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PhD subjects

2 sujets IRAMIS

Dernière mise à jour : 17-09-2019


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• Analytic chemistry

 

In situ analysis of an organic redox flow cell through magnetic resonance and additive manufacturing

SL-DRF-19-0556

Research field : Analytic chemistry
Location :

Service Nanosciences et Innovation pour les Materiaux, la Biomédecine et l'Energie

Laboratoire Structure et Dynamique par Résonance Magnétique (LCF)

Saclay

Contact :

Lionel DUBOIS

Patrick BERTHAULT

Starting date : 01-10-2019

Contact :

Lionel DUBOIS
CEA - DRF/INAC/SyMMES/CAMPE

04 38 78 92 57

Thesis supervisor :

Patrick BERTHAULT
CEA - DRF/IRAMIS/NIMBE/LSDRM

+33 1 69 08 42 45

Personal web page : http://iramis.cea.fr/Pisp/patrick.berthault/

Laboratory link : http://iramis.cea.fr/nimbe/lsdrm/

In the thesis project we want to take advantage of our recent advances in 3D printing combined with the development of integrated dynamic nuclear magnetic resonance devices to study operating systems by NMR and perform in situ or operando experiments. We wish to apply these developments according to an important area of ??research in the field of energy: the identification and study of migrations of different molecular species generated during the operation of an organic redox flow battery (RFBO).



In this purpose it will be necessary to build a mini battery that will be integrated within a conventional NMR magnet. The solution flow in each of the compartments will be driven using our patented mini bubble Pump approach. Here the modularity of our low cost system will allow us to follow spectroscopy and imaging different molecular species in several positions of the battery. The components and geometry will be adapted to organic flow cells, the main goal being to understand and analyze the degradation mechanism and products of the redox molecule (anthraquinone derivatives) on the redox cycle.



The work requested from the doctoral student will go from a strong implication in the design of the mini-battery, to its construction and the magnetic resonance studies. In this area, dedicated protocols and new sequences, using both spectroscopic and recent MRI techniques, will have to be developed.
Fluidics and NMR micro-detection for real-time in situ monitoring of chemical reactions

SL-DRF-19-0791

Research field : Analytic chemistry
Location :

Service Nanosciences et Innovation pour les Materiaux, la Biomédecine et l'Energie

Laboratoire Structure et Dynamique par Résonance Magnétique (LCF)

Saclay

Contact :

Patrick BERTHAULT

Starting date : 01-10-2019

Contact :

Patrick BERTHAULT
CEA - DRF/IRAMIS/NIMBE/LSDRM

+33 1 69 08 42 45

Thesis supervisor :

Patrick BERTHAULT
CEA - DRF/IRAMIS/NIMBE/LSDRM

+33 1 69 08 42 45

Personal web page : http://iramis.cea.fr/Pisp/patrick.berthault/

Laboratory link : http://iramis.cea.fr/nimbe/lsdrm/

More : http://www.cortecnet.com

A large number of chemical processes are complex and require for their optimization to understand the reaction mechanisms by real-time observation of intermediate compounds and end products. Nuclear Magnetic Resonance (NMR) can perform this task, but this requires taking into account several aspects: to overcome the lack of intrinsic sensitivity of NMR, to bring the detection zone as close as possible to the synthesis reactor and to be able to accurately quantify the data obtained.



Recently LSDRM researchers developped and patented a 3D-printed NMR device based on a mini bubble pump associated with fluidics and micro-detection, installable on a commercial probe inside the NMR magnet. An insert version plugged into a micro-imaging probe and a version using an inductive coupling between the micro-coil and the commercial coil have been developed. The system allows a significant improvement of the NMR signal for the slowly relaxing nuclei, since the constituents of the reaction mixture are located in a magnetic field close to that of the NMR study, thus allowing a pre-polarization of the whole solution. Moreover, thanks to the controlled of the flow, between two scans, the fresh spins replace those previously excited in the detection region; it is therefore not necessary to wait several relaxation times between each scan acquisition.



Based on CortecNet's expertise in the synthesis of stable isotope-enriched compounds, and LSDRM, a research laboratory recognized for its know-how in the creation of innovative devices for improving the NMR technique, the objective of this research project is to develop a complete NMR monitoring system, in situ, of chemical syntheses in order to provide organic chemists with an indispensable measuring instrument in their daily activities.

 

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