Sample tube transfer device

Abstract

To allow a sample tube to be reliably transferred while protecting the sample tube.SOLUTION: A loading unit 34 injects a loading gas to a first position P1 on a passage from a cone-shaped gas G1. This creates a first gas flow for loading a sample tube. An injection unit 36 injects an ejecting gas to a second position P2 on the passage from a cone-shaped gas G2. This creates a second gas flow for ejecting the sample tube.SELECTED DRAWING: Figure 2

Description

[Technical field]

[0001] The present invention relates to a sample tube transfer device, and more particularly to a technique for transferring a sample tube between a sample tube holder and a sample tube rotator in an NMR measurement system. [Background technology]

[0002] An NMR (Nuclear Magnetic Resonance) measurement system is a system that measures NMR generated in a sample in order to analyze the sample. The NMR measurement system includes a static magnetic field generator, an NMR measurement probe, a spectrometer, and the like.

[0003] When the subject of NMR measurement is a solid sample, the MAS (Magic angle spinning) method is generally used. In the MAS method, NMR measurement is performed on a solid sample in a sample tube while rotating the sample tube with the sample tube tilted at a specified angle (approximately 54.7 degrees) with respect to the static magnetic field. The solid sample is, for example, a powder. When implementing the MAS method, a sample tube rotator (hereinafter simply referred to as the "rotator") is provided in the NMR measurement probe. In the rotator, the rotating sample tube is the rotor, and the rotator itself is the stator. The rotator is also called the MAS module.

[0004] If a user is required to remove or attach an NMR measurement probe when setting a sample tube on a rotator or removing the sample tube from the rotator, this places a heavy burden on the user.

[0005] In order to facilitate the replacement of sample tubes, a sample tube transfer device has been proposed (see Patent Documents 1 to 3). The sample tube transfer device is a device that automatically transfers sample tubes between a sample tube container (hereinafter simply referred to as "container") and a rotator. The container is, for example, a sample tube carrier.

[0006] In the sample tube transfer devices disclosed in Patent Documents 1 and 2, sample tubes are transferred between a container provided above a static magnetic field generator and a rotator inside the static magnetic field generator. A unit for ejecting the sample tube is provided in the middle of the passage between the container and the rotator. The unit has an injection hole that injects gas into the passage from a direction inclined to the central axis of the passage. The injection of gas generates a gas flow from the rotator to the container. The sample tube is ejected by this gas flow. Patent Documents 1 and 2 do not disclose a specific configuration that functions when loading a sample tube.

[0007] In the sample tube transport device disclosed in Patent Document 3, sample tubes are transported between a container provided below a static magnetic field generator and a rotator inside the static magnetic field generator. The sample tubes are transported by a gas flow, but Patent Document 3 does not disclose a specific configuration for generating the gas flow. [Prior art documents] [Patent documents]

[0008] [Patent Document 1] Patent No. 6016373 specification [Patent Document 2] Patent No. 6876471 Specification [Patent Document 3] Patent No. 6445484 specification Summary of the Invention [Problem to be solved by the invention]

[0009] In a sample tube transport device in an NMR measurement system, it is desirable to apply an appropriate transport force to the sample tube throughout the entire passage through which the sample tube moves. Specifically, it is desirable to simultaneously avoid damage and wear to the sample tube and to prevent the sample tube from stopping midway through the passage. Recently, the diameter of the sample tube has become smaller and smaller, and the sample tube is more likely to stop midway through the passage due to static electricity or dirt on the sample tube surface. If the sample tube stops midway during loading, NMR measurement of the sample becomes impossible.

[0010] An object of the present invention is to transport a sample tube reliably while protecting the sample tube. Another object of the present invention is to transport a sample tube in a manner that prevents the sample tube from becoming unstable. [Means for solving the problem]

[0011] The sample tube transfer device of the present invention is characterized by including a load unit that injects a load gas into a first position in a passage between a sample tube holder and a sample tube rotator before NMR measurement of a sample in a sample tube, thereby generating a first gas flow that transfers the sample tube from the sample tube holder to the sample tube rotator, and an eject unit that injects an eject gas into a second position in the passage after NMR measurement of the sample, thereby generating a second gas flow that transfers the sample tube from the sample tube rotator to the sample tube holder. Effect of the Invention

[0012] According to the present invention, the sample tube can be securely transported while being protected, or the sample tube can be transported without becoming unstable in its position. [Brief description of the drawings]

[0013] [Figure 1] FIG. 1 is a diagram showing an NMR measurement system including a sample tube transport device according to an embodiment. [Diagram 2] FIG. 1 is a cross-sectional view showing an example of a structure. [Diagram 3]FIG. 13 is a schematic diagram showing the operation when loading a sample tube. [Figure 4] FIG. 13 is a schematic diagram showing the operation when ejecting a sample tube. [Diagram 5] FIG. [Figure 6] FIG. 2 is a cross-sectional view showing a carrier (container). [Figure 7] 5A to 5C are cross-sectional views showing the operation of the carrier. [Figure 8] 4 is a timing chart showing gas supply control. [Figure 9] 10 is a flowchart showing an example of the operation of the sample tube transport device. [Figure 10] 10 is a flowchart showing another example of the operation of the sample tube transport device. [Figure 11] FIG. 11 is a cross-sectional view showing another example of a structure. [Figure 12] 12A to 12C are diagrams illustrating the operation of the structure shown in FIG. [Figure 13] FIG. 13 shows a sample tube transport device according to another embodiment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0014] Hereinafter, an embodiment will be described with reference to the drawings.

