JP2007033110A - Nmr apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an NMR apparatus safely and reliably inserting and extracting a sample tube containing a test sample into and out of a sample tube arrangement space located in a center part of a magnet without causing any damage. <P>SOLUTION: One exposed side part of the sample tube 53 to which a holder 50 is mounted is covered with partial protective tubes 59 and 58. When the sample tube 53 is arranged in the arrangement space 10, the partial protective tubes 59 and 58 are housed in the holder 50 and the partial protective tubes 59, and only the sample tube 53 is arranged. When a specimen part 5 is inserted and extracted into and out of the NMR apparatus 1, the sample tube 53 is prevented from being damaged due to unintentional impact of collision etc. and simultaneously perform NMR inspection through the use of the sample tube 53 without degrading sensitivity, resolution, etc. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to an NMR apparatus that transmits and receives an RF signal by arranging a sample tube containing a test sample in the center of a cylindrical space in a vertically hollow state where a uniform static magnetic field is formed.

  In recent years, NMR (Nuclear Magnetic Resonance) devices have been used to increase the static magnetic field applied to samples, to reduce the amount of samples, and to diversify samples in order to achieve higher resolution and higher sensitivity as analytical devices. Yes.

  Here, the NMR apparatus has a magnet that generates a static magnetic field in the vertical direction, and this magnet has a cylindrical space in a cylindrical state along the central axis in the vertical direction. A static magnetic field with high magnetic field uniformity is formed in this cylindrical space, and an operator arranges a rod-shaped sample tube filled with a test sample in the vicinity of the center position with the best magnetic field uniformity in this cylindrical space. To do. On the other hand, an arrangement space having a small inner diameter for arranging the sample tube is formed in the vicinity of the center position of the cylindrical space.

  Here, when the sample tube is inserted into the cylindrical space and the arrangement space, an unintended collision with the wall surfaces constituting the cylindrical space and the arrangement space occurs, and the sample tube is damaged. In order to prevent this collision, for example, a telescopic holder used in an electron spin resonance apparatus is used (for example, see Patent Document 1).

  However, for example, in an NMR apparatus having a magnet having a static magnetic field strength of about 14 T (Tesla), the cylindrical space has a diameter of about 5 to 6 cm and a vertical length of about 1 to 2 m. The space has a small diameter of 10 mm or less. Therefore, it is difficult for the operator to place the sample tube directly in his / her hand in the arrangement space near the center position of the cylindrical space.

  In addition, since the test sample is sealed in a sample tube made of a glass tube having a diameter of about 3 to 5 mm, for example, the test sample is vulnerable to impact and easily damaged by an unintended collision or the like, and the test sample leaks into the cylindrical space. It also happens. The sample tube is also equipped with a holder that safely holds the glass tube and a spinner rotor that rotates the sample tube in the cylindrical space together with the holder.

  Therefore, in order to arrange the sample tube accurately and safely in the arrangement space located near the center position of the cylindrical space that cannot be reached by the operator, (1) air is compressed from below in the cylindrical space with a compressor or the like. For example, (2) using an operating rod with a sample tube attached to the tip.

  In the case of (1) described above, the operator inserts the holder holding the sample tube and the spinner rotor from vertically above the cylindrical space. Here, the holder and the spinner rotor form a highly airtight space in the cylindrical space by the housing part mounted on the inner wall of the cylindrical space and the RF transmitting / receiving part fixedly arranged vertically below the cylindrical space. As a result, the holder and the spinner rotor are substantially suspended at an intermediate position in the cylindrical space without falling to the center position of the cylindrical space. Then, the operator adjusts the amount of air flowing in by the compressor, in other words, the air pressure in the highly airtight space, so that the spinner rotor on which the sample tube is mounted is disposed near the center position of the cylindrical space. It can be safely lowered into the space, and conversely, the spinner rotor equipped with the sample tube in the arrangement space can be raised vertically above the cylindrical space.

In the case of (2) described above, the operator fits the holder holding the sample tube and the spinner rotor in advance with the tip of the operating rod, and inserts the operating rod vertically from above the cylindrical space. Here, the operation rod becomes long and heavy in order to lower the spinner rotor to the vicinity of the center position of the cylindrical space and dispose the sample tube.
Japanese Utility Model Publication No. 60-134150, (pages 2 and 3, Fig. 2)

  However, according to the above background art, the sample tube containing the test sample may be damaged. That is, in the case of (1) described above, the spinner rotor to which the sample tube is mounted has a slight play space between the housing portion forming the wall surface and is lowered in the cylindrical space by adjusting the air pressure. In this case, the sample tube position located on the central axis of the cylindrical space is blurred. Then, the sample tube whose center axis is deviated may come into contact with and be damaged at the entrance of a small arrangement space.

