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USE OF SYSTEM PEAKS IN LIQUID CHROMATOGRAPHY FOR CONTINUOUS ON-LINE MONITORING OF CHEMICAL REACTIONS

机译:系统色谱峰在液相色谱中用于化学反应的连续在线监测

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System peaks, which occur in chromatography with multicomponent mobile phases, can be used for the continuous on-line monitoring of chemical reactions. The mobile phase reservoir is the chemical reactor, and the mobile phase, which contains the reaction mixture, is recycled continuously through the column, At predetermined times, a neat solvent normally the solvent of the reaction, is injected, The system peaks that result reflect the status of the reaction, We describe here the use of system peaks to follow the progress of two reactions: titration of aniline and hydrolysis of aspirin, In the case of aniline titration, we obtained a titration curve by plotting the capacity ratio of the aniline system peak versus the acid volume added during the titration, The experimental endpoint agreed very well with the theoretical equivalence point. A plot of the capacity factor as a function of mobile phase pH behaves similarly to such plots in conventional chromatography. In the hydrolysis of aspirin, we followed the progress of the reaction by monitoring the formation of salicylic acid via its system peak, The data allowed us to calculate the apparent hydrolysis rate constant. The value obtained is in excellent agreement with literature values.
机译:在具有多组分流动相的色谱中出现的系统峰可用于化学反应的连续在线监测。流动相储存器是化学反应器,包含反应混合物的流动相连续地通过色谱柱循环。在预定的时间,通常是反应溶剂的纯净溶剂被注入,系统峰反映了反应的状态,我们在这里描述了使用系统峰跟踪两个反应的进展:苯胺滴定和阿司匹林的水解。在苯胺滴定的情况下,我们通过绘制苯胺的容量比得出滴定曲线。系统峰与滴定过程中添加的酸量之间的关系。实验终点与理论当量点非常吻合。容量因子随流动相pH的变化曲线与常规色谱图中的曲线相似。在阿司匹林的水解过程中,我们通过监测水杨酸的系统峰来监测水杨酸的形成,从而跟踪反应进程。数据使我们能够计算表观水解速率常数。获得的值与文献值非常一致。

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