Probehead of an NMR-MAS apparatus with a device for determining the angle between the MAS rotor and the static magnetic field

Patent metadata

Field	Value
Publication number	US-9945654-B2
Application number	US-201715441991-A
Country	US
Kind code	B2
Filing date	Feb 24, 2017
Priority date	Feb 25, 2016
Publication date	Apr 17, 2018
Grant date	Apr 17, 2018

Abstract

A probehead of an NMR-MAS apparatus with a rotation axis (RA), which lies in an xz-plane, titled by an angle θ>0 relative to a z-axis. The angle θ is adjusted by tilting around a tilt axis (DA) parallel to the y-axis relative to a target angle θ target . An angle measurement apparatus ( 9 ) has a first sensor element ( 7 ), which, together with a second sensor element ( 8 ) generates sensor signals dependent on the amplitude B0 of the static magnetic field and the vectorial orientation between the magnetic field B0 and a sensitivity vector. Two sensitivity vectors have an angle 5°<αi<175° to the z-axis and an angle β>10° to each other. The angle between the rotation axis and the z-axis can be measured precisely and reliably over a large range, providing a feedback signal for regulated adjustment or tracking of the angle θ.

First claim

What is claimed is:

1. A probehead of a Nuclear Magnetic Resonance (NMR)-Magic Angle Spinning (MAS) apparatus, which is introduced in operation in a magnet system that generates a homogeneous static magnetic field B 0 along a z-axis, the probehead comprising:
a measurement sample with a rotation axis that lies in an xz-plane and is tilted at an angle θ>0 with respect to the z-axis, wherein the angle θ is configured to adjust by tilting the rotation axis around a tilt axis parallel to a y-axis to reach a tilt at which the angle θ equals a target angle θ target , and wherein z=0 is defined as a point of intersection of the rotation axis and the z-axis at the angle θ=θ target ; and
an angle measurement apparatus that generates a signal S(θ) dependent on the angle θ, the angle measurement apparatus comprising a plurality of sensor elements

wherein each sensor element of the plurality of sensor elements generates a sensor signal that depends on the amplitude of the homogenous static magnetic field B 0 and the angular orientation between the homogenous static magnetic field B 0 and a respective sensitivity vector associated with the sensor element, wherein each sensor element generates a maximum sensor signal when the respective sensitivity vector is oriented orthogonal to the homogenous static magnetic field B 0 , and wherein the signal S(θ) is a function of at least two sensor signals from at least two sensor elements associated with at least two respective sensitivity vectors, each of the at least two respective sensitivity vectors being oriented at an angle α i between 5° and 175° with respect to the z-axis, and wherein the at least two respective sensitivity vectors are oriented at an angle β>10° with respect to each other.

2. The probehead according to claim 1 , wherein each of the at least two respective sensitivity vectors are oriented at the angles α i between 30° and 60°.

3. The probehead according to claim 2 , wherein each of the at least two respective sensitivity vectors are oriented at the angles α i =45°.

4. The probehead according to claim 1 , wherein each of the plurality of sensor elements is mounted at an angle<45° with respect to the homogenous static magnetic field B 0 .

5. The probehead according to claim 4 , wherein each of the plurality of sensor elements is mounted at an angle<20° with respect to the homogenous static magnetic field B 0 .

6. The probehead according to claim 5 , wherein each of the plurality of sensor elements is mounted at an angle<10° with respect to the homogenous static magnetic field B 0 .

7. The probehead according to claim 6 , wherein each of the plurality of sensor elements is mounted at an angle<5° with respect to the homogenous static magnetic field B 0 .

8. The probehead according to claim 1 , further comprising an automated angle adjustment device for adjusting the angle θ based on the sensor signals.

9. The probehead according to claim 1 , wherein the plurality of sensor elements comprises at least two groups of at least two sensor elements that are interconnected such that a total of ratios of the sensor signals within each group of the at least two groups provides a regulating signal that adjusts or tracks the angle θ.

10. The probehead according to claim 1 , wherein the plurality of sensor elements are manufactured on a shared substrate or carrier.

11. The probehead according to claim 1 , further comprising a stator that is manufactured from a material with a first thermal conductivity λ 1 , wherein the plurality of sensor elements are attached to the stator through a connection with a second thermal conductivity λ 2 , and wherein the first thermal conductivity λ 1 and the second thermal conductivity λ 2 are each greater than 30 W/(m K).

12. The probehead according to claim 11 , wherein the first thermal conductivity λ 1 and the second thermal conductivity λ 2 are each greater than 100 W/(m K).

13. The probehead according to claim 12 , wherein the first thermal conductivity λ 1 and the second thermal conductivity λ 2 are each greater than 200 W/(m K).

14. The probehead according to claim 1 , wherein at least some of the plurality of sensor elements comprise Hall sensors.

15. The probehead according to claim 14 , wherein all of the plurality of sensor elements comprise Hall sensors.

16. The probehead according to claim 1 , wherein at least some of the plurality of sensor elements comprise magnetodiodes or magnetotransistors.

17. The probehead according to claim 16 , wherein all of the plurality of sensor elements comprise magnetodiodes or magnetotransistors.

18. The probehead according to claim 1 , wherein the plurality of sensor elements includes at least three sensor elements that have an identical design and have at least partly identical sensitivity vectors.

19. The probehead according to claim 1 , wherein at least two particular sensor elements of the plurality of sensor elements have a common sensitivity vector, and the at least two particular sensor elements are coupled orthogonally.

20. A Nuclear Magnetic Resonance (NMR) spectrometer comprising:
a magnet system configured to generate a homogeneous static magnetic field B 0 along a z-axis;
an NMR Magic Angle Spinning (MAS) apparatus for carrying out NMR-MAS measurements, the NMR-MAS apparatus comprising:
a rotatable mechanism with a stator carrying a movable rotor configured to support an NMR measurement sample; and
a probehead, which is introduced in operation in the magnet system and comprises:
a measurement sample with a rotation axis that lies in an xz-plane and is tilted at an angle θ>0 with respect to the z-axis, wherein the angle θ is configured to adjust by tilting the rotation axis around a tilt axis parallel to a y-axis to reach a tilt at which the angle θ equals a target angle θ target , and wherein z=0 is defined as a point of intersection of the rotation axis and the z-axis at the angle θ=θ target ; and
an angle measurement apparatus that generates a signal S(θ) dependent on the angle θ, the angle measurement apparatus comprising a plurality of sensor elements

wherein each sensor element of the plurality of sensor elements generates a sensor signal that depends on the amplitude of the homogenous static magnetic field B 0 and the angular orientation between the homogenous static magnetic field B 0 and a respective sensitivity vector associated with the sensor element, wherein each sensor element generates a maximum sensor signal when the respective sensitivity vector is oriented orthogonal to the homogenous static magnetic field B 0 , and wherein the signal S(θ) is a function of at least two sensor signals from at least two sensor elements associated with at least two respective sensitivity vectors, each of the at least two respective sensitivity vectors being oriented at an angle α i between 5° and 175° with respect to the z-axis, and wherein the at least two respective sensitivity vectors are oriented at an angle β>10° with respect to each other.

Assignees

• Bruker Biospin Ag

Inventors

• Freytag Nicolas

Classifications

• G01R33/46

  NMR spectroscopy · CPC title

• G01N24/087

  Structure determination of a chemical compound, e.g. of a biomolecule such as a protein · 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

• G01D5/145

  influenced by the relative movement between the Hall device and magnetic fields (see G01R33/06) · CPC title

• G01R33/38

  Systems for generation, homogenisation or stabilisation of the main or gradient magnetic field · CPC title