Thermostatted micro-reactor NMR probe head for monitoring fast reactions
Thermostatted micro-reactor NMR probe head for monitoring fast reactions
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DOI：
10.1016/j.jmr.2014.02.013
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发表时间：
2014-05-01
影响因子：
2.2
通讯作者：
Hasse, H.
中科院分区：
文献类型：
--
作者：
Braecher, A.;Hoch, S.;Hasse, H.
描述了一种用于监测快速化学反应的新型核磁共振（NMR）探头。它将微反应技术与毛细管流动NMR光谱学相结合。两种反应物被分别送入探头，在微混合器中有效混合。然后，混合的反应物通过配备有螺线管射频线圈的毛细管NMR流动池，在该流动池中获取NMR信号。反应物的整个流动路径使用液体FC-43（全氟三丁胺）进行恒温，以便在几乎等温的条件下研究放热和吸热反应。该装置可以对反应进行动力学研究，时间常数仅为几秒钟。非反应性混合实验进行了新的探头表明，它有利于收购恒定的高分辨率的NMR信号，适用于定量技术混合物中的不同物种。在测试系统上的反应动力学测量证明了新的NMR探头用于监测快速反应的适用性。(C)2014爱思唯尔公司All rights reserved.
A novel nuclear magnetic resonance (NMR) probe head for monitoring fast chemical reactions is described. It combines micro-reaction technology with capillary flow NMR spectroscopy. Two reactants are fed separately into the probe head where they are effectively mixed in a micro-mixer. The mixed reactants then pass through a capillary NMR flow cell that is equipped with a solenoidal radiofrequency coil where the NMR signal is acquired. The whole flow path of the reactants is thermostatted using the liquid FC-43 (perfluorotributylamine) so that exothermic and endothermic reactions can be studied under almost isothermal conditions. The set-up enables kinetic investigation of reactions with time constants of only a few seconds. Non-reactive mixing experiments carried out with the new probe head demonstrate that it facilitates the acquisition of constant highly resolved NMR signals suitable for quantification of different species in technical mixtures. Reaction kinetic measurements on a test system are presented that prove the applicability of the novel NMR probe head for monitoring fast reactions. (C) 2014 Elsevier Inc. All rights reserved.