JP3876103B2 - Method and tool for operating NMR sample tube - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an operation method of an NMR sample tube used when an NMR sample tube is introduced into or removed from an NMR detector in an NMR apparatus, and particularly, the risk of damage to the NMR sample tube is greatly increased. The present invention relates to a method of operating an NMR sample tube that can be reduced to a minimum.
[0002]
[Prior art]
FIG. 1 shows the structure of the main part of a conventional NMR apparatus. An NMR detector 2 is set in the vertical hole portion of the superconducting magnet 1 that generates a strong static magnetic field. An NMR sample tube 3 containing a liquid sample is set in the NMR detector 2. Furthermore, the spinner rotor 4 used for rotating the NMR sample tube 3 at the time of NMR measurement is attached to the NMR sample tube 3 for the purpose of sharpening the linearity of the NMR signal.
[0003]
As apparent from FIG. 1, the NMR detector 2 is inserted deep in the vertical hole of the superconducting magnet 1, and the NMR sample tube 3 is inserted into the head of the NMR detector 2, so that it is usually external. Can not be withdrawn by hand. For this reason, a housing 5 is provided along the vertical hole of the superconducting magnet 1 as a passage for taking in and out the NMR sample tube 3 and is connected to the head of the NMR detector 2.
[0004]
When the NMR sample tube 3 is introduced into the NMR detector 2, air is previously fed into the housing 5 from the lower air supply port 6 using a compressor (not shown), and the NMR sample tube 3 is opened at the upper end of the housing 5 by the air pressure. The NMR sample tube 3 is lowered along the housing 5 to the position of the NMR detector 2 by allowing it to float in the vicinity and then lowering the air pressure. Further, when the NMR sample tube 3 is taken out from the NMR detector 2, air is sent from an air supply port 6 below the NMR detector 2 by a compressor (not shown), and the NMR sample tube 3 is floated along the housing 5 by the air pressure. Then, it is moved to the opening at the upper end of the housing 5.
[0005]
During these operations, the buoyancy due to the air pressure is received mainly by the portion of the spinner rotor 4 attached to the NMR sample tube 3, so that in order to obtain a good descent / levitation operation, the inner periphery of the housing 5 is used. It is important that the clearance between the portion and the outer peripheral portion of the spinner rotor 4 is appropriately provided.
[0006]
However, the presence of this clearance, on the contrary, may cause the shaft shake of the NMR sample tube 3 during the descent / levitation operation. The bottom of the NMR sample tube 3 often comes into contact with the inlet of the NMR detector 2 due to shaft wobbling, and sometimes the NMR sample tube 3 is broken. This is an unavoidable difficulty as long as a pneumatic sample introduction mechanism is used, and in many cases, by slowing the descent and levitation of the NMR sample tube 3, the probability of this breakage is lowered. I have to.
[0007]
[Problems to be solved by the invention]
In such a configuration, the normal NMR measurement is made so that the probability of breakage of the NMR sample tube 3 as described above is sufficiently small. However, in recent years, the following new situations have arisen.
[0008]
(1) In order to ensure detection sensitivity when measuring a very small amount of a valuable sample with a low yield, an extremely thin NMR sample tube and a thin NMR detector that matches the outer diameter of the sample tube may be used.
[0009]
(2) When a weak NMR signal is observed, an extremely thin NMR sample tube may be used in order to improve detection sensitivity.
[0010]
(3) Samples that are not allowed to be scattered in the environment, such as radioactive substances, may be measured.
[0011]
Among these, in the cases of (1) and (2), the probability of breakage of the NMR sample tube is greatly deteriorated. In the case of (1) and (3), even if the probability is small, the probability of damage of the NMR sample tube cannot be ignored.
[0012]
The object of the present invention is to provide an NMR sample that can greatly reduce the risk of damage to the NMR sample tube when the NMR sample tube is introduced into or removed from the NMR detector. It is to provide a tube setting method.
[0013]
[Means for Solving the Problems]
In order to achieve this object, the method of operating an NMR sample tube according to the present invention includes an NMR sample tube equipped with a spinner rotor between an NMR detector installed inside the superconducting magnet and the outside of the superconducting magnet. A method of operating an NMR sample tube for taking in and out,
The upper part of the spinner rotor that is in contact with the NMR sample tube is provided with a hole that opens upward, a fitting part is provided on the inner periphery of the spinner rotor side, and an operating rod is fitted to the fitting part. It is characterized in that to carry out the loading and unloading of the NMR sample tube by.
