JP2006234539A - Automatic sample exchanger for nmr apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an automatic sample exchanger for an NMR apparatus which can set a sample tube at a low position and achieve reduced cost. <P>SOLUTION: The automatic sample exchanger for an NMR apparatus comprises (1) a lifting means which is placed on the floor to lift the sample tube upwardly up to a predetermined height from a sample tube rack: (2) a relay means which is placed on a vibration isolation table, receives the sample tube lifted by the lifting means, and further lifts it upwardly up to a predetermined height: and (3) a transfer means which laterally moves the sample tube lifted by the relay means, and transfers it to immediately above a sample tube introduction port of a magnet device placed on the vibration isolation table. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to an automatic sample changer used for an NMR apparatus, and particularly for an NMR apparatus used in a pharmaceutical company or the like when routinely analyzing a large amount of a compound synthesized by a combichem-like method with an NMR apparatus at a high throughput. The present invention relates to an automatic sample analyzer.

  An NMR device applies a strong static magnetic field (main magnetic field) to a sample to induce a precession around the direction of the static magnetic field in the magnetic moment of a nucleus having a nuclear spin in the sample. NMR emitted when a precession of the nuclear magnetic moment is excited by applying a high-frequency magnetic field in a direction perpendicular to the magnetic field direction, and then the nuclear magnetic moment precession returns from the excited state to the ground state. This is an apparatus for observing a signal as a high-frequency magnetic field having a frequency specific to a sample.

  At present, a considerable part of the NMR measurement is routine measurement with a fixed procedure, and the sample is automatically taken in and out in order to improve the efficiency of setting and taking out the sample continuously. An automatic sample changer is used (Patent Documents 1 to 3).

  In the case of an automatic sample changer with a small number of samples that can be set automatically, as shown in Fig. 1, it is possible to attach an automatic sample changer directly to the top of the superconducting magnet (SCM) and perform NMR sample change It is. However, as the number of sample points increases, the table on which the sample is placed becomes larger, so that the attachment as shown in FIG. 1 becomes impossible. For this reason, the enlarged automatic sample changer must be placed on the floor.

  When the automatic sample changer placed on the floor is directly coupled to the SCM, the mechanical vibration of the floor is transmitted to the SCM via the automatic sample changer and appears as noise on the observed NMR spectrum. Therefore, in order to prevent such noise from being picked up, a method has been adopted in which the automatic sample changer and the SCM are placed on the same vibration isolation table and are shielded from mechanical vibrations on the floor.

  FIG. 2 is an example of a conventional floor-mounted automatic sample changer. In the figure, reference numeral 21 denotes a vibration isolator. On the anti-vibration table 21, an SCM 22 and an automatic sample changer 23 are placed. A turntable 24 in which sixteen sample tubes are arranged in the circumferential direction is provided on the upper part of the automatic sample changer 23. The turntable 24 can move a desired sample tube to the sampling position 25 by rotating.

  The desired sample tube moved to the sampling position 25 is pushed upward by the rod-shaped Z actuator 26 and is carried to the manipulator 28 through the cylindrical cylinder 27. When the manipulator 28 grasps the rotor of the sample tube, the manipulator 28 moves in the lateral direction and transports the sample tube to a position directly above the bore (sample tube inlet) of the SCM 22. The sample tube conveyed to the position immediately above the bore of the SCM 22 starts to descend by releasing the rotor of the sample tube held by the manipulator 28, and is introduced into the SCM 22 while being controlled by the air blowing up the bore. Provided for measurement.

  When the NMR measurement is completed, the sample tube is raised to the bore opening end of the SCM 22 by air. Therefore, the manipulator 28 grasps the rotor of the sample tube, moves in the lateral direction, and conveys the sample tube to a position directly above the cylindrical cylinder 27. The sample tube conveyed to the position directly above the cylindrical cylinder 27 is lowered downward by the Z actuator 26 and returns to the sampling position 25 of the turntable 24. Thereafter, the turntable 24 is rotated by a predetermined angle, and the next sample tube is carried to the sampling position 25. Thereafter, the same operation is repeated.