[0015] (1) Overview of the embodiment The sample tube transfer device according to the embodiment includes a load unit and an eject unit. The load unit injects a load gas to a first position in a passage between the sample tube holder and the sample tube rotator before NMR measurement of a sample in the sample tube, and generates a first gas flow that transfers the sample tube from the sample tube holder to the sample tube rotator. The eject unit injects an eject gas to a second position in the passage after NMR measurement of the sample, and generates a second gas flow that transfers the sample tube from the sample tube rotator to the sample tube holder.

[0016] According to the above configuration, since both the load unit and the eject unit are provided, loading and ejecting of the sample tube can be performed reliably. More specifically, gas (load gas, eject gas) is fed into the passage (first position, second position), which generates gas flows (first gas flow, second gas flow), so that an appropriate transport force can be applied to the sample tube throughout the entire passage. Therefore, the sample tube can be transported reliably while being protected.

[0017] In the above configuration, the sample tube container is a member provided at one end of the passage. The sample tube container is, for example, a carrier, a holder, a magazine rack, an insertion port, etc. The sample tube rotator is a module provided at the other end of the passage, and specifically, causes the sample tube to perform a rotational motion according to the MAS method. The sample tube may be inserted from above the static magnetic field generator, or from below the static magnetic field generator. A part of the passage may form a curved portion, or a direction changer may be provided midway along the passage.

[0018] In an embodiment, the load unit includes a first gap having a first outlet facing the sample tube rotator side and for injecting a load gas into the passage, and the eject unit includes a second gap having a second outlet facing the sample tube container side and for injecting an eject gas into the passage.

[0019] When the load gas is sent from the first opening to the first position during sample tube loading, the gas present on the upstream side of the first position is drawn downstream, and at the same time, the gas present at the first position is pushed downstream. That is, a first upstream gas flow is generated in a section (first upstream section) upstream of the first position, and a first downstream gas flow is generated in a section (first downstream section) downstream of the first position. In the embodiment, a negative pressure is generated in the first upstream section, and the atmosphere present in the outside world flows into the first upstream section through one end of the passage. In the embodiment, a positive pressure is generated in the first downstream section, and the gas is released to the outside world through the other end of the passage. Thus, it is possible to prevent the transport force by the first upstream gas flow from becoming excessive, and to prevent the transport force by the first downstream gas flow from becoming excessively small. The first upstream gas flow and the first downstream gas flow constitute a first gas flow. The first gas flow exerts an appropriate transport force throughout its entirety.

[0020] On the other hand, when the ejection gas is sent from the second opening to the second position during sample tube ejection, the gas present on the upstream side of the second position is drawn downstream, and the gas present at the second position is pushed downstream. That is, a second upstream gas flow is generated in a section (second upstream section) upstream of the second position, and a second downstream gas flow is generated in a section (second downstream section) downstream of the second position. In the embodiment, a negative pressure is generated in the second upstream section, and the atmosphere present in the outside world flows into the second upstream section through the other end of the passage, etc. In the embodiment, a positive pressure is generated in the second downstream section, and the gas is released to the outside world through the one end of the passage, etc. Thus, it is possible to prevent the transport force by the second upstream gas flow from becoming excessive, and to prevent the transport force by the second downstream gas flow from becoming excessively small. The second upstream gas flow and the second downstream gas flow constitute the second gas flow. The second gas flow exerts an appropriate transport force throughout its entirety.

[0021] In the embodiment, the first gap and the second gap are each a cone-shaped gap. The first outlet and the second outlet are each annular outlet. With this configuration, when loading the sample tube, a load gas is injected from the periphery of the sample tube toward the side of the sample tube when the sample tube passes through the first position, so that the attitude of the sample tube can be prevented from becoming unstable. Also, when ejecting the sample tube, an ejection gas is injected from the periphery of the sample tube toward the side of the sample tube when the sample tube passes through the second position, so that the attitude of the sample tube can be prevented from becoming unstable.

[0022] In the embodiment, of the first and second positions, the one closer to the sample tube rotator is the first position, and the one closer to the sample tube container is the second position. With this configuration, the second position can be set in the first upstream section (i.e., in the negative pressure section), and the first position can be set in the second upstream section (i.e., in the negative pressure section). Therefore, when loading a sample tube, it is possible to prevent the attitude of the sample tube from becoming unstable when the sample tube passes through the second position. Also, when ejecting a sample tube, it is possible to prevent the attitude of the sample tube from becoming unstable when the sample tube passes through the first position. Negative pressure and positive pressure are generally defined with reference to atmospheric pressure or external pressure.

[0023] In the embodiment, the load unit and the eject unit are coupled to each other. This configuration makes it easy to align the central axes of the two units (specifically, the central axes of the two internal passages) and to bring the first position and the second position closer to each other.

[0024] In an embodiment, the sample tube rotator has a thrust gas bearing that blows gas against one end face of the sample tube housed therein. The load unit generates a first gas flow in a rotation state in which the sample tube rotates in the sample tube rotator. In the rotation state, gas from the first gas flow is blown against the other end face of the sample tube. With this configuration, the position of the sample tube in the rotation state of the sample tube can be stabilized in the direction of the central axis of rotation.

