Sample extension on the sampling head side to reduce the B0 field disturbance at the end of the sample tube

Patent metadata

Field	Value
Publication number	US-11668774-B2
Application number	US-202117904654-A
Country	US
Kind code	B2
Filing date	Jan 29, 2021
Priority date	Feb 21, 2020
Publication date	Jun 6, 2023
Grant date	Jun 6, 2023

Abstract

An NMR apparatus having a magnet system for generating a homogeneous static magnetic field B 0 along a z direction, with a sampling head (1) comprising an RF transmitting and receiving coil system (2) and an opening (3) extending in the z direction for receiving a sample tube (4) containing a sample substance to be analyzed by means of NMR measurement, a compensation element (5) being present which at least partially compensates for disturbances in the homogeneous magnetic field B 0 due to the sample substance and the material of the sample tube at the sample end of the sample tube that protrudes farthest into the sampling head during measuring operation, is characterized in that the compensation element is arranged outside the sample tube protruding into the sampling head during measuring operation of the NMR apparatus and in the z direction below the sample end, and is mounted so as to be movable, in particular displaceable, in the z direction. Thus, the compensation element can nestle against the sample tube during operation without problem. In this way, the susceptibility jump and the resulting B 0 field disturbance in the lower region of the NMR-active sample liquid caused by the lower end of the sample tube are effectively minimizable with particularly uncomplicated technical means.

First claim

The invention claimed is:

1. A sampling head for an NMR apparatus comprising:
an RF transmission and reception coil system;
an opening extending in a z direction for receiving a sample tube containing a sample substance to be analyzed by means of NMR measurement; and
a compensation element which at least partially compensates for disturbances of a homogeneous magnetic field B 0 due to the sample substance and a material of the sample tube at a sampling end of the sample tube protruding into the sampling head during a measuring operation, the compensation element being arranged outside the sample tube and protruding into the sampling head during the measuring operation and in the z direction below the sampling end, and being movably mounted in the z direction on a spring device acting in the direction of the z axis or on an air cushion formed by a flow of temperature control gas in the sampling head.

2. The sampling head according to claim 1 , wherein the compensation element is mounted so as to be freely rotatable about the z axis and is able to rotate with the sample tube during the measuring operation.

3. The sampling head according to claim 1 , wherein the compensation element is hollow and is protected against uncontrolled removal from the sampling head by being firmly attached via a retaining element to the sampling head.

4. The sampling head according to claim 1 , wherein an upper stop for the compensation element is provided in the sampling head in the z direction.

5. The sampling head according to claim 1 , wherein the compensation element has gas passages on its outside in the form of longitudinal grooves parallel to the z direction and/or on the z axis in the form of an axial through-hole.

6. The sampling head according to claim 1 , wherein the compensation element has a susceptibility X which is between an average susceptibility of the sample tube and a typical susceptibility of the sample substance.

7. The sampling head according to claim 1 , wherein the compensation element has a susceptibility X and is configured to be exchangeable for another compensation element with a different susceptibility X′.

8. An NMR apparatus having a magnet system for generating homogeneous static magnetic field B 0 along a z direction, and comprising a sampling head according to claim 1 .

9. The NMR apparatus according to claim 8 , wherein the compensation element is configured to continue the cross-sectional geometry of the sample tube in the z direction.

10. The NMR apparatus according to claim 8 , wherein the compensation element has a contour that clings to a contour of the sample tube at the sampling end, wherein the sampling end of the sampling tube has a hemispherical shape and a portion of the compensation element opposite the sample tube is shaped like a hemispherical shell.

11. The NMR apparatus according to claim 8 , wherein the compensation element is formed from or coated with a material which minimizes a frictional resistance between the compensation element and the sample tube resting against it during the measuring operation, the material having an average susceptibility X between 0.4 cgs and 0.8 cgs.

12. The NMR apparatus according to claim 8 , wherein the compensation element is configured to allow a fluid flow of temperature control gas from the compensation element into an annular gap between an outer shell of the sample tube protruding into the sampling head during the measuring operation and a wall element surrounding the sample tube, which carries the RF transmitting and receiving coil system.

Assignees

• Bruker Switzerland Ag

Inventors

• Schmidig Daniel

Classifications

• G01R33/31 Primary

  Temperature control thereof · CPC title

• G01R33/30 Primary

  Sample handling arrangements, e.g. sample cells, spinning mechanisms · 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