Japanese Patent Laid-Open No. 10-62315 US Pat. No. 5,534,780 U.S. Pat. No. 4,581,583

  By the way, in order to handle a large number of sample tubes, it is indispensable that the sample tubes can be set at a low position so that attachment and removal can be easily performed by human hands. However, in the prior art, in order to lift the sample tube high in the vertical direction, the sample tube is set on a turntable at a high position because a long Z actuator is employed. This is ergonomically undesirable.

  In addition, since a large number of sample tubes are handled, the turntable becomes large, and the automatic sample changer cannot be installed on the SCM, and is placed on the floor. It had to be mounted on a shaking table, and a large damping table was necessary. However, a large vibration isolation table is expensive and may lead to an increase in cost.

  In view of the above-described points, an object of the present invention is to provide an automatic sample exchange apparatus for an NMR apparatus in which a sample tube can be set at a low position and the cost is kept low.

In order to achieve this object, an automatic sample changer for an NMR apparatus according to the present invention comprises:
After lifting the sample tube upward from the sample tube rack placed on the floor, the sample tube is moved laterally and transported directly above the sample tube inlet of the magnet device placed on the anti-vibration table. An automatic sample changer for introducing a sample tube from directly above the apparatus into the magnet apparatus, taking out the sample tube from the magnet apparatus and returning it to the sample tube rack,
(1) A push-up means that is placed on the floor and pushes the sample tube upward from the sample tube rack to a predetermined height;
(2) A relay unit that is placed on a vibration isolation table, receives the sample tube pushed up by the push-up unit, and further lifts it up to a predetermined height;
(3) Conveying means for moving the sample tube lifted by the relay means in the lateral direction and conveying it directly above the sample tube inlet of the magnet device placed on the vibration isolation table;
It is characterized by having the following three means.

  Further, the relay means is configured to lift the sample tube to the upper limit of the relay means together with the carrier on which the sample tube is mounted if the sensor provided at the position for receiving the sample tube detects the presence of the sample tube. It is characterized by.

  The relay means is driven by an air cylinder.

  Further, in addition to the above three means, there is provided an axis alignment means for aligning the center axis of the push-up means placed on the floor and the center axis of the relay means placed on the vibration isolation table. .

According to the automatic sample changer for NMR apparatus of the present invention,
After lifting the sample tube upward from the sample tube rack placed on the floor, the sample tube is moved laterally and transported directly above the sample tube inlet of the magnet device placed on the anti-vibration table. An automatic sample changer for introducing a sample tube from directly above the apparatus into the magnet apparatus, taking out the sample tube from the magnet apparatus and returning it to the sample tube rack,
(1) A push-up means that is placed on the floor and pushes the sample tube upward from the sample tube rack to a predetermined height;
(2) A relay unit that is placed on a vibration isolation table, receives the sample tube pushed up by the push-up unit, and further lifts it up to a predetermined height;
(3) Conveying means for moving the sample tube lifted by the relay means in the lateral direction and conveying it directly above the sample tube inlet of the magnet device placed on the vibration isolation table;
Because it has three means,
It is possible to provide an automatic sample changer for an NMR apparatus in which a sample tube can be set at a low position and the cost is kept low.

  FIG. 3 is an example of a floor-standing type automatic sample exchange apparatus according to the present invention. In the figure, reference numeral 15 denotes a vibration isolator. Only the SCM 14 is placed on the vibration isolation table 15, and the automatic sample changer 1 is placed directly on the floor. In order to prevent the mechanical vibration of the floor from being directly transmitted to the SCM 14 via the automatic sample changer 1, the automatic sample changer 1 is separated from the SCM 14 and the sample tube transport unit 16 in a spatially non-contact manner. Yes. As a result, the SCM and the automatic sample changer need not be placed on one vibration isolator at the same time, so that the vibration isolator can be reduced in size and the cost can be reduced.

