A solid nuclear magnetic resonance spectrometer automatic sample injector and sample injection method

Abstract

The invention relates to an automatic sample injector for a solid nuclear magnetic resonance spectrometer, comprising a bracket, a servo motor is fixed on the bracket, the lower end of the servo motor is connected to the shaft of a sample bin turntable through a coupling and a shaft holding regulator, and then connected to the sample bin turntable, the lower end of the sample bin is connected to a sample funnel conduit, a Y-shaped sample conduit side tube and a Y-shaped sample conduit straight tube, and then connected to a sample collection bin, the Y-shaped sample conduit straight tube is connected to the nuclear magnetic resonance spectrometer sample tube conduit at the top of a magnet of the solid nuclear magnetic resonance spectrometer, two sides of the Y-shaped sample conduit straight tube are provided with opposite-radiation photoelectric sensors, the photoelectric sensor and the servo motor are both connected to a control box, and a liquid crystal panel is provided on the control box to perform parameter setting operations and display status information.

Description

Technical Field

[0001] The invention relates to an automatic sample injector, in particular to an automatic sample injector and a sample injection method in the technical field of solid nuclear magnetic resonance spectrometer. Background Art

[0002] Nuclear magnetic resonance testing technology is one of the important means of contemporary material analysis and testing and structural identification. Solid-state nuclear magnetic resonance spectrometer is mainly used for structural analysis and performance research of solid substances, and is widely used in biology, medicine, materials, chemistry, plants, petrochemicals, food, organic synthesis and many other fields.

[0003] At present, liquid nuclear magnetic resonance spectrometers have successfully realized automatic sample replacement by automatic sample injectors; while solid nuclear magnetic resonance spectrometers all use manual sampling, which requires someone to be on duty during testing, and the efficiency of equipment utilization needs to be improved urgently. Summary of the invention

[0004] The problem to be solved by the present invention is that the existing solid-state nuclear magnetic resonance spectrometer does not have an automatic sample injector and cannot replace samples when unattended. The technical solution of the present invention is:

[0005] The invention discloses an automatic sampler for a solid nuclear magnetic resonance spectrometer, comprising a bracket, a servo motor is fixed on the bracket, the lower end of the servo motor is connected to the shaft of a sample bin turntable through a coupling and a shaft holding regulator, and then connected to the sample bin turntable, the lower end of the sample bin is connected to a sample funnel conduit, a Y-shaped sample conduit side tube and a Y-shaped sample conduit straight tube, and then connected to a sample collection bin, the Y-shaped sample conduit straight tube is connected to the nuclear magnetic resonance spectrometer sample tube conduit at the top of a magnet of the solid nuclear magnetic resonance spectrometer, two sides of the Y-shaped sample conduit straight tube are provided with opposite-radiation photoelectric sensors, the photoelectric sensors and the servo motor are both connected to a control box, and a liquid crystal panel is provided on the control box for parameter setting operation and status information display.

[0006] Furthermore, the sample chamber is provided with a turntable positioning point and a reflective photoelectric sensor, and the sample chamber is initially positioned by the turntable positioning point and the reflective photoelectric sensor.

[0007] Furthermore, the bracket clamps two liquid helium inlet and outlet tubes above the nuclear magnetic resonance spectrometer magnet through two liquid helium inlet and outlet tube clamps respectively, the lifting ring fixture and the nuclear magnetic resonance spectrometer magnet lifting ring are locked by bolts, and the base of the automatic sampler bracket is formed by connecting two weight-reducing hole-dug horizontal support rods, and the vertical support tube is fixed to the bracket base through a support rod connector.

[0008] Furthermore, the vertical support tube clamp holds the vertical support tube to fix the weight-reducing hole-digging horizontal arm, the servo motor is fixed on the end of the weight-reducing hole-digging horizontal arm, the display controller of the reflective photoelectric sensor and the through-beam photoelectric sensor is fixed on the weight-reducing hole-digging horizontal arm, the servo motor is connected to the control host through a power line and a signal line, and the control box includes a power supply, a single-chip microcomputer, and a touch screen.