[0025] In the embodiment, the ejection unit generates the second gas flow even after the sample tube is returned into the sample tube container. This configuration can prevent foreign matter from entering the passage. In particular, it is desirable to continuously generate the second gas flow after the sample container is floated.

[0026] The sample tube transfer device according to the embodiment includes an upper end member that surrounds at least an upper end portion of a passage. The sample tube container has a container chamber that contains a sample tube and an opening / closing mechanism. The opening / closing mechanism is provided at the bottom of the container chamber and changes from a closed state to an open state when the sample tube container is connected to the upper end member and changes from the open state to a closed state when the sample tube container is detached from the upper end member. The opening / closing mechanism includes a plurality of movable elements that support the sample tube in the container chamber in the closed state.

[0027] According to the above-mentioned configuration, since the opening and closing mechanism operates in accordance with the attachment and detachment of the sample tube holder to and from the upper end member, there is no need to externally control the opening and closing mechanism. Also, it becomes possible to stably support the sample tubes by a plurality of movable elements.

[0028] The sample tube transport device according to the embodiment includes a hollow guide member provided in the bore of the static magnetic field generator. The sample tube holder performs a dropping motion in the guide member, whereby the sample tube holder is connected to the upper end member. The sample tube transport device according to the embodiment includes a lift unit that generates an ascending gas flow in the guide member to separate the sample tube holder from the guide member and to float the sample tube holder.

[0029] (2) Details of the embodiment An NMR measurement system 10 including a sample tube transfer device according to an embodiment is shown in Fig. 1. The NMR measurement system is a system for analyzing a sample, and more specifically, a system for measuring NMR occurring in a solid sample.

[0030] The NMR measurement system 10 includes a static magnetic field generator 12, an NMR measurement probe 14, a sample tube transport device 18, a spectrometer 63, and the like. In FIG. 1, the specific configuration of the spectrometer 63 is omitted. The NMR measurement system 10 further includes a flow rate regulator group 48 and a main control unit 60. The flow rate regulator group 48 and the main control unit 60 may be understood as parts of the sample tube transport device 18. In FIG. 1, each element is represented diagrammatically or exaggeratedly. In FIG. 1, a plurality of pipes provided inside the NMR measurement probe 14 are omitted.

[0031] The static magnetic field generator 12 has a superconducting magnet and generates a static magnetic field. The direction of the static magnetic field is the vertical direction in Fig. 1. The static magnetic field generator 12 has a bore 12A as a through hole.

[0032] The NMR measurement probe 14 is composed of a main body 20 and a base 22. The main body 20 is a part that is inserted into the bore 12A and has a cylindrical shape. The base 22 is a part that is disposed outside (below) the bore 12A. A rotator 24 is disposed inside the upper end of the main body 20 together with a detection coil (not shown). Also, a structure 30 including a load unit 34 and an eject unit 36, which will be described in detail later, is provided inside the upper end.

[0033] The base 22 and a spectrometer 63 are electrically connected via a signal line 62. The spectrometer includes a transmitter, a receiver, an NMR spectrum generator, etc. A hollow guide member 16 is disposed in the bore 12A. Specifically, the guide member 16 is disposed on the upper side of the main body 20 of the NMR measurement probe 14.

[0034] The sample tube transfer device 18 is a device that transfers sample tubes containing samples. Specifically, when loading a sample tube, it transfers the sample tube from the carrier 26 to the rotator 24, and when ejecting the sample tube, it transfers the sample tube from the rotator 24 to the carrier 26. The carrier 26 is a type of container. Sample tubes stored in a holder, magazine rack, etc. may be loaded. The rotator 24 is an MAS module that rotates the sample tube. A passage for transferring the sample tube is provided between the carrier 26 and the rotator 24.

[0035] The sample tube transfer device 18 has an axial member 28, a structure 30, a curved tube 32, etc. The carrier 26 and the rotator 24 may be considered to be parts of the sample tube transfer device 18. A hollow member is disposed inside the axial member 28, and the interior of the hollow member is part of the passage. A through hole formed in the structure 30 is also part of the passage. The interior of the curved tube 32 is also part of the passage. The upper end of the axial member 28 is the part that surrounds the upper end of the passage.

[0036] The carrier 26 has a storage chamber for storing sample tubes. The sample tubes before NMR measurement and the sample tubes after NMR measurement are stored in the storage chamber. The rotator 24 has a storage space for storing sample tubes. A rotational driving force is applied to the sample tubes stored in the storage space. One end (upper end) of the above passage is connected to the storage chamber in the carrier 26, and the other end (lower end) of the above passage is connected to the storage space in the rotator 24.

[0037] The structure 30 has a load unit 34 and an eject unit 36. The load unit 34 has an injection port facing the rotator 24, and injects load gas obliquely into the passage when loading a sample tube. This generates a first gas flow in the passage. The first gas flow is from top to bottom in FIG. 1. The first gas flow transfers the sample tube from the carrier 26 to the rotator 24.

[0038] The eject unit 36 ​​has an ejection port facing the carrier 26, and ejects the ejection gas from an oblique direction to the passage when ejecting the sample tube. This generates a second gas flow in the passage. The second gas flow is from bottom to top in FIG. 1. The second gas flow transfers the sample tube from the rotator 24 to the carrier 26.