[0014]
In addition, the NMR sample tube is operated using an operation rod for inserting and removing the NMR sample tube equipped with the spinner rotor between the NMR detector installed inside the superconducting magnet and the outside of the superconducting magnet. And
The operation rod has a double cylinder structure including an inner cylinder and an outer cylinder, and a protrusion provided on the inner cylinder protrudes from a window provided on the outer cylinder, and is fitted into a groove provided on the spinner rotor. It is characterized by the fact that they are combined .
[0015]
An NMR sample tube operation tool for inserting and removing the NMR sample tube equipped with the spinner rotor between the NMR detector installed inside the superconducting magnet and the outside of the superconducting magnet,
An operating rod having a fitting portion that can be fitted to a fitted portion provided on the spinner rotor side, and the operating rod is foldable provided on the inner cylinder, the outer cylinder, and the inner cylinder. It is characterized by comprising a projection and a window provided on the outer cylinder for projecting the projection .
[0016]
Moreover, the operation rod is characterized that you have made of non-magnetic material that is not attracted by the magnetic force.
[0019]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention will be described below with reference to the drawings. FIG. 2 shows an embodiment of the operating rod for the NMR sample tube used in the present invention. In the figure, (a) is a cross-sectional view of the operating rod used in the present invention, (b) is an external view of components constituting the operating rod used in the present invention, and (c) is a cross-sectional view of the spinner rotor used in the present invention. FIG.
[0020]
In this embodiment, as shown in FIGS. 2 (a) and 2 (b), an operating rod having a double tube structure comprising an inner cylinder 7 and an outer cylinder 8 having an inner diameter slightly larger than the outer diameter of the inner cylinder 7 is provided. Use. Several protrusions (convex portions) 9 are provided at the front end portion of the inner cylinder 7 at equal intervals along the outer periphery of the cylinder. Further, the same number of windows 10 as the number of projections 9 are provided at the tip of the outer cylinder 8 at positions corresponding to the positions of the projections 9 provided at the tip of the inner cylinder 7. 7 projections 9 are formed so as to pass through the window 10 and protrude toward the outside of the outer cylinder 8. They are made of non-magnetic materials that are not attracted by magnetic forces for use in strong magnetic fields.
[0021]
The protrusion 9 of the inner cylinder 7 protruding outward from the window 10 of the outer cylinder 8 is folded inside the inner cylinder 7 when the inner cylinder 7 is rotated in the circumferential direction in the outer cylinder 8, The tube 8 is configured to be retracted inward from the window 10. Further, when the inner cylinder 7 is further rotated so that the position of the protrusion 9 once retracted matches the position of the window 10 of the outer cylinder 8, the protrusion 9 again protrudes outward from the window 10 of the outer cylinder 8. It is configured.
[0022]
FIG. 2C shows the spinner rotor 4 mounted on the NMR sample tube 3. As shown in FIG. 2 (c), the spinner rotor 4 used in this embodiment includes a hole 11 that can be inserted into the tip of the operation rod, and a groove (carved on the inner wall of the hole 11). (Concave portion) 12. The groove 12 is formed in a size that allows the projection 9 protruding from the tip of the operation rod to be fitted. The present spinner rotor 4 is not different from the conventional spinner rotor except that the groove portion 12 is provided on the inner wall of the hole portion 11.
[0023]
The setting operation of the NMR sample tube is performed as follows. First, the spinner rotor 4 is attached to the NMR sample tube 3. Next, with the projection 9 of the inner cylinder 7 of the operation rod folded inward from the window 10 of the outer cylinder 8, the tip of the operation rod is inserted into the hole 11 of the spinner rotor 4. Next, the inner cylinder 7 is rotated in the circumferential direction so that the protrusion 9 protrudes outward from the window 10 of the outer cylinder 8 and is fitted into the groove 12 of the spinner rotor 4. As a result, the NMR sample tube 3 and the spinner rotor 4 are fixed and held at the tip of the operation rod. Therefore, the operation rod is inserted from the opening at the upper end of the housing 5 toward the NMR detector 2, and the NMR detector is inserted. An NMR sample tube 3 and a spinner rotor 4 are set on the head of 2. Finally, the inner cylinder 7 is rotated in the circumferential direction, the projection 9 is folded inward from the window 10 of the outer cylinder 8, the NMR sample tube 3 and the spinner rotor 4 are separated from the operation rod, and the operation rod is pulled out.