  A rack 3 placed on an XY stage 2 is placed inside the automatic sample changer 1. In the rack 3, a large number of sample tubes 4 are put together with sample containers for preventing the sample tubes 4 from being damaged in a state where the rotor is attached. Then, by moving the XY stage 2 in the XY direction, the desired sample tube 4 can be moved to the sampling position 17 at random.

  Above the sampling position 17, the sample tube transport unit 16 supported by the support column 13 installed on the anti-vibration table is located in contact with the automatic sample changer with a space. The C-shaped cylinder 7 and the lifter guide 18 of the sample tube transport unit 16 extend just above the sampling position 17 of the automatic sample changer 1.

  The desired sample tube 4 moved to the sampling position 17 is pushed upward together with the sample container and the carrier 5 attached to the tip of the Z actuator 6 by a rod-shaped Z actuator 6 shorter than the conventional one, and a C-shaped cylinder. 7 is inserted. At this position, if the sensor 10 detects that the sample tube rotor is present, the lifter 8 inserts the lifter pin 9 into the constriction at the intermediate portion of the carrier 5 and holds the sample tube together with the sample container and the carrier 5. The sample tube 4 is lifted to the upper limit along the guide 18 and the sample tube 4 is inserted into the manipulator 11. An air cylinder that is not affected by a magnetic field is used to drive the lifter 8.

  FIG. 4 is an enlarged view of the sample tube delivery portion. For reference, the conventional example and this example are displayed side by side. As is apparent from the figure, the difference between the two is that the prior art tried to lift the sample tube using only the Z actuator, but in the present invention, the sample tube was lifted halfway by the Z actuator. It was a two-stage configuration that took it over and relayed it with a lifter and lifted it further. As a result, the length of the Z actuator can be shortened by the length of the lifter, so that the rack for storing the sample tube can be placed at a lower position than in the prior art. As a result, the sample tube can be easily attached to and removed from the rack by a human hand, resulting in an ergonomic structure.

  Now, when a sensor (not shown) in the manipulator 11 determines that there is a sample tube, the manipulator 11 grips the rotor of the sample tube 4. When it is confirmed that the rotor has been gripped, the lifter 8 moves down along the lifter guide 18 and lowers the sample container and the carrier 5 back to the lower limit position of the C-shaped cylinder 7. At the same time, the manipulator 11 moves in the lateral direction and transports the sample tube 4 to a position directly above the bore (sample tube inlet) of the SCM 14. The sample tube conveyed to the position immediately above the bore of the SCM 14 starts to descend by releasing the rotor of the sample tube 4 held by the manipulator 11, and is introduced into the SCM 14 while being controlled by the air blowing up the bore. It is used for NMR measurement.

  When the NMR measurement is completed, the sample tube 4 is raised to the bore opening end of the SCM 14 by air. Therefore, the manipulator 11 grabs the rotor of the sample tube 4, moves in the lateral direction, and transports the sample tube 4 to a position directly above the C-shaped cylinder 7. The sample tube 4 conveyed to a position directly above the C-shaped cylinder 7 is temporarily held there.

  At this time, if a sensor (not shown) determines that there is a sample tube, the Z actuator 6 pushes up the sample container returned to the rack 3 together with the carrier 5 attached to the tip of the Z actuator 6, and the lifter 8 further They are lifted along the lifter guide 18 to the upper limit of the C-shaped cylinder 7. When it is confirmed that the sample container and the carrier 5 have reached the upper limit of the C-shaped cylinder 7, the manipulator 11 releases the gripped rotor and drops the sample tube 4 into the sample container.

  When the sample container receives the sample tube 4, the lifter 8 descends along the lifter guide 18 and transfers the sample tube 4 and the sample container to the Z actuator 6 at the lower limit position. The Z actuator 6 descends and returns the sample tube 4 and the sample container to the original position of the rack 3. After that, the XY stage 2 moves by a predetermined amount and carries the next sample tube 4 to the sampling position 17, and the same operation is repeated thereafter.