[0039] Prior to NMR measurement, the carrier 26 containing the sample tube is dropped into the guide member 16. This falling motion connects the carrier 26 to the shaft member 28. The first gas flow then sends the sample tube out of the interior of the carrier 26 into the passage. After NMR measurement, the second gas flow transfers the sample tube from the rotator 24 into the interior of the carrier 26. The lift gas then applies a levitation force to the carrier 26, causing it to move upward (float). A stopper (not shown) restricts the carrier 26 from moving any further upward. The carrier 26 has a storage chamber and an opening / closing mechanism, as described below.

[0040] Line 38 is for supplying load gas, line 40 is for supplying ejection gas, line 42 is for supplying lift gas, line 44 is for supplying bearing gas, and line 46 is for supplying drive gas.

[0041] In the illustrated configuration example, the flow regulator group 48 is composed of five flow regulators 50, 52, 54, 56, and 58. The flow regulator 50 is a controller that adjusts the flow rate of the load gas. The flow regulator 52 is a controller that adjusts the flow rate of the eject gas. The flow regulator 54 is a controller that adjusts the flow rate of the lift gas. The flow regulator 56 is a controller that adjusts the flow rate of the bearing gas. The flow regulator 58 is a controller that adjusts the flow rate of the drive gas.

[0042] The load gas and eject gas may be dry air (e.g., with a dew point lower than 0 degrees Celsius), an inert gas (e.g., nitrogen gas, argon gas), a mixture of these, or the like. The flow rate of the load gas and eject gas is, for example, 1 L / min or more. The pressure of these gases is, for example, 5 kPa or more. Gases other than the load gas and eject gas may also be composed of dry air, an inert gas, etc.

[0043] The main control unit 60 controls the operation of each element constituting the NMR measurement system. The main control unit 60 controls the operation of the flow rate regulator group 48. The gas control performed by the main control unit 60 will be described later.

[0044] In the configuration shown in FIG. 1, the upper end of the shaft member 28 may be raised above the static magnetic field generator 12, and a sample tube holder, a magazine rack having a plurality of sample tubes, or the like may be connected to the upper end.

[0045] 2 shows a cross section of the structure 30. The structure 30 has a load unit 34 and an eject unit 36. P1 indicates a first position where the injection of the load gas occurs, and P2 indicates a second position where the injection of the eject gas occurs.

[0046] More specifically, the structure 30 has a main body 65, an upper member 66, an intermediate member 68, and a lower member 70. The main body 65 has a cylindrical shape and has a through hole 64 extending in the vertical direction. The upper member 66, the intermediate member 68, and the lower member 70 are arranged in the through hole 64.

[0047] The main body 65 has a flow passage 76 through which a load gas flows, a flow passage 78 through which an eject gas flows, and a flow passage 80 through which a lift gas flows. A load gas 86 is sent to the flow passage 76 through a port 82. An eject gas is sent to the flow passage 78 through a port 84. A lift gas 90 is sent to the flow passage 80 through a path not shown. The lift gas is sent upward from the flow passage 80. The flow passage 80 and the piping etc. connected thereto constitute a lift unit that generates an ascending gas flow. Note that the illustration of multiple piping etc. is omitted in FIG. 2.

[0048] The intermediate member 68 has a downward nozzle 94 and an upward nozzle 96. The intermediate member 68 has a through hole 98. The lower member 70 has a cone-shaped (conical, funnel-shaped, or umbrella-shaped) inclined surface 100 surrounding the nozzle 94. A cone-shaped gap G1 is generated between the inclined surface 100 and the outer surface (tapered surface) 95 of the nozzle 94. The gap G1 has an annular outlet (injection port) a1 facing the rotor side. The load gas sent from a storage chamber 102 connected to the flow path 76 is injected through the gap G1 to a first position P1 (specifically, a junction space 104). This injection generates a first gas flow in the passage.

[0049] Specifically, by ejecting the load gas to the first position P1, gas existing upstream of the first position P1 is drawn into the first position P1, and at the same time, gas existing at the first position P1 is pushed downstream of the first position P1. As a result, a first upstream gas flow is generated in the first upstream section upstream of the first position P1, and a first downstream gas flow is generated in the first downstream section downstream of the first position P1. In the embodiment, negative pressure is generated in the first upstream section, and the atmosphere existing in the outside world enters the passage through one end of the passage, etc. Positive pressure is generated in the first downstream section, and gas is released to the outside world from the other end of the passage, etc. The first upstream gas flow and the first downstream gas flow constitute a first gas flow.

[0050] The through hole 106 formed in the lower member 70 communicates with the internal space of the straight pipe 74. The straight pipe 74 is connected to the curved pipe 32. The through hole 98, the merging space 104 and the through hole 106 are part of a passage.

[0051] The upper member 66 has a cone-shaped inclined surface 108 surrounding the nozzle 96. A cone-shaped gap G2 is formed between the inclined surface 108 and the outer surface (tapered surface) 97 of the nozzle 96. The gap G2 has an annular outlet (ejection port) a2 facing the carrier side. Eject gas sent from a storage chamber 110 connected to the flow path 78 is ejected through the gap G2 to a second position P2 (specifically, a junction space 112). This ejection generates a second gas flow.

