化工学报 ›› 2017, Vol. 68 ›› Issue (7): 2805-2811.DOI: 10.11949/j.issn.0438-1157.20161636

• 分离工程 • 上一篇    下一篇

基于Russell机理分光光度法检测液相体系·OH浓度的改进

赵海谦1, 高杏存1, 刘城昊1, 王忠华1, 周伟2, 高继慧2   

  1. 1 东北石油大学土木建筑工程学院, 黑龙江 大庆 163318;
    2 哈尔滨工业大学能源科学与工程学院, 黑龙江 哈尔滨 150001
  • 收稿日期:2016-11-18 修回日期:2017-03-18 出版日期:2017-07-05 发布日期:2017-07-05
  • 通讯作者: 赵海谦
  • 基金资助:

    国家自然科学基金项目(51606036,91434134);黑龙江省青年科学基金项目(QC2014C047)。

Improvement of spectrophotometric method based on Russell mechanism for detection of ·OH concentration in liquid

ZHAO Haiqian1, GAO Xingcun1, LIU Chenghao1, WANG Zhonghua1, ZHOU Wei2, GAO Jihui2   

  1. 1 Institute of Civil Engineering & Architecture, Northeast Petroleum University, Daqing 163318, Heilongjiang, China;
    2 College of Energy Science and Engineering, Harbin Institute of Technology, Harbin 150001, Heilongjiang, China
  • Received:2016-11-18 Revised:2017-03-18 Online:2017-07-05 Published:2017-07-05
  • Contact: 10.11949/j.issn.0438-1157.20161636
  • Supported by:

    supported by the National Natural Science Foundation of China (51606036, 91434134) and the Heilongjiang Science Funds for Youths (QC2014C047).

摘要:

基于Russell反应机理检测液相体系·OH浓度的分光光度法具有费用低、操作简单等优点,但测试精度低、重复性差是该方法面临的主要问题。分析了该方法精度低的主要原因,提出改进型方法,分析了常见阴阳离子对萃取剂萃取坚牢蓝BB盐(FBBs)的影响,确定了改进型方法的关键检测条件,在此基础上重新建立了·OH浓度与重氮砜产物吸光度之间的函数关系。结果表明:FBBs的干扰是造成检测精度低的根本原因;FeSO4对抑制萃取剂萃取FBBs作用明显,从而大幅度削弱FBBs的干扰;Na+、K+、NO3-几乎对重氮砜产物的吸收峰不产生影响,Cl-对测试结果的影响与其浓度有直接关系;改进型方法的合理萃取时间为300 s,FBBs与甲基亚磺酸(MSIA)摩尔比为50;并得到了·OH浓度与吸光度之间的函数关系式。

关键词: 液相体系, ·OH, 分光光度法, Russell反应机理, 改进型方法

Abstract:

Spectrophotometric method based on Russell mechanism for detection of ·OH concentration in liquid has many advantages, such as low-cost, simple operation, and so on. However, low precision and poor repeatability are its main disadvantages. The reason of this method's low precision was elucidated, and a modified method was proposed. The influence of typical cations and anions on extraction of Fast Blue BB salt (FBBs) was analyzed. Key operating conditions for the modified method was determined. Based on the results, a relationship between ·OH concentration and absorbance of diazosulfones was rebuilt. The interference of FBBs in the diazosulfone extraction process is the main reason of low precision. FeSO4 has a strong ability to hold back extraction of FBBs by extraction agent, which decreases influence of FBBs on diazosulfones detection violently. Na+, K+, NO3- do not have obvious effects on the detection result, while Cl- influence is in relation to its concentration. The conditions for the modified method are: extraction time 300 s and molar ratio of FBBs to methylsulfinic acid (MSIA) is 50. The function relationship between ·OH concentration and absorbance is obtained.

Key words: liquid system, ·OH, spectrophotometric method, Russell mechanism, modified method

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