  In the case of (2) described above, the operating rod is long and heavy, whereas the sample tube attached to the tip of the operating rod is small and fragile. Therefore, inserting an operating rod from vertically above the cylindrical space and inserting the sample tube at the tip into a small arrangement space near the center of the cylindrical space requires high skill and concentration. There is a great burden on the operator.

  In particular, the NMR apparatus is required to have a high static magnetic field strength in order to achieve high resolution and high sensitivity, and therefore the magnet tends to be large. Therefore, the cylindrical space in the magnet tends to be long in the vertical direction, and it is becoming increasingly difficult to dispose the sample tube in a small disposition space.

  Further, from the viewpoint of improving the sensitivity of the NMR apparatus, it is preferable that the diameter of the arrangement space is reduced and the coil is arranged close to the sample tube. At the same time, sample tubes are becoming smaller and more fragile due to the small amount of test samples.

In addition, when a dangerous substance such as a radioactive substance is used in accordance with the diversification of inspection samples, breakage of the sample tube in the cylindrical space causes leakage of the dangerous substance, which is particularly undesirable.
From these facts, it is important how to realize an NMR apparatus that can safely and reliably put in and out the sample tube containing the test sample in the space where the sample tube located in the center of the magnet is not damaged. Become.

  The present invention has been made to solve the above-described problems caused by the background art, and the sample tube containing the test sample can be safely and reliably damaged without being damaged in the arrangement space of the sample tube located at the center of the magnet. An object of the present invention is to provide an NMR apparatus that can be taken in and out.

  In order to solve the above-described problems and achieve the object, an NMR apparatus according to the invention described in claim 1 includes a static magnetic field generation unit having a cylindrical space in a cylindrical state in a vertical direction in which a uniform static magnetic field is formed. An object part having a rod-shaped sample tube containing a test sample, which is inserted from above in the cylindrical space, and a vertical center of the cylindrical space, which is fixedly arranged at a substantially intermediate position in the vertical direction of the cylindrical space. And an RF signal transmission / reception unit having a cylindrical arrangement space in which the sample tube is arranged along an axis, wherein the subject unit is a cylindrical protective tube containing the sample tube And when the sample tube is inserted into the arrangement space, the protective tube is provided with a remaining means for remaining in the cylindrical space vertically above the arrangement space.

  According to the first aspect of the present invention, the subject portion includes the sample tube by the cylindrical protective tube, and when the sample tube is inserted into the arrangement space, the protective tube is disposed by the remaining means. It remains in the cylindrical space vertically above the installation space.

  The NMR apparatus according to claim 2 is the NMR apparatus according to claim 1, wherein the residual means protects the sample tube when the sample tube is pulled out from the arrangement space. It is included in a tube.

In the invention according to claim 2, the residual means repeatedly includes the sample tube with the protective tube.
The NMR apparatus according to the invention described in claim 3 is the NMR apparatus according to claim 1 or 2, wherein the subject portion partially includes one end portion of the rod-shaped sample tube, and It is characterized by comprising a holder that compresses and holds the tube wall of the sample tube evenly.

In the invention according to claim 3, the subject part partially encloses one end portion of the rod-shaped sample tube by the holder and holds the sample tube.
According to a fourth aspect of the present invention, in the NMR apparatus of the third aspect, the subject portion has a hollow cylindrical housing portion sharing a central axis in the cylindrical space. In this case, it is provided with a cylindrical holder holding means for holding and rotating the holder around the central axis and having an outer diameter that approximates the inner diameter in a direction orthogonal to the central axis of the housing portion. And

In the invention according to the fourth aspect, the subject portion is brought into a state close to the housing portion by the holder holding means.
The NMR apparatus according to the invention described in claim 5 is the NMR apparatus according to claim 3 or 4, wherein the protective tube includes one end portion that is not included in the holder of the rod-shaped sample tube. It is characterized by.

In the invention according to the fifth aspect, the protective tube includes one end of the sample tube.
In addition, the NMR apparatus according to the invention described in claim 6 is the NMR apparatus according to claim 5, wherein the residual means is a slide for taking the protection tube in and out of a gap portion sandwiched between the holder and the sample tube. Means are provided.

