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Liquid Overhauser DNP

600MHz DNP Instruments

A liquid Overhauser DNP instrument at 14.1 T is currently in its final development stage to measure small molecules applied to areas of research such as natural products, metabolomics.

A 14T liquid DNP spectrometer was built to develop new methods with the goal to increase the signal to noise ratio of measurements in liquid nuclear magnetic resonance.

This system shares a gyrotron, the 395 GHz microwave source, with the MAS-DNP NMR user instrument. The NMR part of the instrument is performed using a Tecmag console (3 channels with a lock) in combination with an Oxford Instruments 51-mm bore 14.1-T magnet. Two liquid DNP probes are available, a 3-mm HCN and a 3-mm XH. Both probes are fitted with sweep coils to fine tune the magnetic field to match the resonant conditions of the radical used.


Specs

The Overhauser DNP spectrometer is not part of the user program (yet). This instrument is currently in its final development stage to measure small molecules applied to areas of research such as natural products, metabolomics.

  • Frequency: 395 GHz for electron, 600 MHz for 1H
  • Field Strength: 14.1 tesla
  • Bore Diameter: 38mm
  • Homogeneity: 0.01ppm
  • Console: Tecmag Redstone
  • Temperature: 0 – 45 °C
  • Temperature range: 263 – 323 K
  • Sample Type: liquids, supercritical fluids
  • Pressure: up to 100 bar (supercritical fluids)
  • Gyrotron microwave source with quasi-optic stable: 0 – 30 W microwave power

Solution-State NMR Technique

Two liquid DNP probes are available, a 3-mm HCN and a 3-mm XH. Both probes are fitted with sweep coils to fine tune the magnetic field to match the resonant conditions of the radical used. The mail coil is set close to TEMPO (g = 2.006) while the sweep coil allows us to reach BDPA (g = 2.0026) in liquids. Note that as a large sweep coil set point decreases the field homogeneity at the sample to about 0.2 ppm.

A broad variety of standard chemistry laboratory equipment is available to prepare and store samples, such as a glovebox, - 80°C freezer, microliter volume pipettes.

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Credit: National MagLab


Last modified on 08 December 2023

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