Convenient and accurate insight into solution-phase equilibria from FlowNMR titrations,Reaction Chemistry & Engineering

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Convenient and accurate insight into solution-phase equilibria from FlowNMR titrations
Reaction Chemistry & Engineering ( IF 3.4 ) Pub Date : 2022-06-09 , DOI: 10.1039/d2re00123c
Daniel B. G. Berry _{1,

2} , Ian Clegg ₃ , Anna Codina ₃ , Catherine L. Lyall _{1,

2} , John P. Lowe _{1,

2} , Ulrich Hintermair _{1,

2,

4}

Affiliation

Chemical solution-phase equilibria such as acid/base reactions and complex formation are typically investigated by titration studies that either use in situ analysis of a continuously changing sample with techniques that measure single attributes (e.g. pH or UV-vis absorbance at a specific wavelength) or ex situ analysis of multiple samples with high-resolution techniques (e.g. high field NMR spectroscopy). Here we present multi-nuclear high resolution FlowNMR spectroscopy as an effective technique for the online analysis of complex solution-phase equilibria that combines the accuracy and convenience of simple in situ measurements with the high specificity and information content of high-resolution NMR spectroscopy. With a closed-loop flow setup reagent addition can be automated using a simple syringe pump and complimentary sensors (such as pH probes and UV-vis flow cells) may be added to the setup. By conducting the titration inside a glovebox connected to the FlowNMR setup even highly air- and moisture-sensitive systems may be investigated. The effectiveness of this approach is demonstrated with examples of Brønsted acid/base titrations (incl. multi-component mixtures and systems with solvent participation), hydrogen bonding interactions, Lewis acid/base interactions, and dynamic metal–ligand binding.

中文翻译：

通过 FlowNMR 滴定方便准确地了解溶液相平衡

化学溶液相平衡，例如酸/碱反应和复合物形成，通常通过滴定研究进行研究，滴定研究使用测量单一属性（例如特定波长下的 pH 值或紫外-可见吸光度）的技术对连续变化的样品进行原位分析或使用高分辨率技术（例如高场核磁共振光谱）对多个样品进行异位分析。在这里，我们提出了多核高分辨率 FlowNMR 光谱作为在线分析复杂溶液相平衡的有效技术，它结合了简单原位的准确性和便利性。具有高分辨率 NMR 光谱的高特异性和信息含量的测量。通过闭环流量设置，可以使用简单的注射泵自动添加试剂，并且可以将免费传感器（例如 pH 探针和 UV-vis 流通池）添加到设置中。通过在与 FlowNMR 装置相连的手套箱内进行滴定，甚至可以研究对空气和水分高度敏感的系统。这种方法的有效性通过 Brønsted 酸/碱滴定（包括溶剂参与的多组分混合物和系统）、氢键相互作用、路易斯酸/碱相互作用和动态金属-配体结合的例子得到证明。

更新日期：2022-06-09

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