[0052] Specifically, by ejecting the ejection gas to the second position P2, gas existing upstream of the second position P2 is drawn into the second position P2, and at the same time, gas existing at the second position P2 is pushed downstream of the second position P2. As a result, a second upstream gas flow is generated in the second upstream section upstream of the second position P2, and a second downstream gas flow is generated in the second downstream section downstream of the second position P2. In the embodiment, negative pressure is generated in the second upstream section, and the atmosphere existing in the outside world enters the passage through one end of the passage, etc. Positive pressure is generated in the second downstream section, and gas is released to the outside world from the other end of the passage, etc. The second upstream gas flow and the second downstream gas flow constitute a second gas flow.

[0053] A through hole 114 formed in the upper member 66 communicates with the merging space 112. The through hole 114 communicates with the internal space of the straight pipe 72. The merging space 112 and the through hole 114 are also part of the passage.

[0054] 3 shows the operation when loading a sample tube. In the load unit 34, the load gas 118 is injected from the cone-shaped gap G1 toward the first position P1. This injection generates a first upstream gas flow 120 that applies a first transport force to the sample tube 124 in a first upstream section 126 upstream of the first position P1, and simultaneously generates a first downstream gas flow 122 that applies a second transport force to the sample tube in a first downstream section 128 downstream of the first position P1. A negative pressure is generated in the first upstream section 126, and a positive pressure is generated in the first downstream section 128. This makes it possible to prevent the first transport force from becoming excessively large, and to prevent the second transport force from becoming excessively small.

[0055] When the sample tube passes through the load unit 34, the load gas is sprayed evenly against the side of the sample tube, so the position of the sample tube does not become unstable. When loading the sample tube, the eject unit 36 ​​does not operate, but even if a small amount of gas is allowed to flow through the gap G2, only a gas flow 123 enters the passage, and the position of the sample tube passing through the eject unit 36 ​​does not become unstable.

[0056] 4 shows the operation when ejecting a sample tube. In the eject unit 36, the eject gas 132 is injected from the cone-shaped gap G2 toward the second position P2. This injection generates a second upstream gas flow 134 that applies a third transport force to the sample tube 138 in the second upstream section 140 upstream of the second position P2, and at the same time, generates a second downstream gas flow 136 that applies a fourth transport force to the sample tube in the second downstream section 142 downstream of the second position P2. A negative pressure is generated in the second upstream section 140, and a positive pressure is generated in the second downstream section 142. Thus, in the embodiment, it is possible to prevent the third transport force from becoming excessively large, and to prevent the fourth transport force from becoming excessively small.

[0057] When the sample tube passes through the eject unit 36, the eject gas is sprayed evenly against the side of the sample tube, so the position of the sample tube does not become unstable. When the sample tube is ejected, the load unit 34 does not operate, but even if a small amount of gas is allowed to flow through the gap G1, only a gas flow 137 enters the passage, and the position of the sample tube passing through the load unit 34 does not become unstable.

[0058] In the configuration shown in Figures 2 to 4, the load unit 34 and the eject unit 36 ​​are connected together, that is, they are integrated. This makes it easy to align the central axes of the two units 34, 36. In addition, there are other advantages such as a reduced number of parts and easy assembly. However, the two units 34, 36 may be separate.

[0059] The rotator 24 is shown diagrammatically in Fig. 5. The rotator 24 is connected to the end of the curved tube 32. The rotator 24 has a storage space 144 that stores a sample tube 146. One end of the sample tube 146 is provided with a marker 147 for detecting rotation. The other end of the sample tube 146 is provided with a plurality of turbine blades 148. The inside of the sample tube 146 is a sample chamber that stores a sample.

[0060] The diameter of the sample tube 146 is, for example, within a range of 0.5 to 2 mm. In particular, when the diameter of the sample tube 146 is about 1 mm or less, the sample tube 146 is likely to stop midway through its passage due to static electricity, dirt on the sample tube surface, etc. In the embodiment, as described above, the load unit and eject unit are provided, so that the sample tube can be reliably prevented from stopping when loading and ejecting the sample tube.

[0061] Two gas bearings 152, 154 are provided to surround the accommodation space 144. Each gas bearing 152, 154 is a mechanism for holding the sample tube 146 in a non-contact manner by blowing bearing gas against the side surface of the sample tube 146. In addition, a thrust gas bearing 156 is provided for blowing gas against one end surface of the sample tube 146. A drive unit 158 ​​generates a rotational force in the sample tube 146 by blowing drive gas against a plurality of turbine blades 148. Reference numeral 150 denotes the central axis of the sample tube 146, which coincides with the axis of rotation.

[0062] In this embodiment, even when the sample tube is rotating after loading, the load gas is supplied to the passage, that is, the first gas flow is maintained. Gas 162 from the first gas flow is blown against the other end face of the sample tube 146. The blowing direction of the gas 162 is opposite to the blowing direction of the gas from the thrust gas bearing 156. This makes it possible to hold the position of the sample tube 146 with high accuracy in the direction of the central axis 150.

[0063] Detector 160 detects the rotation of sample tube 146. Detector 160 has an optical fiber that emits laser light and an optical fiber that receives the laser light reflected by the sample tube (reflected light). Since marker 147 rotates with the rotation of sample tube 146, the amount of reflected light changes periodically. From this change, the number of rotations per unit time, i.e., the rotation speed, is calculated.

[0064] Fig. 6 shows a cross section of the carrier 26. Note that in Fig. 6, a plurality of pipes and the like are omitted from the illustration.

