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Mobile tool for HPLC reaction monitoring

机译:用于HPLC反应监测的移动工具

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摘要

A mobile HPLC reaction monitoring tool consisting of a cart-mounted microfluidic HPLC instrument equipped with a tethered, automated sampling and dilution module is described. Several examples of the use of the instrument for carrying out reaction progress analysis are presented. Reaction aliquot size is typically only a few microliters, allowing extensive sample monitoring from small volume reactions. Reaction quenching is possible, and aliquot dilution is adjustable, with suitable precision and accuracy even at hundredfold dilution. A sampling capillary with a chemically inert stainless steel fritted terminus allows sampling from some heterogeneous reactions. The sampling interval is adjustable, from a minimum of about 4 min, upwards. Visualization of an ongoing or completed study as either stacked "waterfall" chromatograms or as graphs of integrated peak areas (or any derived function, such as percent ee or percent conversion) vs time affords the process chemist valuable information on reaction kinetics and a useful record of reaction progress over time. While online HPLC analysis has been known for some time, the compact and mobile nature of this instrument renders it especially useful for carrying out reaction progress monitoring in the laboratory environment.
机译:描述了一种移动式HPLC反应监测工具,该工具由安装在推车上的微流体HPLC仪器组成,该仪器配有系留的自动采样和稀释模块。介绍了使用仪器进行反应进度分析的几个示例。反应等分试样的大小通常只有几微升,因此可以从小体积反应中进行广泛的样品监测。可以进行反应淬灭,并且等分试样稀释度是可调的,即使在百倍稀释度下也具有合适的精度和准确度。带有化学惰性不锈钢多孔末端的采样毛细管允许从某些异质反应中进行采样。采样间隔是可调的,至少从大约4分钟开始。将正在进行或已完成的研究可视化为堆积的“瀑布”色谱图或积分峰面积(或任何衍生函数,例如ee或转化百分比)随时间变化的图表,可为过程化学家提供有关反应动力学的有价值的信息和有用的记录随着时间的推移反应进度。尽管在线HPLC分析已为人所知,但该仪器的紧凑和移动特性使其特别适用于在实验室环境中进行反应进度监控。

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