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Solid State NMR platform
(NMR center of Caen-Normandy)

The manager of the solid-state NMR platform at LCS is Aurélie Vicente, Associate professor.

The solid-state NMR platform has several missions:

  1. to be an analytical service for the benefit of all LCS users who need a structural characterization of their materials, e.g. after synthesis or post-synthesis modification of zeolites materials.
  2. to provide training sessions, in particular for the PhD students and post-docs, in order they acquire full experimental autonomy in a short term.
  3. to maintain and develop NMR methods, i.e., by implementing the most interesting advanced techniques available in literature, or by developing new ones. This allows the service to stay at least at the current state of the art of the technique.

The NMR equipment of the laboratory has been renewed recently (2013) with the help of the EMC3 Labex and FEDER funds. We now possess the last generation of Bruker spectrometers (400 and 500 MHz advance III HD). Solid-state NMR probeheads allows us to operate at MAS spinning speed up to 45 kHz, and in triple resonance (1H/X/Y). We possess a MAS probehead able to work at temperatures up to 400°C, and under flow conditions (operando). We have set up a full system to allow the production of Hyperpolarized Xenon, a gas that has been proved to be very interesting for the characterization of porous materials. Finally, we recently merge the solid state NMR at LCS and the liquid state NMR platform located at the LCMT, to create a unique NMR center in Normandy.

 

List of the equipments of the NMR center

400 MHz WB NMR spectrometer for Xenon and operando NMR

This spectrometer is mostly dedicated to operando and 129Xe NMR.

  • This spectrometer has an ultrashielded wide bore magnet
  • The spectrometer console is an Avance III HD equipped with a two independent receivers and high-power amplifiers (1 kW)

It is equipped with the following probes:

  • 10-mm BBO probehead for xenon NMR
  • 7-mm double-resonance probehead 1H/X
  • MASCAT: 7-mm double-resonance probehead 1H/X designed for catalysis with high temperature and flow of reactants capabilities
  • 4-mm double-resonance probehead 1H/X
  • 4-mm triple-resonance probehead 1H/X/Y
  • 2.5-mm double-resonance probehead 1H/X

500 MHz NB NMR spectrometer

This spectrometer is mainly dedicated to solid-state NMR characterization  and HR-MAS NMR.

  • This spectrometer has an ultrashielded narrow bore magnet
  • The spectrometer console is an Avance III HD

It is equipped with the following probes:

  • 5-mm TXO probehead for C/P/H
  • 4-mm double-resonance probehead H/X
  • 4-mm HR-MAS probehead H/C
  • 3.2-mm triple-resonance probehead H/X/Y
  • 1.9-mm triple-resonance probehead H/X/Y

400 MHz NB NMR spectrometer

This spectrometer (located in the LCMT) is dedicated to solution-state NMR.

  • This spectrometer has an shielded narrow bore magnet
  • The spectrometer console is an Avance III Nanobay.

It is equipped with the following probe:

  • ?-mm BBFO ATMA probehead

A sample changer can be used for routine/automatic experiments.

500 MHz NB NMR spectrometer

This spectrometer (located in the LCMT) is dedicated to solution-state NMR.

  • This spectrometer has an shielded narrow bore magnet
  • The spectrometer console is an Avance III.

It is equipped with the following probeheads:

  • ?-mm BBFO ATMA probehead
  • 5-mm triple-resonance TXO C/P/H

A sample changer can be used for routine/automatic experiments.

Home-built dehydration / pretreatment / adsorption setup

This setup allows for full dehydration of NMR sample, and possibly the activation (under various gas atmosphere O2, H2, …) up to 500 °C. It also allows performing adsorption of probe molecules up to 3 bars.

Learn more

Home-built operando NMR setup

This setup allows operating the operando NMR probehead (MASCAT):

  • Gas injection in continuous or stop-flow mode.
  • Saturator and cryostat to manage injection of probe molecules (generally organic molecules)

The MASCAT probe allows operation up to 400°C under flow of reactants.

Learn more

Home-built noble-gas hyperpolarization setup

This setup allows the production of 129Xenon with the very high polarization.

It is mainly used for the study of the porous system of porous materials. It can also be used for other application in solution state NMR for instances.

Learn more

Related posts

[Position filled] 18-month fixed-term NMR engineer position

16 December 2018 | news,Platforms,nmr,Job opportunities at LCS | Christian FERNANDEZ

We propose, for the beginning of the year 2019, a position for an engineer for a project concerning the NMR (Nuclear Magnetic Resonance) of Hyperpolarized Xenon-129  financed by the Carnot Institute ESP (http://www.carnot-esp.fr) Project: Instrumental

Recrystallization on Alkaline Treated Zeolites in the Presence of Pore-Directing Agents

17 March 2018 | news,nmr | Christian FERNANDEZ

by Eddy Dib, Hussein El Siblani, Shrikant M Kunjir, Aurelie Vicente, Nicolas Nuttens, Danny Verboekend, Bert F Sels, and Christian Fernandez  in Cryst. Growth Des., DOI: 10.1021/acs.cgd.7b01416 Abstract Eddy Dib, Hussein El Siblani, Shrikant M

hpxenon

18 December 2016 | nmr | Christian FERNANDEZ

operando NMR

18 December 2016 | nmr | Christian FERNANDEZ

dehydration and adsorption setup for solid-state NMR

18 December 2016 | nmr | Christian FERNANDEZ

 

Copyright 2021 - Laboratoire Catalyse & Spectrochimie - Directeur de publication : Guillaume CLET | Creative Commons 4.0 International
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