Efficient method for in situ agitation of liquids directly inside NMR spectrometer

Antonio De Souza Braga Neto; Baptiste Rigaud; Guillaume Mériguet; Anne-Laure Rollet; Juliette Sirieix-Plénet

doi:10.1016/j.mex.2023.102254

Efficient method for in situ agitation of liquids directly inside NMR spectrometer

MethodsX. 2023 Jun 19:11:102254. doi: 10.1016/j.mex.2023.102254. eCollection 2023 Dec.

Authors

Antonio De Souza Braga Neto¹, Baptiste Rigaud², Guillaume Mériguet¹, Anne-Laure Rollet¹, Juliette Sirieix-Plénet¹

Affiliations

¹ Physicochimie des Electrolytes et Nanosystèmes interfaciaux (PHENIX), Sorbonne Université, 4 Place Jussieu, Paris F-75005, France.
² Fédération de Chimie et Matériaux de Paris Centre, Sorbonne Université, 4 Place Jussieu, Paris F-75005, France.

Abstract

The objective of the method is to allow agitation and fast homogenization of liquid systems in NMR tubes, directly inside the NMR spectrometer. The setup makes it possible to record spectra of samples that are macroscopically not stable, as dispersions of large particles. It makes also possible to fasten the homogeneization of liquid during a reaction or a phase transition. In the present paper, the method has been evaluated using homogeneous liquid extraction (HLLE). This configuration can also be used to introduce gases in different systems to perform various types of experiments. The set up consists in a Teflon tube inserted in the NMR tube bringing gas that yields agitation by bubbling. The gas flow is tuned using an electronically operated valve connected to gas line and to the NMR console. The method details how to reach proper homogenization without any perturbation, as liquid leaks.•An easy method for agitation of liquids inside NMR spectrometers.•The set up can be used for the insertion of gases in the NMR tube inside the spectrometer.•The method allows the study of the mixing of biphasic systems by NMR techniques.

Keywords: Agitation method for samples inside NMR spectrometer; In situ agitation; Ionic liquids; Liquid-liquid extraction; Localized spectroscopy (LOCSY); NMR; Sample homogenisation.