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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;FeSO_4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~+、NO_3-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。
The spectrophotometric method based on Russell reaction mechanism for detecting the concentration of OH in liquid phase system has the advantages of low cost and simple operation. However, the low precision and poor repeatability of this method are the main problems of this method. The main reason for the low accuracy of the method was analyzed. An improved method was proposed to analyze the effect of common anion and cation on the extraction of FBBs. The key detection conditions of the improved method were determined. Based on this, A functional relationship between · OH concentration and absorbance of diazosulfone product was established. The results showed that the interference of FBBs was the root cause of low detection accuracy. FeSO_4 inhibited the extraction of FBBs obviously, which greatly weakened the interference of FBBs. Na ~ +, K ~ +, NO_3- The effect of Cl ~ - on the test results is directly related to the concentration. The optimized extraction time is 300 s and the molar ratio of FBBs to MSIA is 50. OH concentration and absorbance as a function of the relationship between.