色谱

色谱

• 技术与应用 • 上一篇    下一篇

阴离子交换离子色谱法测定乳酸催化制备的丙烯酸

石海宁1, 王辉2, 陶丽芝2, 王宗花1, 丁明玉2*   

  1. 1. 青岛大学国家培育基地-纤维新材料与现代纺织重点实验室, 山东 青岛 266071; 2. 清华大学化学系, 北京 100084
  • 收稿日期:2009-12-08 修回日期:2010-02-08 出版日期:2010-06-28 发布日期:1980-06-25
  • 通讯作者: 丁明玉

Determination of acrylic acid from catalytic preparation lactic acid by anion-exchange chromatography

SHI Haining1, WANG Hui2, TAO Lizhi2, WANG Zonghua1, DING Mingyu2*   

  1. 1. Laboratory of Fiber Materials and Modern Textile, the Growing Base for State Key Laboratory, Qingdao University, Qingdao 266071, China; 2. Department of Chemistry, Tsinghua University, Beijing 100084, China
  • Received:2009-12-08 Revised:2010-02-08 Online:2010-06-28 Published:1980-06-25
  • Contact: DING Mingyu

PDF

594

被引次数

29

摘要： 通过乳酸催化脱水制备丙烯酸具有良好的应用前景。为了对其中的催化过程进行有效、及时的监控,建立了一种同时测定乳酸及丙烯酸的阴离子交换色谱法(AEC)。选择Metrohm A Supp 5阴离子交换柱(150 mm×4.0 mm),以2 mmol/L Na2CO3+2 mmol/L NaHCO3混合水溶液为流动相,采用化学抑制电导检测技术,乳酸和丙烯酸在6 min内即可实现完全分离。乳酸和丙烯酸工作曲线的线性范围分别为0.1～500 mg/L和0.1～200 mg/L,检出限分别为0.030 mg/L和0.035 mg/L,加标回收率分别为100.7%～106%和99.6%～103%,相对标准偏差分别为2.16%~2.49%和2.42%~2.48%。该方法准确、快速、灵敏、重现性好。

关键词: 丙烯酸, 催化制备 , 乳酸, 阴离子交换色谱法

Abstract: Acrylic acid is a kind of important monomer and basic organic chemical raw material. In the process of catalytic preparation of acrylic acid from lactic acid, in order to monitor the catalytic process effectively and timely, an anion-exchange chromatographic (AEC) method has been established for the simultaneous determination of lactic acid and acrylic acid. The separation was carried out on a Metrohm A Supp 5 anion-exchange column (150 mm×4.0 mm) with 2 mmol/L Na2CO3+2 mmol/L NaHCO3 as the mobile phase. The flow rate of the mobile phase was 0.7 mL/min. A chemically suppressed conductivity detector was used. The linear ranges of calibration curves were 0.1-500 mg/L for lactic acid and 0.1-200 mg/L for acrylic acid. The detection limits with S/N=3 were 0.030 mg/L for lactic acid and 0.035 mg/L for acrylic acid. The recoveries of lactic acid and acrylic acid were 100.7%-106% and 99.6%-103% with the relative standard deviations of 2.16%-2.49% and 2.42%-2.48%, respectively. This method is accurate, speedy, sensitive and reproducible, and has been successfully used for the determination of lactic acid and acrylic acid in the catalytic reaction product.

Key words: acrylic acid, catalytic preparation , lactic acid, anion-exchange chromatography