In the invention according to claim 6, the remaining means moves the protective tube in and out of the gap portion sandwiched between the holder and the sample tube by the sliding means.
The NMR apparatus according to the invention of claim 7 is the NMR apparatus according to claim 6, wherein the slide means has a cross section perpendicular to the central axis of the holder, the protective tube, and the sample tube. It arrange | positions in the shape which makes a concentric circle, It is characterized by the above-mentioned.

In the invention described in claim 7, the slide means arranges the holder, the protective tube, and the sample tube so that the cross-sections are concentric.
An NMR apparatus according to an eighth aspect of the present invention is the NMR apparatus according to the sixth or seventh aspect, wherein the protective tube comprises a plurality of partial protective tubes having different inner diameters in a direction perpendicular to the central axis. It is characterized by that.

In the invention according to claim 8, the protective tube is composed of a plurality of partial protective tubes having different inner diameters.
The NMR apparatus according to the invention described in claim 9 is the NMR apparatus according to claim 8, wherein the slide means is provided in the gap portion sandwiched between the partial protective tube and the sample tube by the partial protective tube. Also, the partial protective tube having a small inner diameter is taken in and out.

In the invention according to the ninth aspect, the sliding means inserts and removes the partial protective tube having a small inner diameter into and out of the gap portion sandwiched between the partial protective tube and the sample tube.
An NMR apparatus according to the invention described in claim 10 is the NMR apparatus according to claim 8 or 9, wherein the partial protective tube has an outer diameter in a direction orthogonal to the central axis of the arrangement space. The size is larger than the inner diameter in the direction perpendicular to the central axis.

In the invention according to the tenth aspect, the partial protection tube is sized so as not to enter the installation space.
The NMR apparatus according to claim 11 is the NMR apparatus according to any one of claims 1 to 10, wherein the arrangement space is formed in a mortar shape at an entrance of the sample tube vertically above. It is characterized by comprising an opening that extends into the area.

In the invention according to claim 11, the arrangement space expands the opening corresponding to the entrance of the sample tube in a mortar shape.
The NMR apparatus according to the invention described in claim 12 is characterized in that, in the NMR apparatus according to claim 11, the protective tube includes a tip portion having a shape that fits the opening.

In the invention according to this twelfth aspect, the protective tube has the tip end adapted to the opening.
An NMR apparatus according to the invention described in claim 13 is the NMR apparatus according to any one of claims 1 to 12, wherein the sample tube, the protective tube, the holder, and the holder holding means are It is characterized by using a magnetic material.

  In the invention described in claim 13, the sample tube, the protective tube, the holder and the holder holding means do not affect the magnetic field strength in the cylindrical tube.

  As described above, according to the first aspect of the present invention, the subject portion is retained when the sample tube includes the sample tube and is inserted into the installation space by the cylindrical protective tube. Since the protective tube is left in the cylindrical space vertically above the installation space by the means, the protective tube prevents the sample tube from being damaged before being inserted into the installation space. The sample tube arranged in (1) can perform a normal inspection without causing deterioration in resolution and sensitivity of the NMR inspection by the protective tube, and thus the NMR inspection can be made safe and easy for the operator.

  According to the second aspect of the present invention, since the residual means repeatedly encloses the sample tube with the protective tube, the sample tube is provided even when the sample tube is drawn out from the installation space or the cylindrical space including the installation space. Can be prevented from being damaged.

  According to the third aspect of the present invention, the subject portion partially encloses one end portion of the rod-shaped sample tube by the holder and holds the sample tube, so that the sample tube is damaged. It can be easily carried without it.

  According to the fourth aspect of the present invention, since the subject portion is brought into a state close to the housing portion by the holder holding means, the subject portion is gently adjusted by adjusting the air pressure in the housing portion. It can be conveyed to the upper part of the arrangement space.

  According to the invention described in claim 5, since the protective tube encloses one end of the sample tube, the sample tube can be safely transferred from the one end to the cylindrical space and further to the installation space. Insertion can be performed.

  According to the sixth aspect of the present invention, since the residual means is configured to insert and remove the protective tube into and from the gap portion sandwiched between the holder and the sample tube by the slide means, the protective tube portion is contracted and stored in the holder. can do.

  According to the seventh aspect of the present invention, the slide means is arranged such that the holder, the protective tube, and the sample tube are arranged so that the cross section is concentric. It can be easily taken in and out.

