MAS-stator with suctioning-off device

Patent metadata

Field	Value
Publication number	US-10132881-B2
Application number	US-201615152573-A
Country	US
Kind code	B2
Filing date	May 12, 2016
Priority date	May 13, 2015
Publication date	Nov 20, 2018
Grant date	Nov 20, 2018

Abstract

An MAS stator ( 7 ) for an NMR-MAS probe head ( 1 ) has a bottom bearing ( 8 ) with at least one nozzle and at least one radial bearing ( 9 a, 9 b ), wherein one substantially circular cylindrical MAS rotor ( 21 c ) is provided for receiving a measurement substance. The MAS rotor can be supported by compressed gas in a measurement position within the MAS stator by means of a gas supply device and can be rotated about the cylinder axis of the MAS rotor by means of a pneumatic drive. A suction device ( 100 ) is provided in a space below the radial bearing for suctioning-off the gas introduced by the gas supply device, and generates an underpressure in the space below the radial bearing during measurement operation. This provides a stator for NMR-MAS spectroscopy in which the closure at the head end of the stator is omitted.

First claim

We claim:

1. An MAS stator for an NMR-MAS probe head, the stator structured to cooperate with a substantially circular cylindrical MAS rotor having a cylinder axis, the MAS rotor structured for receiving a measurement substance, the stator comprising:
a bottom bearing with at least one nozzle and at least one radial bearing;
a gas supply device structured to support the MAS rotor with compressed gas in a measurement position within the MAS stator;
a pneumatic drive structured to rotate the MAS rotor about the cylinder axis thereof; and
a suction device, said suction device disposed in a space below said radial bearing and structured for suctioning-off gas introduced by said gas supply device, wherein said suction device is designed to generate an underpressure with respect to an atmosphere surrounding the MAS stator in said space below said radial bearing and during measurement operation.

2. The MAS stator of claim 1 , wherein the MAS stator is designed to receive an MAS rotor having a diameter of 0.2 mm to 2.5 mm or of 0.7 mm to 1.9 mm.

3. The MAS stator of claim 1 , wherein said suction device has a gas line for suctioning-off gas introduced by said gas supply device, said gas line having a cross-section of 0.2 mm 2 to 100 mm 2 or of 1.5 mm 2 to 10 mm 2 .

4. The MAS stator of claim 1 , wherein said suction device is structured to accept an underpressure load during measurement operation with respect to the atmosphere surrounding the MAS stator of −0.1 bar to −1 bar.

5. The MAS stator of claim 1 , wherein said nozzle in said bottom bearing has an inner diameter of between 25 μm and 500 μm or of between 80 μm and 200 μm.

6. The MAS stator of claim 1 , wherein said gas supply device comprises only one single nozzle in said bottom bearing, that nozzle commonly supplying gas for a pressure gas bearing as well as gas for said pneumatic drive for rotation of the MAS rotor during operation.

7. The MAS stator of claim 1 , further comprising an additional device for supplying gas to the MAS rotor in order to keep the measurement substance at a predeterminable operating temperature during measurement operation.

8. The MAS stator of claim 1 , wherein the MAS stator is structured to rotate for adjusting an MAS angle.

9. A probe head comprising the MAS stator of claim 1 , further comprising a pneumatic sample changing system having a transport line for supplying and discharging the MAS rotor to the MAS stator.

10. The probe head of claim 9 , wherein, when said suction device is switched off, said nozzle in said bottom bearing is a component of said pneumatic sample changing system by means of which the MAS rotor can be ejected from the MAS stator.

11. A method for operating the probe head of claim 9 , wherein, after positioning the MAS rotor in the MAS stator, said suction device is initially started before compressed gas is supplied to said bottom bearing such that the MAS rotor remains in the MAS stator and can rotate in a more vibration-free manner.

12. The method of claim 11 , wherein, after termination of an NMR measurement, underpressure generation by said suction device is switched off, said gas supply device supplies compressed gas to said bottom bearing and an overpressure is built up in said space below said radial bearing thereby ejecting the MAS rotor out of the measurement position.

13. The method of claim 11 , wherein the MAS rotor has a diameter of 0.2 mm to 2.5 mm or of 0.7 mm to 1.9 mm.

Assignees

• Bruker Biospin Gmbh

Inventors

• Osen David
• Knott Benno
• Purea Armin

Classifications

• G01R33/307 Primary

  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

• G01R33/302

  Miniaturized sample handling arrangements for sampling small quantities, e.g. flow-through microfluidic NMR chips · CPC title

• G01R33/44

  using nuclear magnetic resonance [NMR] (G01R33/24, G01R33/62 take precedence) · CPC title