[0009] Furthermore, a plurality of holes are provided on the sample chamber turntable in a rotationally symmetrical manner at the center thereof for accommodating sample tubes.

[0010] Furthermore, the sample bin turntable is a circular structure, with a plurality of sample bins symmetrically distributed at the center for containing sample tubes; a sample bin bottom plate injection hole is provided below the sample bin, and its size is the same as the diameter of the sample bin.

[0011] Furthermore, the sample funnel conduit is connected to the Y-shaped sample conduit straight tube through a Y-shaped sample conduit side tube; the upper and lower ends of the sample conduit straight tube are both open, and their size is larger than the diameter of the sample tube, and the sample conduit straight tube is located in the center of the collection chamber.

[0012] Furthermore, the collection bin is a cylindrical cavity, including a collection bin top plate and a collection bin side, as well as a collection bin bottom plate and a collection bin sample outlet, and a collection bin buffer pad is provided on the collection bin bottom plate; and a side sliding door is provided on the collection bin side.

[0013] Furthermore, the Y-shaped sample conduit is connected to the sample tube conduit of the nuclear magnetic resonance spectrometer, and the inner diameters of the connection are the same to ensure a smooth inner wall; an air blowing device is provided below the sample tube conduit of the nuclear magnetic resonance spectrometer to eject the sample tube.

[0014] According to another aspect of the present invention, a method for automatic sampling of a solid-state nuclear magnetic resonance spectrometer is provided, comprising the following steps:

[0015] Step 1. Press the "Reset" button on the LCD panel of the host, and the servo motor will rotate. The sample bin turntable will rotate through the coupling, the shaft regulator, and the shaft of the sample bin turntable. When the white turntable positioning point is facing the reflective photoelectric sensor, the light emitted by the reflective photoelectric sensor is reflected back through the white turntable positioning point. The host receives the signal from the reflective photoelectric sensor and then rotates a preset angle to align the sample bin bottom plate injection hole with the No. 0 sample bin. The reset action is completed.

[0016] Step 2, put sample tubes No. 1 to 6 into the sample bin in sequence, press the "Start" button on the LCD panel of the host, and the servo motor rotates a fixed angle to align the No. 1 sample bin with the sample inlet hole on the bottom plate of the sample bin, and the No. 1 sample tube enters the sample tube conduit on the top of the nuclear magnetic resonance spectrometer through the sample funnel conduit, the Y-type sample conduit side tube, and the Y-type sample conduit straight tube; when the sample tube passes through the Y-type sample conduit straight tube, the opposing photoelectric sensor transmits a signal to the host, and the sample tube entry action is completed;

[0017] Step 3, after the nuclear magnetic resonance spectrometer completes the test, the compressed gas pushes the sample tube from the nuclear magnetic resonance probe through the sample tube guide tube, the Y-shaped sample guide tube straight tube, and enters the collection bin from the sample outlet of the collection bin, bounces off the cushions on the top and bottom of the collection bin several times, and falls into the collection bin. When the sample tube passes through the Y-shaped sample guide tube straight tube, the opposing photoelectric sensor transmits the signal to the host again, and the sample tube collection action is completed;

[0018] Step 4, when the host receives the signals of the two opposing photoelectric sensors in sequence, the servo motor rotates a fixed angle to align the No. 2 sample chamber with the sample inlet hole on the bottom plate of the sample chamber, and the No. 2 sample tube enters the nuclear magnetic resonance spectrometer, and the sample tube entry action and collection action are repeated;

[0019] Step 5: When the servo motor rotates a fixed angle and does not receive a signal from the photoelectric sensor within a predetermined time, it will feedback "injection completed";

[0020] Step 6: When all samples have been tested, slide the side sliding door of the collection chamber sideways, take out all sample tubes, and close the side sliding door of the collection chamber. All actions are completed.