According to the eighth aspect of the present invention, since the protective tube is composed of a plurality of partial protective tubes having different inner diameters, a wide area of the sample tube can be included.
According to the ninth aspect of the present invention, since the sliding means is designed so that the partial protective tube having a small inner diameter is taken in and out of the gap portion sandwiched between the partial protective tube and the sample tube, a large number of partial protective tubes are provided in the holder. Can be stored.

  According to the invention described in claim 10, since the partial protection tube is sized so as not to enter the installation space, only the sample tube is inserted into the installation space, and the partial protection tube is provided in the installation space. Can be left in the cylindrical space vertically above.

  According to the eleventh aspect of the present invention, since the opening space corresponding to the inlet of the sample tube is expanded in a mortar shape, the arrangement space is also provided when the sample tube deviates from the position of the central axis. Can lead to space.

According to the twelfth aspect of the present invention, since the protective tube has the tip end adapted to the opening, the position of the sample tube in the arrangement space can be stabilized.
According to the thirteenth aspect of the invention, the sample tube, the protective tube, the holder, and the holder holding means do not affect the magnetic field strength in the cylindrical tube, so that an NMR signal with good resolution and sensitivity is detected. be able to.

The best mode for carrying out an NMR apparatus according to the present invention will be described below with reference to the accompanying drawings. Note that the present invention is not limited thereby.
First, the whole structure of the NMR apparatus 1 concerning this Embodiment is demonstrated. FIG. 2 is a cross-sectional view showing the overall configuration of the NMR apparatus 1. The NMR apparatus 1 includes a static magnetic field generation unit 2, a housing unit 3, an RF signal transmission / reception unit 4, a subject unit 5, a compressor 6, and a column 7. The static magnetic field generator 2 is a magnet that generates a static magnetic field B0 along the central axis of the static magnetic field coil that faces in the vertical direction. For this magnet, a superconducting magnet having high static magnetic field stability is used. Note that the xyz coordinates shown in FIG. 2 and all the coordinate axes shown in the following drawings are the same coordinate axes.

  Here, there is a cylindrical space 8 that is in a cylindrical state along the central axis of the magnet, and a static magnetic field B 0 is formed inside the cylindrical space 8. Inside the cylindrical space 8, there are a housing part 3, a subject part 5 and an RF signal transmitting / receiving part 4. As described above, in the case of a magnet having a static magnetic field strength of 14T, the diameter in the direction orthogonal to the central axis of the cylindrical space 8 is approximately 5 to 6 cm, and the length in the vertical direction is approximately 1 to 2 m. It becomes.

  The subject section 5 has a rod-shaped sample tube 53 in which a test sample is enclosed. In the arrangement shown in FIG. 2, the sample tube 53 is located on the central axis. As described above, the diameter of the sample tube 53 is about 3 to 5 mm, and the subject portion 5 will be described in detail later.

  The RF signal transmission / reception unit 4 is inserted from the vertically lower side of the cylindrical space 8 and is fixedly disposed between the cylindrical space 8 and a substantially central portion in the vertical direction. The RF signal transmitting / receiving unit 4 includes a coil that transmits an RF signal to the subject unit 5 and receives an RF signal from the subject unit 5. The RF signal transmitting / receiving unit 4 has a cylindrical arrangement space 10 in which the sample tube 53 is arranged along the central axis of the cylindrical space 8, and the coil is close to surround the arrangement space 10. Arranged. The diameter in the direction orthogonal to the central axis of the arrangement space 10 is arranged as close as possible to the RF signal transmitting / receiving unit with respect to the rod-shaped sample tube 53 from the viewpoint of improving the sensitivity of the NMR signal. It is about 10 mm.

  The coil is connected to an RF waveform generator and an RF waveform receiver (not shown), and the RF waveform generator and the RF waveform receiver are controlled by a control unit (not shown), and the test sample contained in the sample tube is used as a nucleus. An excited state of magnetic resonance is set, and an RF signal of the excited test sample is received.

  Further, the lower end portion of the arrangement space 10 is connected to the compressor 6 through a valve 9 by a pipe. Here, the operator adjusts the amount of air flowing from the compressor 6 into the installation space 10 and further into the cylindrical space 8 located above the installation space 10 by opening and closing the valve 9.