[0024]
When taking out the NMR sample tube 3 and the spinner rotor 4 from the NMR detector 2, the operation is performed in the reverse order. That is, first, in a state where the projection 9 of the inner cylinder 7 of the operating rod is folded inward from the window 10 of the outer cylinder 8, the operating rod is directed from the opening at the upper end of the housing 5 toward the NMR detector 2. Is inserted, and the tip is inserted into the hole 11 of the spinner rotor 4 set at the head of the NMR detector 2. Next, the inner cylinder 7 is rotated in the circumferential direction so that the protrusion 9 protrudes outward from the window 10 of the outer cylinder 8 and is fitted into the groove 12 of the spinner rotor 4. As a result, the NMR sample tube 3 and the spinner rotor 4 are fixed and held at the tip of the operation rod, so that the operation rod is pulled out from the NMR detector 2 toward the opening at the upper end of the housing 5 to obtain the NMR detector. The NMR sample tube 3 and the spinner rotor 4 are taken out from the head of 2. Finally, the inner cylinder 7 is rotated in the circumferential direction, the projection 9 is folded inward from the window 10 of the outer cylinder 8, and the NMR sample tube 3 and the spinner rotor 4 are separated from the operation rod.
[0025]
Various modifications can be made to the present invention. For example, in this embodiment, the convex portion is provided on the operating rod side and the concave portion is provided on the spinner rotor side, but this may be reversed. Further, in this embodiment, the operation rod is configured to have a double cylinder structure so that the protrusions can be taken in and out. However, this operation is not necessarily performed unless the double cylinder structure is used, and this operation is performed in a single way. You may make it carry out with a cylinder structure. For example, protrusions that can be taken in and out are provided at equal intervals on the tip of the cylinder, and the protrusions are usually stored inside the cylinder. When necessary, the protrusion is projected toward the outside of the cylinder by pushing with a stick from the inside of the cylinder.
[0026]
【The invention's effect】
As described above, according to the method of operating the NMR sample tube of the present invention, instead of the conventional method using air pressure, the operation rod is used to introduce the NMR sample tube into the NMR detector and from the NMR detector. Since the extraction is performed, it is possible to greatly reduce the risk of the NMR sample tube being damaged when the NMR sample tube is introduced into the NMR detector or removed from the NMR detector.
[Brief description of the drawings]
FIG. 1 is a diagram showing the configuration of a conventional NMR apparatus.
FIG. 2 is a diagram showing an embodiment of a method for setting an NMR sample tube according to the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Superconducting magnet, 2 ... NMR detector, 3 ... NMR sample tube, 4 ... Spinner rotor, 5 ... Housing, 6 ... Air inlet, 7 ... Inner cylinder 8 ... outer cylinder, 9 ... projection, 10 ... window, 11 ... hole, 12 ... groove.

Claims (4)

An NMR sample tube operating method for inserting and removing an NMR sample tube equipped with a spinner rotor between an NMR detector installed inside a superconducting magnet and the outside of the superconducting magnet,
The upper part of the spinner rotor that is in contact with the NMR sample tube is provided with a hole that opens upward, a fitting part is provided on the inner periphery of the spinner rotor side, and an operating rod is fitted to the fitting part. The method for operating an NMR sample tube, wherein the NMR sample tube is taken in and out. An NMR sample tube operation method using an operation rod for inserting and removing an NMR sample tube equipped with a spinner rotor between an NMR detector installed inside the superconducting magnet and the outside of the superconducting magnet,
The operation rod has a double cylinder structure including an inner cylinder and an outer cylinder, and a protrusion provided on the inner cylinder protrudes from a window provided on the outer cylinder, and is fitted into a groove provided on the spinner rotor. A method for operating an NMR sample tube, characterized in that the two are combined. An NMR sample tube operating tool for taking in and out an NMR sample tube equipped with a spinner rotor between an NMR detector installed inside a superconducting magnet and the outside of the superconducting magnet,
Ri operating rod der having a fitted portion to be fitted to the fitting portion provided in the spinner rotor side,該操Sakubo includes an inner cylinder, an outer cylinder, foldable provided on the inner cylinder Do projection and, the operation tool of NMR sample tube, wherein forming isosamples a window portion provided on the outer tube in order to project the protrusion portion. 4. The NMR sample tube operating method or operation tool according to claim 1, wherein the operating rod is made of a nonmagnetic material that is not attracted by magnetic force.

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