[0021] Beneficial effects:

[0022] The present invention adopts a servo motor to control the tray-type sample bin, which can accurately control the angle of rotation of the sample bin, ensuring that the sample tube to be tested can slide from the sample bin through the Y-type sample conduit side tube into the rotor conduit at the top of the magnet of the solid nuclear magnetic resonance spectrometer, and finally enter the nuclear magnetic resonance probe. The sample tube after the test is pushed by compressed gas from the nuclear magnetic probe through the rotor conduit and the Y-type sample conduit straight tube into the collection bin. After setting various parameters, the solid nuclear magnetic spectrometer can be in an unattended state and work independently, which greatly improves the detection speed of samples, improves the utilization efficiency of equipment, and greatly alleviates the contradiction between insufficient equipment time and scientific research needs. The utilization efficiency of the nuclear magnetic resonance spectrometer is improved and the manpower of operation is saved. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 : Schematic diagram of the structure of the automatic sample injector of the present invention;

[0024] Figure 2 : Enlarged view of the connection between the Y-type sample duct and the nuclear magnetic resonance spectrometer sample tube duct.

[0025] Figure 3 : Schematic diagram of the automatic sampler bracket structure.

[0026] Description of reference numerals:

[0027] 1 servo motor, 2 coupling, 3 shaft regulator, 4 sample bin turntable shaft, 5 sample bin turntable, 6 sample bin, 7 sample tube, 8 turntable positioning point, 9 sample bin bottom plate, 10 reflective photoelectric sensor, 11 sample bin bottom plate injection hole, 12 sample funnel guide tube, 13 Y-type sample guide tube side tube, 14 collection bin top plate, 15 collection bin buffer pad, 16 collection bin side sliding door, 17 collection bin side, 18 collection bin bottom plate, 19 collection bin sample outlet, 20 through-beam photoelectric sensor, 21 Y-type sample guide tube straight tube, 22 nuclear magnetic resonance spectrometer sample tube guide tube, 23 nuclear magnetic resonance spectrometer magnet liquid helium inlet and outlet tube, 24 nuclear magnetic resonance spectrometer magnet lifting ring, 25 liquid helium inlet and outlet tube clamp, 26 lifting ring fixer, 27 weight-reducing hole-digging horizontal support rod, 28 support rod connector, 29 vertical support tube, 30 vertical support tube clamp, 31 weight-reducing hole-digging horizontal arm. DETAILED DESCRIPTION

[0028] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the protection scope of the present invention.

[0029] See also Figure 1 According to one embodiment of the present invention, there is provided a solid-state nuclear magnetic resonance spectrometer automatic sample injector, comprising: a bracket (see Figure 3 ), a servo motor 1 is fixed on the bracket, the lower end of the servo motor 1 is connected to the shaft 4 of the sample chamber turntable through a coupling 2 and a shaft regulator 3, and is connected to the sample chamber turntable 5. The sample chamber 6 is provided with a turntable positioning point 8 and a reflective photoelectric sensor 10. The initial positioning of the sample chamber can be performed through the turntable positioning point and the reflective photoelectric sensor 10. The lower end of the sample chamber 6 is connected to a sample funnel conduit 12 and a Y-type sample conduit side tube 13, and a Y-type sample conduit straight tube 21. The Y-type sample conduit straight tube 21 is connected to the nuclear magnetic resonance spectrometer sample tube conduit 22 at the top of the solid nuclear magnetic resonance spectrometer magnet, see Figure 2 It is an enlarged view of the connection between the Y-shaped sample conduit and the nuclear magnetic resonance spectrometer sample tube conduit 22; opposite-beam photoelectric sensors 20 are provided on both sides of the Y-shaped sample conduit straight tube 21, and the photoelectric sensors and servo motors are connected to the control box, which has a liquid crystal panel for parameter setting operations and status information display.