  The housing part 3 is a cylindrical structure that is internally arranged so as to form a concentric circle with the cylindrical space 8, and is provided on the wall surface of the cylindrical space 8 from the upper part of the cylindrical space 8 to the position where the RF signal transmitting / receiving part 4 is fixedly arranged. The structure is in close contact. Note that the inner surface of the housing portion 3 has a structure close to the side surface of the subject portion 5. Thus, when the subject portion 5 is inserted from vertically above the housing portion 3 when the valve 9 is opened and air is flowing into the cylindrical space 8, the inside of the housing portion 3 is connected to the subject portion 5 and the RF. The space sandwiched between the signal transmitting / receiving unit 4 becomes a positive pressure compared to the outside, and the subject unit 5 is in a floating state in the housing unit 3. Then, the operator adjusts the amount of air flowing into the housing portion 3 by the valve 9, gradually lowers the subject portion 5 from the entrance portion of the housing portion 3 to the RF signal transmitting / receiving portion 4, and samples the subject portion 5. The tube 53 is arranged in the arrangement space of the RF signal transmitting / receiving unit 4.

  There is a slight play space between the inner surface of the housing portion 3 and the side surface of the subject portion 5 for releasing air flowing in from the vertically lower side of the cylindrical space 8. This play space allows the subject portion 5 inserted from above the housing portion 3 to be lowered smoothly only by adjusting the air pressure, and the position of the sample tube 53 of the subject portion 5 is slightly shifted from the central axis. And

  FIG. 3 is an explanatory view showing this state. The subject portion 5 is slightly inclined with respect to the central axis due to the play space between the side surface of the subject portion 5 and the wall surface of the housing portion 3. Further, the sample tube 53 attached to the subject unit 5 also has the same inclination. This inclination changes every time the subject part 5 is inserted into the housing part 3, and in some cases, as shown in FIG. 3, the vertical lower end of the sample tube 53 has an arrangement space 10 having a diameter of about 10 mm. Lands at a position deviated from the entrance of the tube and causes a shock to the sample tube 53. The subject unit 5 and the RF signal transmission / reception unit 4 are shown only schematically, and details will be described later.

  FIG. 4 is a cross-sectional view showing the detailed structure of the xy cross section of the subject portion 5. The subject unit 5 includes a sample tube 53, a spinner rotor 54 as a holder holding means, a holder 50, and partial protection tubes 58 and 59 forming a protection tube. The sample tube 53 is made of a rod-shaped glass tube, and a liquid test sample is sealed inside. The glass tube has a diameter of about several mm.

  The holder 50 has a fitting part 52 and a screw 51. The fitting portion 52 is for holding the fragile sample tube 53 safely and reliably, forms a cylindrical structure, penetrates the sample tube 53 along the central axis of the structure, and the tube of the sample tube 53 Press and hold the walls evenly. The screw 51 attaches the fitting portion 52 to the holder 50 by screwing and presses the fitting portion 52 to ensure the holding of the sample tube 53.

  The spinner rotor 54 serves as a holder holding means, and has a rotation mechanism such as a bearing that rotates the holder 50 around the central axis by power using air pressure or the like. Further, the spinner rotor 54 has a diameter in a direction perpendicular to the central axis slightly below the inner diameter of the housing part 3, and there is a play space between the side surface of the spinner rotor 54 and the inner surface of the housing part 3.

  The holder 50 is a cylindrical hollow structure and covers a portion that is substantially half of one side of the rod-shaped sample tube 53 and is not inserted into the arrangement space 10. Here, the holder 50 inserts partial protection tubes 58 and 59, which will be described later, into a gap between the holder 50 and the sample tube 53 disposed on the central axis.

  The partial protection tubes 58 and 59 are cylindrical metal tubes formed of, for example, non-magnetic stainless steel. A sample tube 53 is disposed on the central axis of the tube, and the fitting portion 52 and the screw 51 of the holder 50 are provided. Mounted on the non-existent side. Here, the partial protection tubes 58 and 59 have sliding means as residual means, and this sliding means has an outer diameter in a direction perpendicular to the central axis of the partial protection tube 59 smaller than the inner diameter of the holder 50. The partial protective tube 59 and the holder 50 are arranged so that the cross section in the direction orthogonal to the central axis forms a concentric circle with the central axis as the center. Then, the partial protective tube 59 is slid and moved to the gap portion between the holder 50 and the sample tube 53 by an external force, for example, a force pushing vertically upward. The partial protective tube 59 that has moved to the gap portion contacts the screw 51 and stops moving.

  Further, the partial protection tube 58 disposed between the holder 50 and the sample tube 53 slides vertically downward and protrudes below the holder 50 by an external force, for example, its own weight. At this time, the vertical upper end portion of the partial protective tube 59 has a stopper 60 having a larger outer diameter than the intermediate portion, and is present at the end portion of the holder 50 on the side where the fitting portion 52 and the screw 51 do not exist. Engage with the small inner diameter and stop sliding downward vertically.

