002%（质量分数），回收率在91.2%~105.4%之间。该法在乙二醇生产控制、产品检测、市场贸易等过程中具有良好的应用前景。

关键词: 纯度和杂质, 气相色谱法, 乙二醇

Abstract:

A new test method was established for the determination of purity and impurities of ethylene glycol (EG) by gas chromatography (GC) using a Rtx-624 column (30 m×0.32 mm×1.8 μm). The method determined not only the impurities in EG from the ethylene oxidation process, such as diethylene glycol, triethylene glycol and (1,3-dioxolan-2-yl)methanol, but also the impurities from the oxalate hydrogenation process, such as 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol, and ethylene carbonate, etc. The method showed good repeatability and high detection sensitivity. The lowest LOD of the impurities reached to 0.0002% (mass fraction), and the recoveries of the impurities were in the range of 91.2%-105.4%. The proposed method can be applied in production control, product testing and market trade of ethylene glycol.

Key words: ethylene glycol (EG), gas chromatography (GC), purity and impurities

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