[0065] The carrier 26 has a main body 164, a cap 166, a movable member 168, and an opening / closing mechanism 170. The main body 164 has a through hole 172 for a load gas and a through hole 174 for an ejection gas. The main body 164 also has a through hole for a lift gas, but this is not shown in FIG. 1. A storage chamber 171 is formed in the main body 164. The upper end of the storage chamber 171 is connected to the outside world via a plurality of communication holes 173. The main body 164 has a protruding portion 164A protruding downward. A cap 166 is provided so as to cover the protruding portion 164A. The opening / closing mechanism 170 is provided inside the cap 166.

[0066] Reference numeral 176 indicates an enlarged view of a portion surrounded by a dashed circle in FIG. 6. A shaft portion of the movable member 168 passes through an opening 166A formed in the cap 166. In the illustrated configuration example, the opening / closing mechanism 170 has two levers 184, 186. The two levers 184, 186 are evenly arranged around a central axis of the carrier, specifically, on one side and the other side of the central axis. Each lever 184, 186 is a movable piece capable of rotating around the rotation shafts 180, 182.

[0067] The lever 184 has a shoulder 188 and an upper end 192. The shoulder 188 functions as a base that supports the sample tube 200 when the opening / closing mechanism 170 is in the closed state. A slope is formed on the underside of the shoulder 188. The upper end 192 abuts against a slope 196 formed on the protruding portion. When the lever 184 is in the lowered state, the lever 184 is in an upright position (vertical position). When the lever moves upward, the upper end 192 moves open along the slope 196 to the left in the figure, and the lever 184 is in an inclined position. In this state, the supporting function of the shoulder 188 disappears.

[0068] The levers 184 and 186 are in a line-symmetrical relationship. The lever 186 has a shoulder 190 and an upper end 194. The shoulder 190 functions as a base that supports the sample tube 200 when the opening / closing mechanism 170 is in a closed state. A slope is formed on the underside of the shoulder 190. The upper end 194 abuts against a slope 198 formed on the protruding portion. When the lever 186 is in a lowered state, the lever 186 is in an upright position (vertical position). When the lever 186 moves upward, the upper end 194 moves open toward the right in the figure along the slope 198, and the lever 186 is in an inclined position. In this state, the supporting function of the shoulder 190 disappears.

[0069] As indicated by the reference numeral 178, the movable member 168 is movable in the vertical direction. When the movable member 168 comes into contact with the tip of the shaft-shaped member and moves upward, the opening / closing mechanism 170 changes from the closed state to the open state. This opens the bottom of the storage chamber. When the carrier 26 leaves the tip of the shaft-shaped member and the movable member 168 moves downward, the opening / closing mechanism 170 changes from the open state to the closed state. This closes the bottom of the storage chamber.

[0070] Each of the levers 184, 186 is a movable element that constitutes the opening / closing mechanism 170. Three or more levers may be provided. Instead of multiple levers, multiple movable pieces or multiple spring members may be provided. In that case, each of the multiple spring members elastically deforms in accordance with the movement of the movable member 168. Multiple movable pieces or spring members are provided evenly around the central axis of the carrier 26.

[0071] FIG. 7 shows the connected state. After the carrier 26 falls, the carrier 26 is connected to the upper end 202 of the shaft-shaped member. This applies an upward force 204 to the movable member 168, which moves upward. This causes the opening and closing mechanism 170 to change from the closed state to the open state, as indicated by reference numeral 206. At the same time, load gas is supplied to the passage, and a first gas flow is generated. The sample tube in the storage chamber 171 moves downward due to the gravitational effect and the first gas flow. The storage chamber 171 is connected to the outside world through a plurality of communication holes 173 as described above. Atmosphere flows from the outside world into the storage chamber through the plurality of communication holes 173.

[0072] 8 shows the gas control executed by the main control unit. In the standby state, in S10, the carrier is placed in the guide member. The carrier falls, and a connected state is generated. In the standby state, the supply of ejection gas continues (see reference numeral 212), and the supply of lift gas also continues (see reference numeral 214). The flow rate of the lift gas is small enough not to impede the falling movement of the carrier.

[0073] In S12, the main control unit outputs a load instruction. For example, the load instruction may be output according to a predetermined operation by the user. When the load instruction is output, the supply of eject gas is stopped and the supply of load gas is started (see reference numeral 216). In S14, the loading of the sample tube is completed. That is, the sample tube is placed in the rotator. In practice, the completion of loading is determined when a certain time t1 has elapsed from the load instruction. Reference numeral 128 indicates the period of sample tube transport by the first gas flow generated by the supply of load gas.

[0074] In S16, a rotation command is output from the main control unit. This starts the supply of bearing gas and drive gas to the rotator (see reference numeral 222). After the rotation starts, in S20, it is determined whether the sample tube is rotating. Based on this determination, it is checked afterwards whether the sample tube is accommodated in the rotator. The error operation when the sample tube is not accommodated in the rotator will be described later.

[0075] In S18, NMR measurement is performed. The first gas flow is maintained throughout the entire NMR measurement period (see reference numeral 220). This suppresses positional deviation in the thrust direction of the sample tube. Note that the flow rate of the first gas flow may be changed during the NMR measurement period. For example, a first flow rate may be set during loading, and a second flow rate less than the first flow rate may be set during rotation (see reference numeral 224).