  The partial protection tube 58 is attached to the side of the partial protection tube 59 where the stopper 60 does not exist. Here, the partial protection tube 58 has slide means as residual means, and this slide means has an outer diameter in a direction orthogonal to the central axis smaller than an inner diameter of the partial protection pipe 59 and is orthogonal to the central axis. The partial protective tube 58 and the partial protective tube 59 are arranged so that the cross section in the direction to be formed is a concentric circle with the central axis as the center. Then, the partial protective tube 58 is slid and moved to the gap portion between the partial protective tube 59 and the sample tube 53 by an external force, for example, a force pushing vertically upward. The partial protective tube 58 that has moved to the gap is stopped by a stopper 63 having a small inner diameter adjacent to the stopper 60 of the partial protective tube 59.

  Further, the partial protection tube 58 disposed between the partial protection tube 59 and the sample tube 53 slides vertically downward and protrudes vertically below the partial protection tube 59 by an external force, for example, its own weight. At this time, the vertical upper end portion of the partial protective tube 58 has a stopper 61 having a larger outer diameter than that of the intermediate portion, and the inner diameter of the partial protective tube 59 present at the end portion on the side where the stopper 60 does not exist is small. Engage with the part and stop sliding vertically downward.

  A tip 62 is present vertically below the partial protection tube 59. The distal end portion 62 is shaped to match an opening of the arrangement space 10 described later. The sample tube 53 is attached to the holder 50 using the fitting portion 52 and the screw 51 so that the end portion is positioned vertically upward from the tip portion 62 by several mm with the partial protection tubes 58 and 59 extended. The

  FIG. 5 is a cross-sectional view showing details of a region where the housing part 3 and the RF signal transmitting / receiving part 4 in the cylindrical space 8 form a boundary. 5 shows a holder guide 42 attached to the RF signal transmitting / receiving unit 4 that is not shown in FIGS. The arrangement space 10 of the RF signal transmitting / receiving unit 4 has an opening 41 at the entrance vertically above where the sample tube 53 is inserted. In the opening 41, the diameter of the entrance expands in a mortar shape vertically upward of the central axis. The tip portion 62 is shaped to fit the opening 41, and when the sample tube 53 is inserted into the arrangement space 10, the tapered portion of the tip portion 62 is in close contact.

  Further, as shown in FIG. 5, a region including the opening 41 is separately provided as a support 43 that can be attached to and detached from the RF signal transmission / reception unit 4, and the material of the support 43 or the extent of the opening 41 is changed according to the sample tube 53. It is also possible to replace it with a material suitable for the sample tube 53 having a material that is difficult to damage or having a different tip 62 shape.

  The RF signal transmission / reception unit 4 includes a holder guide 42 above the opening 41. The holder guide 42 is a cylindrical structure, the cylindrical side surface is in close contact with the housing portion 3, and the inner diameter in the direction perpendicular to the central axis substantially matches the outer diameter of the holder 50. Thereby, the holder 50 of the subject part 5 inserted from vertically above the cylindrical space 8 is inserted into the holder guide 42, and the position of the holder 50 in the cylindrical space 8 is ensured. The vibration of the sample tube 53 disposed inside is prevented.

  Next, the operation until the subject part 5 is inserted from vertically above the cylindrical space 8 and the sample tube 53 is arranged in the arrangement space 10 will be described with reference to FIGS. First, the operator inserts the portion where the sample tube 53 of the subject unit 5 is covered with the partial protection tubes 58 and 59 into the cylindrical space 8 of the static magnetic field generating unit 2 from above. At this time, the valve 9 of the NMR apparatus 1 is opened, and air is sent from the compressor 6 to the cylindrical space 8. Since the air pressure inside the cylindrical space 8 is positive, the inserted subject portion 5 is brought into a semi-floating state in the housing portion 3 of the cylindrical space 8. The air pressure in the cylindrical space 8 is reduced by adjustment or the like, and the subject portion 5 is gradually lowered in the cylindrical space 8. In this insertion step, the sample tube 53 is vertically covered with the partial protection tubes 58 and 59, so that the sample tube 53 is prevented from being damaged due to an unintended collision with the housing portion 3 or the like.

