Temperature control of an NMR-MAS rotor

Patent metadata

Field	Value
Publication number	US-10459044-B2
Application number	US-201715718723-A
Country	US
Kind code	B2
Filing date	Sep 28, 2017
Priority date	Sep 28, 2016
Publication date	Oct 29, 2019
Grant date	Oct 29, 2019

Abstract

A method for operating an NMR probehead ( 10 ) with an MAS stator ( 11 ) receiving a circular-cylindrical hollow MAS rotor ( 13 ) with an outer jacket. The MAS rotor is mounted on pressurized gas in a measuring position within the MAS stator via a gas supply device with a bearing nozzle ( 12 ′) and rotates about the cylinder axis of the MAS rotor at a rotation frequency f≥30 kHz. During a measurement, a temperature control gas is blown by a temperature control nozzle ( 12 ) onto the outer jacket of the rotor at an angle α<90° with respect to the longitudinal axis of the cylinder-symmetrical rotor. The flow speed of the temperature control gas corresponds in the nozzle cross section to at least half the circumferential speed of the outer jacket of the rotating rotor and to at most the speed of sound in the temperature control gas.

First claim

What is claimed is:

1. A method for operating a Nuclear Magnetic Resonance (NMR) probehead having a Magic-Angle-Spinning (MAS) stator configured to receive a substantially circular-cylindrical hollow MAS rotor with an outer jacket of external diameter D and with a sample substance in a sample volume, comprising:
mounting the MAS rotor on pressurized gas in a measuring position within the MAS stator via a gas supply device having a bearing nozzle, and
rotating the MAS rotor about a cylinder axis of the MAS rotor with a pneumatic drive at a rotation frequency f≥30 kHz,
during an NMR-MAS measurement, blowing a temperature control gas with a temperature control nozzle onto an outer jacket of the MAS rotor at an angle α<90° with respect to a longitudinal axis of the cylinder-symmetrical MAS rotor, and
regulating a flow speed of the temperature control gas blown through the temperature control nozzle onto the MAS rotor to correspond in the nozzle cross section to at least half a circumferential speed of the outer jacket of the rotating MAS rotor and to at most an upper limit of the circumferential speed of the outer jacket of the rotating MAS rotor.

2. The method as claimed in claim 1 , wherein the outer jacket of the MAS rotor has an external diameter D≤1.9 mm, and the MAS rotor is rotated at a rotation frequency f≥50 kHz.

3. The method as claimed in claim 2 , wherein the MAS rotor is rotated at a rotation frequency f≥67 kHz.

4. The method as claimed in claim 1 , wherein a standard volumetric flow of the temperature control gas blown through the temperature control nozzle is between 0.01 l/min and 10 l/min.

5. An MAS stator configured to carry out the method as claimed in claim 1 , with a temperature control device which comprises at least one temperature control nozzle configured to control the temperature of the MAS rotor, wherein the at least one temperature control nozzle has an internal diameter d of between 0.04 mm and 0.5 mm, and wherein a pressure of between 1 bar to 5 bar is applied to the temperature control nozzle.

6. An NMR-MAS probehead with an MAS stator as claimed in claim 5 , wherein the outer jacket of the MAS rotor has an external diameter D≤1.9 mm and wherein the MAS rotor is rotated at a rotation frequency f≥67 kHz.

7. The NMR-MAS probehead with an MAS stator as claimed in claim 6 , wherein the outer jacket of the MAS rotor has an external diameter 0.7 mm≤D≤1.3 mm.

8. The NMR-MAS probehead as claimed in claim 6 , wherein the MAS stator has an open construction, such that a stream of temperature control gas escapes into the environment after contacting the outer jacket of the MAS rotor, and wherein the temperature control nozzle is arranged such that the stream of temperature control gas is blown onto the outer jacket of the MAS rotor at an angle α≤45° relative to the longitudinal axis of the cylinder-symmetrical MAS rotor.

9. The NMR-MAS probehead as claimed in claim 8 , wherein the temperature control nozzle is arranged such that the stream of temperature control gas is blown onto the outer jacket of the MAS rotor at an angle α≤30° relative to the longitudinal axis of the cylinder-symmetrical MAS rotor.

10. The NMR-MAS probehead as claimed in claim 6 , wherein the MAS stator has a closed construction, such that a stream of temperature control gas cannot escape directly into the environment after contacting the outer jacket of the MAS rotor, and wherein the temperature control nozzle is arranged such that an angle α relative to the longitudinal axis of the cylinder-symmetrical MAS rotor ( 43 ) is α≤10°.

11. The NMR-MAS probehead as claimed in claim 10 , wherein a gap with a gap width b of between 0.02 mm and 0.3 mm is left free for the stream of temperature control gas between the outer jacket of the MAS rotor and the surrounding inner surface of the MAS stator.

12. The NMR-MAS probehead according to claim 10 , wherein the temperature control nozzle is arranged such that a stream of temperature control gas is blown along the outer jacket of the MAS rotor at an angle α≈0°, which is parallel to the longitudinal axis of the cylinder-symmetrical MAS rotor.

13. The NMR-MAS probehead as claimed in claim 6 , wherein the MAS rotor is surrounded by a solenoid-shaped RF coil which is wound onto the outer face of a tube and is arranged such that the stream of temperature control gas is guided between the rotor and the tube.

14. The NMR-MAS probehead according to claim 13 , wherein the MAS rotor is surrounded by the solenoid-shaped RF coil at a distance of between 0.02 mm and 0.3 mm from the inner wall of the tube.

15. The NMR-MAS probehead as claimed in claim 6 , further comprising further temperature control nozzles, wherein the temperature control nozzles are arranged about the longitudinal axis of the cylinder-symmetrical MAS rotor.

16. The NMR-MAS probehead as claimed in claim 15 , wherein the temperature control nozzles are of identical configuration to each other and are arranged symmetrically about the longitudinal axis of the cylinder-symmetrical MAS rotor.

17. The NMR-MAS probehead as claimed in claim 6 , wherein the temperature control nozzle is built into a radial bearing of the MAS rotor.

18. The NMR-MAS probehead as claimed in claim 6 , wherein the temperature control nozzle is supplied with temperature control gas via a separate line.

19. The NMR-MAS probehead as claimed in claim 6 , wherein the MAS rotor is constructed from sapphire, tetragonally stabilized zirconium oxide and/or silicon nitride, with a wall thickness of between 0.2 mm and 0.7 mm.

Assignees

• Bruker Biospin Gmbh

Inventors

• Osen David
• Purea Armin
• Knott Benno
• KUEHLER Fabian
• Helbing Florian
• Hassan Alia
• Guidoulianov Jevgeni
• Freytag Nicolas

Classifications

• G01R33/31 Primary

  Temperature control thereof · CPC title

• G01R33/307

  specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer · CPC title