Liquid- and solid-state 800MHz NMR spectrometer (USTL)
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…) and quadrupolar isotopes (27Al, 11B, 17O, …). 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 II 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:
- 4 mm HX (187W – 65Cu) MAS probe using Revolution NMR rotor;
- 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;
- 2.5 mm TriGamma HXY (1H/X=31P-13C/Y=15N-29Si) DVT MAS probe;
- 1.3 mm HX (14N-31P) DVT MAS probe;
- 4 or 3 mm HX (X=197Au-71Ga) PhoenixNMR static probe, temperature range: [-100; +150°C].
Prof. Olivier Lafon
Dr. Julien TREBOSC
Dr. Manjunatha Reddy