  In FIG. 1A, the subject portion 5 inserted into the cylindrical space 8 gradually descends in the cylindrical space 8, and the distal end portion 62 of the partial protection tube 58 has landed on the opening 41 of the arrangement space 10. It is sectional drawing which shows a state. Here, it is preferable that the sample tube 53 is accurately positioned on the central axis of the cylindrical space 8, but for the reason described above, a slight deviation occurs from the central axis.

  FIG. 6 is an enlarged view showing the vicinity of the opening 41 in this state. The partial protective tube 58 that covers the sample tube 53 is not positioned on the central axis of the cylindrical space 8, and the tapered portion of the tip 62 is in contact with the mortar portion of the opening 41. At the time of landing, the vertical lower tip of the sample tube 53 is covered by the tip 62 of the partial protection tube 58, so that an impact is prevented from being applied to the sample tube 53.

  Here, since the opening 41 has a mortar shape and the tip 62 has a tapered shape, the partial protective tube 58 slides in the mortar-shaped opening 41 and moves in the horizontal direction when further descending. The opening 41 and the tip 62 are fitted, and the sample tube 53 is present on the central axis.

  FIG. 1B is a cross-sectional view showing a state in which the subject portion 5 is further lowered and the distal end portion 62 of the partial protection tube 58 is fitted to the opening 41. The subject part 5 shows a state in which the sample tube 53 is located on the central axis and at the same time a part of the partial protection tube 58 is slid into the partial protection tube 59 positioned vertically upward. Since a part of the partial protection tube 58 enters the inside of the partial protection tube 59, the sample tube 53 has a vertically lower end located at the front end 62 of the partial protection tube 58 and at the entrance of the arrangement space 10. To position.

  FIG. 1C is a cross-sectional view showing a state in which the subject portion 5 is further lowered and the sample tube 53 has been arranged in the arrangement space 10. The holder 50 of the subject unit 5 is housed in the holder guide 42, and the partial protective tube 59 enters the inside of the holder 50 at the same time that the partial protective tube 58 enters the inside of the partial protective tube 59. Since the partial protection tube 58 enters the inside of the partial protection tube 59 and the partial protection tube 59 enters the inside of the holder 50, the sample tube 53 protrudes vertically downward and is located at the position of the transmission / reception coil in the arrangement space 10. Reach.

  Further, after the inspection of the inspection sample contained in the sample tube 53 is completed, air is sent into the cylindrical space 8 by adjustment in the direction in which the valve 9 is opened, and the subject portion 5 is floated in the cylindrical space 8. Then, the process shown in FIGS. 1 (A) → (B) → (C) is performed in reverse, and the subject portion 5 is raised vertically above the housing portion 3 and is collected by the operator. In this step, the partial protective tube 59 built in the holder 50 and the partial protective tube 58 built in the partial protective tube 59 are sequentially projected from the holder 50 and the partial protective tube 59 by their own weight. When the sample tube 53 moves away from the installation space 10, as shown in FIG. 4, the partial protection tubes 59 and 58 are in a state of covering the sample tube 53, and the sample tube is not subjected to unintended impact in the subsequent process. 53 is prevented from being damaged.

  As described above, in this embodiment, the exposed one side portion of the sample tube 53 to which the holder 50 is attached is covered with the partial protection tubes 59 and 58, and the sample tube 53 is further disposed in the arrangement space 10. In this case, since the partial protection tubes 59 and 58 are built in the holder 50 and the partial protection tube 59 and only the sample tube 53 is disposed, when the subject portion 5 is taken in and out of the NMR apparatus 1. The sample tube 53 can be prevented from being damaged by an unintended impact such as a collision, and at the same time, the NMR inspection using the sample tube 53 can be performed without causing deterioration of sensitivity, resolution, and the like.

  Further, in the present embodiment, when the subject portion 5 is taken in and out of the arrangement space 10, air is introduced from below the cylindrical space 8 and the position of the subject portion 5 is controlled by air pressure. The subject portion 5 can be taken in and out using an operation rod on which the subject portion 5 is mounted.

  FIG. 7 is an explanatory diagram showing a state in which the operator arranges the subject portion 5 in the arrangement space 10 using the operation rod 80. The NMR apparatus 1 is shown in cross-sectional view. The operation rod 80 is a rod having a length approximately equal to the length of the cylindrical space 8 in the vertical direction, and the subject portion 5 is detachably attached to the end of the rod. Then, the operator inserts the subject portion 5 together with the operation rod 80 into the cylindrical space 8 from the upper part of the staircase arranged beside the NMR apparatus 1. At this time, since the sample tube 53 is covered with the partial protection tubes 59 and 58 as shown in FIG. 4, the sample tube 53 can be prevented from being damaged from an impact such as a collision due to an operation error. In the operation using the operation rod 80, the valve 9 is closed and the inflow of air into the cylindrical space 8 is stopped.