  In the present embodiment, as described above, the sample tube is conveyed via the sample container, the carrier, or the rotor. Therefore, since the sample tube (made of glass) is not directly gripped, there is little risk of breakage. Also, even for SCMs of different sizes (for 400 MHz, 500 MHz, 600 MHz, etc.), as long as the lengths of the C-shaped cylinder 7 and the lifter guide 18 are changed, the dimensions of the automatic sample changer 1 may be the same. High versatility.

  In the present embodiment, since the sample tube transport unit 16 and the automatic sample changer 1 are separated spatially in a non-contact manner, the center axis of the C-shaped cylinder 7 on the sample tube transport unit 16 side and the automatic sample change It is indispensable for relaying the sample tube 4 to be controlled so that the central axis of the Z actuator 6 on the apparatus 1 side always coincides.

  This axial alignment can be performed by a positioning sensor 12 comprising a combination of a light receiving sensor provided on the support column 13 side and a light emitting diode provided on the automatic sample changer 1 side. Since the positional deviation information is fed back to the coordinate value of the XY stage 2 in the automatic sample changer 1, even if the positional deviation occurs for some reason, the positional deviation corrects the coordinate value of the XY stage 2. Is compensated by

  It can be widely used for routine measurement using an NMR apparatus.

It is a figure which shows an example of the conventional automatic sample change apparatus for NMR apparatuses. It is a figure which shows an example of the conventional automatic sample change apparatus for NMR apparatuses. It is a figure which shows one Example of the automatic sample change apparatus for NMR apparatuses concerning this invention. It is a figure which shows one Example of the automatic sample change apparatus for NMR apparatuses concerning this invention.

Explanation of symbols

1: automatic sample changer (ASC), 2: XY stage, 3: rack, 4: sample tube, 5: carrier, 6: Z actuator, 7: C-shaped cylinder, 8: lifter, 9: lifter pin, 10: sensor 11: Manipulators, 12: Positioning sensors (plural), 13: Supports, 14: Superconducting magnet (SCM), 15: Anti-vibration table, 16: Sample tube transport unit, 17: Sampling position, 18: Lifter guide, 21 : Anti-vibration table, 22: superconducting magnet (SCM), 23: automatic sample changer (ASC), 24: turntable, 25: sampling position, 26: Z actuator, 27: cylindrical cylinder, 28: manipulator

Claims (4)

After lifting the sample tube upward from the sample tube rack placed on the floor, the sample tube is moved laterally and transported directly above the sample tube inlet of the magnet device placed on the anti-vibration table. An automatic sample changer for introducing a sample tube from directly above the apparatus into the magnet apparatus, taking out the sample tube from the magnet apparatus and returning it to the sample tube rack,
(1) A push-up means that is placed on the floor and pushes the sample tube upward from the sample tube rack to a predetermined height;
(2) A relay unit that is placed on a vibration isolation table, receives the sample tube pushed up by the push-up unit, and further lifts it up to a predetermined height;
(3) Conveying means for moving the sample tube lifted by the relay means in the lateral direction and conveying it directly above the sample tube inlet of the magnet device placed on the vibration isolation table;
An automatic sample changer for an NMR apparatus comprising the following three means. The relay means is configured to lift the sample tube to the upper limit of the relay means together with the carrier on which the sample tube is mounted if the sensor provided at the position for receiving the sample tube detects the presence of the sample tube. The automatic sample changer for an NMR apparatus according to claim 1. 3. The automatic sample exchange apparatus for an NMR apparatus according to claim 1, wherein the relay means is driven by an air cylinder. 2. The apparatus according to claim 1, further comprising an axis aligning means for aligning the center axis of the push-up means placed on the floor and the center axis of the relay means placed on the vibration isolator in addition to the three means. The automatic sample changer for NMR apparatus according to 1.

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