[0076] After the NMR measurement is completed, in S22, the main control unit outputs an eject command. At that point, the supply of the load gas is stopped, and at the same time, the eject gas is supplied, thereby generating a second gas flow (see reference numeral 226). In S24, the completion of the ejection is determined. In practice, the completion of the ejection is determined when a predetermined time t2 has elapsed since the ejection command. A sensor for detecting the sample tube may be provided in the carrier, and the completion of the ejection may be determined based on the output signal of the sensor.

[0077] In S26, the main control unit outputs a lift command. This causes lift gas to be supplied at a high flow rate (see reference numeral 228). The ascending gas flow lifts the carrier upward to a predetermined position. In S28, it is determined that the lift is complete. At that point, the flow rate of the lift gas is changed from a high flow rate to a low flow rate (see reference numeral 230). This creates a state (standby state) in S30 where the next carrier is awaited. In the standby state, both the ejection gas and the lift gas are flowed. This prevents foreign matter from entering the bore, including the passage.

[0078] An example of the operation of the sample tube transport device is shown in Fig. 9. Fig. 9 also shows the control contents of the main control unit. In Fig. 9, details of gas control are omitted.

[0079] In S50, the user places the carrier at the entrance of the guide member. Then, a coupled state occurs. In S52, the main control unit outputs a load instruction. In S54, the sample tube is loaded. That is, the sample tube is transferred from the carrier to the rotator. In S56, after the start of rotation, it is determined whether rotation is detected or not.

[0080] If rotation is detected in S56, NMR measurement is performed in S58. After the measurement is completed, the main control unit outputs an eject command in S60. The sample tube is ejected in S62. In S64, lift gas is supplied to lift the carrier upward.

[0081] On the other hand, if rotation is not detected in S56, it is determined in S66 whether the number of loading operations N has exceeded the maximum value Nmax. If the number of loading operations N is equal to or less than the maximum value Nmax, the number of loading operations N is incremented in S68, and the steps from S54 onwards are executed again. Note that the initial value of the number of loading operations N is 1. If it is determined in S66 that the number of loading operations N has exceeded the maximum value Nmax, an error process is executed in S70. For example, an error is notified to the user.

[0082] Another operation example of the sample tube transport device is shown in Fig. 10. In Fig. 10, the same steps as those shown in Fig. 9 are given the same step numbers, and their explanations are omitted. If the number of load operations N is equal to or less than the maximum value Nmax in S66, an eject command is output in S72, and an eject operation is executed in S74 accordingly. Furthermore, an operation to float the carrier is executed in S76. Then, the number of load operations N is incremented in S68. Thereafter, each step from S52 onwards is executed repeatedly. For example, when a defective coupling state of the carrier is suspected, the other operation example shown in Fig. 10 may be adopted.

[0083] Another example of the structure is shown in Figure 11. The structure 250 has a load unit 252 and an eject unit 254. The unit provided on the upper side is the load unit 252, and the unit provided on the lower side is the eject unit 254.

[0084] The load unit 252 injects load gas from the cone-shaped gap G3 to the first position P1. This generates a first gas flow. The eject unit 254 injects eject gas from the cone-shaped gap G4 to the second position P2. This generates a second gas flow. The outlet (injection port) of the gap G3 faces downward, and the outlet (injection port) of the gap G4 faces upward.

[0085] When loading a sample tube, negative pressure is generated in a first upstream section 256 upstream of the first position P1, and positive pressure is generated in a first downstream section 258 downstream of the first position P1. When ejecting a sample tube, negative pressure is generated in a second upstream section 260 upstream of the second position P2, and positive pressure is generated in a second downstream section 262 downstream of the second position P2.

[0086] Fig. 12 shows the operation of the structure shown in Fig. 11 when loading a sample tube. In the load unit 252, the load gas 264 is sprayed from the gap G3 to the first position P1, which generates a first gas flow. In the load unit 252, the load gas 264 is sprayed evenly against the side surface of the sample tube 266, so the attitude of the sample tube does not become unstable.

[0087] On the other hand, in the first downstream section 258, a positive pressure is generated, and if a small amount of gas flow is permitted in the gap G4, a gas flow 270 may occur that enters the gap G4. Such a gas flow 270 may cause the attitude of the sample tube 272 to become unstable. In order to avoid such a problem, it is desirable to employ the structure shown in Fig. 2. However, if the problem of the attitude of the sample tube 272 becoming unstable does not occur, the structure shown in Fig. 11 may be employed.

[0088] 13 shows a sample tube transfer device according to another embodiment. The sample tube transfer device 273 transfers sample tubes between the carrier 26 and the rotator 24. The sample tube transfer device 273 has a shaft member 280, a load unit 276, an eject unit 278, a shaft member 274, a curved tube, and the like.

[0089] The load unit 276 injects a load gas to a first position on the passage, thereby generating a first gas flow in the passage. The first gas flow is a downward flow in FIG. 13. The eject unit 278 injects an eject gas to a second position on the passage, thereby generating a second gas flow in the passage. The second gas flow is an upward flow in FIG. 13. The load unit 276 and the eject unit 278 may have the configuration shown in FIG. 2.

[0090] The load unit 276 and the eject unit 278 are provided in a position close to the carrier 26, specifically, outside the static magnetic field generator. In the configuration shown in Fig. 13, the carrier 26 does not drop or float. For example, the carrier 26 is attached to a shaft member 280 by a user.