  In the present embodiment, the exposed portion of the sample tube 53 to which the holder 50 is attached is covered with the two partial protective tubes 59 and 58. However, one or three or more partial protective tubes are used. A multi-stage structure can be formed. Thereby, the length of the partial protection tube determined by the length of the holder 50, the depth from the opening 41 to the coil position, and the like can be optimized.

It is explanatory drawing which shows the process of arrange | positioning a sample tube in arrangement | positioning space. It is sectional drawing which shows the whole structure of an NMR apparatus. It is explanatory drawing explaining the shift | offset | difference from the central axis of a sample tube. It is sectional drawing which shows the detail of a subject part. It is sectional drawing which shows the detail of the opening part vicinity of RF signal transmission / reception part. It is an enlarged view of the vicinity of the opening when the partial protective tube has landed on the opening. It is explanatory drawing which shows a mode that a to-be-tested part is inserted in cylindrical space using an operation stick.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 NMR apparatus 2 Static magnetic field generating part 3 Housing part 4 RF signal transmission / reception part 5 Test object part 6 Compressor 7 Support column 8 Cylindrical space 9 Valve 10 Installation space 41 Opening part 42 Holder guide 43 Support part 50 Holder 51 Screw 52 Fitting part 60 , 61, 63 Stopper 53 Sample tube 54 Spinner rotor 58, 59 Partial protection tube 62 Tip 80 Operation rod

Claims (13)

A static magnetic field generating unit having a cylindrical space in a cylindrical state in a vertical direction in which a uniform static magnetic field is formed;
A subject part having a rod-shaped sample tube containing a test sample, which is inserted from vertically above the cylindrical space;
An RF signal transmitter / receiver having a cylindrical arrangement space that is fixedly arranged at a substantially intermediate position in the vertical direction of the cylindrical space and in which the sample tube is arranged along a central axis in the vertical direction of the cylindrical space;
An NMR apparatus comprising:
The subject portion has a cylindrical protective tube that encloses the sample tube, and when the sample tube is inserted into the installation space, the protective tube is positioned vertically above the installation space. An NMR apparatus comprising: a remaining means that remains in space.   2. The NMR apparatus according to claim 1, wherein the residual unit includes the sample tube with the protective tube when the sample tube is pulled out from the arrangement space.   The said subject part is provided with the holder which partially encloses the one side edge part of the said rod-shaped said sample tube, and compresses and hold | maintains the tube wall of the said sample tube equally. The described NMR apparatus.   When the subject portion has a hollow cylindrical housing portion sharing a central axis in the cylindrical space, the outer diameter of the housing portion approximates without exceeding the inner diameter of the housing portion in a direction perpendicular to the central axis. The NMR apparatus according to claim 3, further comprising cylindrical holder holding means for holding and rotating the holder around the central axis.   5. The NMR apparatus according to claim 3, wherein the protective tube includes one end portion that is not included in the holder of the rod-shaped sample tube.   6. The NMR apparatus according to claim 5, wherein the remaining means includes slide means for taking the protective tube in and out of a gap portion between the holder and the sample tube.   7. The NMR apparatus according to claim 6, wherein the slide means arranges the holder, the protective tube, and the sample tube in a shape in which a cross section perpendicular to the central axis forms a concentric circle.   The NMR apparatus according to claim 6 or 7, wherein the protective tube includes a plurality of partial protective tubes having different inner diameters in a direction orthogonal to the central axis.   9. The NMR apparatus according to claim 8, wherein the sliding means inserts and removes a partial protective tube having a smaller inner diameter than the partial protective tube into a gap portion sandwiched between the partial protective tube and the sample tube.   10. The partial protection tube according to claim 8 or 9, wherein an outer diameter in a direction orthogonal to the central axis is larger than an inner diameter in a direction orthogonal to the central axis of the arrangement space. The described NMR apparatus.   11. The NMR apparatus according to claim 1, wherein the arrangement space includes an opening that extends in a mortar shape at an entrance of the sample tube vertically above.   The NMR apparatus according to claim 11, wherein the protective tube includes a tip portion having a shape that fits the opening.   The NMR apparatus according to any one of claims 1 to 12, wherein the sample tube, the protective tube, the holder, and the holder holding means are configured using a nonmagnetic material.

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