Liquid- and solid-state 800MHz NMR spectrometer (ULille)

NMR

Description

NMR spectroscopy is a powerful method to probe the atomic-scale structure and dynamics of a wide range of soft matter samples, including polymer materials, nanocomposites, gels, colloids, surfactant self-assemblies, biomacromolecules and liquid crystals. Because NMR gives information on the local atomic scale, it can easily characterize the bonding environment of atoms in soft materials, which often lack long-range positional order. Furthermore, NMR is a sensitive probe of local dynamics at atomic scale over timescales spanning 15 orders of magnitude, from 10^-12 s to 10² s. It can thus be used to study motions, including bond vibrations, conformational changes, rotational and translational motions of the molecules. 

This high-field (18.8 T) NMR spectrometer is equipped with 4 probes for liquids and 11 probes for solids. This instrument is notably equipped with 2 HRMAS probes, especially a 4 mm ¹H/¹³C/³¹P/²H HRMAS probe, which is not available on the 900 MHz spectrometer. This probe allows detecting ³¹P nuclei in soft materials, such as membranes. The large number of solid-state NMR probes available on this spectrometer allows the observation of the majority of NMR active isotopes in solids and the acquisition of a wide range of NMR experiments. In particular, this spectrometer is equipped with 7 triple-resonance MAS probes, which permits us to probe covalent bonds or proximities between two isotopes other than protons. We have notably developed powerful and efficient methods to probe proximities between spin-1/2 (³¹P, ¹³C, ²⁹Si, etc) and quadrupolar isotopes (²⁷Al, ¹¹B, ¹⁷O, etc). These methods are notably useful to investigate the structure of inorganic particles, such as those employed in nanocomposites. This spectrometer is also equipped with a frequency splitter, which permits to observe proximities between distinct isotopes, such as ¹³C, ²⁷Al, ⁵¹V, ²³Na or ⁴⁵Sc, with Larmor frequencies close to 200 MHz.

The specifications of the instrument are listed below:

Field: 18.8 T

Console: Bruker BioSpin Avance Neo 800 MHz 4 channels

Temperature: BCU 02 and nitrogen evaporator for variable temperature NMR experiments

Liquid-state NMR probes:

• 4 mm ¹H/¹³C/¹⁵N/²H HR-MAS probe with z-gradient, temperature range: [2; 50°C];
• 4 mm ¹H/¹³C/³¹P/²H HR-MAS probe with z-gradient, temperature range: [2; 50°C];
• 3 mm ¹H/BB/²H probe with z-gradient, temperature range: [-150; +180°C];
• 5 mm TXI ¹H/¹³C/¹⁵N/²H probe with z-gradient, temperature range: [-50; +80°C].

 

Solid-state NMR probes:

• 1.3 mm HX (¹⁴N-³¹P) DVT MAS probe;
• 1.6 mm PhoenixNMR HXYD (H=¹H-¹⁹F, X=³¹P – ²⁹Si, Y=²⁷Al – ¹⁰⁹Ag, lock channel), temperature range [-60; +120°C];
• 2.5 mm TriGamma HXY (¹H/X=³¹P-¹³C/Y=¹⁵N-²⁹Si) DVT MAS probe;
• 3.2 mm HX (¹⁵N – ³¹P) DVT MAS probe;
• 3.2 mm HX (¹⁸⁷W – ⁶⁵Cu) DVT MAS probe;
• 3.2 mm BP (³¹P / ⁷¹Ga,¹¹B,¹¹⁵Sn,⁸⁷Rb) VTN MAS probe with VESPEL stator (no ¹¹B background signal);
• 3.2 mm TriGamma HXY (¹H/¹³C/¹⁴N) DVT MAS probe;
• 3.2 mm TriGamma HXY (¹H/¹¹B/²⁹Si) DVT MAS probe;
• Two 3.2 mm TriGamma HXY (X = ³¹P-¹³C, Y = ¹⁵N-²⁹Si) DVT MAS probe;
• 3.2 mm HPX (¹H/³¹P/X = ⁹³Nb, ⁵¹V-²³Al) DVT MAS probe;
• 3,2 mm PhoenixNMR HXY (H=¹H-¹⁹F, X=³¹P – ²⁹Si, Y=²⁷Al – ¹⁰⁹Ag), temperature range [-30; +120°C]
• 4 or 3 mm HX (X=¹⁹⁷Au-⁷¹Ga) PhoenixNMR static probe, temperature range: [-100; +150°C];
• 4 mm HX (¹⁸⁷W – ⁶⁵Cu) MAS probe using Revolution NMR rotor.

 

Local Contacts

• Dr. Manjunatha Reddy
• Prof. Olivier Lafon
• Dr. Julien TREBOSC
• Dr. Bertrand Doumert

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