[0091] In the configuration shown in Fig. 13, a first upstream section and a first downstream section are defined with a first position as a boundary, and a second upstream section and a second downstream section are defined with a second position as a boundary. When an excessively large transport force in the first downstream section or an insufficient transport force in the second upstream section becomes a problem, it is desirable to adopt the configuration shown in Fig. 1.

[0092] In the configuration shown in FIG. 13, the positions of the load unit 276 and the eject unit 278 The load unit 276 and the eject unit 278 may be disposed at an intermediate position inside the bore and above the NMR probe.

[0093] In the above embodiment, the sample tube is inserted from the upper side of the static magnetic field generator, but the sample tube may be inserted from the lower side of the static magnetic field generator. Even in this case, the same effect as the above embodiment can be obtained by setting the first position and the second position in the middle of the passage. In the above embodiment, a cryo-NMR measurement probe may be used.

[0094] The technique of blowing gas onto the other end face of the sample tube while the sample tube is rotating may be applied to a sample tube transfer device other than the sample tube transfer device according to the embodiment. Also, the carrier having the opening and closing mechanism may be applied to a sample tube transfer device other than the sample tube transfer device according to the embodiment (for example, a device for transferring a sample tube containing a solution sample). [Explanation of symbols]

[0095] 10 NMR measurement system, 12 static magnetic field generator, 14 NMR measurement probe, 18 sample tube transfer device, 24 rotator, 26 carrier (container), 30 structure, 34 load unit, 36 eject unit.

Claims

1. a load unit for injecting a load gas into a first position in a passage between a sample tube holder and a sample tube rotator prior to an NMR measurement of a sample in a sample tube, thereby generating a first gas flow for transporting the sample tube from the sample tube holder to the sample tube rotator; an ejection unit for injecting an ejection gas to a second position in the passage after the NMR measurement of the sample, thereby generating a second gas flow for transferring the sample tube from the sample tube rotator to the sample tube holder; Including, the load unit includes a first gap having a first outlet facing the sample tube rotator and for injecting the load gas into the passage; the eject unit includes a second gap having a second outlet facing the sample tube container and for injecting the eject gas into the passage; At least one of the first gap and the second gap is a cone-shaped gap formed around the passage, Among the first outlet and the second outlet, the outlet of the at least one cone-shaped gap is an annular outlet communicating with the passage. A sample tube transfer device comprising:

2. 2. The sample tube transport device according to claim 1, the first gap and the second gap are each a cone-shaped gap formed around the passage, The first outlet and the second outlet are each annular outlets communicating with the passage. A sample tube transfer device comprising:

3. 2. The sample tube transport device according to claim 1, Among the first position and the second position, the one closer to the sample tube rotator is the first position, and the one closer to the sample tube holder is the second position. A sample tube transfer device comprising:

4. 2. The sample tube transport device according to claim 1, The load unit and the eject unit are coupled together. A sample tube transfer device comprising:

5. A load unit for injecting a load gas into a first position in a passage between a sample tube holder and a sample tube rotator prior to NMR measurement of a sample in a sample tube, thereby generating a first gas flow that transfers the sample tube from the sample tube holder to the sample tube rotator; an ejection unit for injecting an ejection gas to a second position in the passage after the NMR measurement of the sample, thereby generating a second gas flow for transferring the sample tube from the sample tube rotator to the sample tube holder; Including, the sample tube rotator has a thrust gas bearing for blowing gas against one end surface of the sample tube accommodated therein; The load unit generates the first gas flow in a rotational state in which the sample tube rotates in the sample tube rotator; In the rotating state, gas from the first gas flow is blown against the other end surface of the sample tube. A sample tube transfer device comprising:

6. A load unit for injecting a load gas into a first position in a passage between a sample tube holder and a sample tube rotator prior to NMR measurement of a sample in a sample tube, thereby generating a first gas flow that transfers the sample tube from the sample tube holder to the sample tube rotator; an ejection unit for injecting an ejection gas to a second position in the passage after the NMR measurement of the sample, thereby generating a second gas flow for transferring the sample tube from the sample tube rotator to the sample tube holder; Including, The ejection unit generates the second gas flow even after the sample tube is returned into the sample tube container. A sample tube transfer device comprising:

7. A load unit for injecting a load gas into a first position in a passage between a sample tube holder and a sample tube rotator prior to NMR measurement of a sample in a sample tube, thereby generating a first gas flow that transfers the sample tube from the sample tube holder to the sample tube rotator; an ejection unit for injecting an ejection gas to a second position in the passage after the NMR measurement of the sample, thereby generating a second gas flow for transferring the sample tube from the sample tube rotator to the sample tube holder; Including, an upper end member surrounding at least an upper end portion of the passage; The sample tube container comprises: a storage chamber for storing the sample tube; an opening / closing mechanism that is provided at the bottom of the storage chamber and that changes from a closed state to an open state when the sample tube holder is connected to the upper end member and changes from the open state to a closed state when the sample tube holder is detached from the upper end member; Including, the opening and closing mechanism includes at least one movable element that supports the sample tube within the storage chamber in the closed state; a hollow guide member disposed within a bore of the static magnetic field generator; The sample tube holder is caused to perform a falling movement within the guide member, whereby the sample tube holder is connected to the upper end member. A sample tube transfer device comprising:

8. 8. The sample tube transport device according to claim 7, a lift unit for generating an ascending gas flow within the guide member to separate the sample tube holder from the guide member and to float the sample tube holder. A sample tube transfer device comprising:

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