[0030] The sample bin turntable is a circular structure, with a plurality of sample bins 6 symmetrically distributed in the center for holding sample tubes 7; a sample bin bottom plate injection hole 11 is provided below the sample bin, and its size is the same as the diameter of the sample bin 6;

[0031] The sample funnel conduit 12 is connected to the Y-shaped sample conduit straight tube 21 through the Y-shaped sample conduit side tube 13; the upper and lower ends of the sample conduit straight tube 21 are both open, and the size thereof is larger than the diameter of the sample tube, and the sample conduit straight tube 21 is located in the center of the collection chamber;

[0032] The collecting bin is a cylindrical cavity, including a collecting bin top plate 14, a collecting bin side 17, a collecting bin bottom plate 18, and a collecting bin sample outlet 19. A collecting bin buffer pad 15 is provided on the collecting bin bottom plate; a side sliding door 16 is provided on the collecting bin side 17;

[0033] See also Figure 2 The Y-shaped sample conduit is connected to the nuclear magnetic resonance spectrometer sample tube conduit 22, and the inner diameters of the connection are the same to ensure that the inner wall is smooth; a blowing device is provided below the nuclear magnetic resonance spectrometer sample tube conduit 22 for ejecting the sample tube 7;

[0034] The automatic sampler bracket clamps two liquid helium inlet and outlet tubes 23 above the nuclear magnetic resonance spectrometer magnet through two liquid helium inlet and outlet tube clamps 25, and the lifting ring fixture 26 is locked with the nuclear magnetic resonance spectrometer magnet lifting ring 24 by bolts. These three points are directly connected through two weight-reducing hole-digging horizontal support rods 27 to form the base of the automatic sampler bracket. The vertical support tube 29 is fixed to the bracket base through the support rod connector 28. The vertical support tube clamp 30 holds the vertical support tube 29 tightly to fix the weight-reducing hole-digging horizontal arm 31. Figure 1 The servo motor 1 is fixed to the end of the weight-reducing hole-digging horizontal arm 31. Figure 1 The display controller of the reflective photoelectric sensor 10 and the through-beam photoelectric sensor 20 is fixed on the weight-reducing hole-digging horizontal arm 31. The servo motor 1 is connected to the control host through a power line and a signal line. The control box includes a power supply, a single-chip microcomputer, and a touch screen. The pre-made software controls the machine to "reset" and "start" sampling, as well as to check the operating status and error information.

[0035] The present invention controls the sample tube of the automatic sampler to enter the probe of the nuclear magnetic resonance spectrometer through the program compiled in the control host, and collects the sample tube ejected from the spectrometer probe after the test is completed. The specific detailed process is as follows:

[0036] Step 1, by controlling the host touch screen and pressing the "reset" button, the servo motor (1) rotates, and the sample bin turntable (5) is driven to rotate through the coupling (2), the shaft adjusting device (3), and the shaft (4) of the sample bin turntable. When the white turntable positioning point (8) faces the reflective photoelectric sensor (10), the light emitted by the reflective photoelectric sensor (10) is reflected back through the white turntable positioning point (8). The host receives the signal of the reflective photoelectric sensor (10), and then rotates a preset angle to align the sample bin bottom plate injection hole (11) with the No. 0 sample bin (6), and the reset action is completed;

[0037] Step 2, place sample tubes No. 1-6 (7) in the sample bin (6) in sequence, press the "Start" button on the control host touch screen, and the servo motor (1) rotates a fixed angle to align the No. 1 sample bin (6) with the sample bin bottom plate injection hole (11), and the No. 1 sample tube (7) enters the sample tube conduit (22) at the top of the nuclear magnetic resonance spectrometer through the sample funnel conduit (12), the Y-type sample conduit side tube (13), and the Y-type sample conduit straight tube (21). When the sample tube (7) passes through the Y-type sample conduit straight tube (21), the opposing photoelectric sensor (20) transmits a signal to the host, and the sample tube entry action is completed;

[0038] Step 3, after the nuclear magnetic resonance spectrometer completes the test, the compressed gas pushes the sample tube (7) from the nuclear magnetic resonance probe through the sample tube conduit (22), the Y-shaped sample conduit straight tube (21), and enters the collection bin from the collection bin sample outlet (19), bounces several times on the buffer pads (15) on the top and bottom of the collection bin, and falls into the collection bin. When the sample tube (7) passes through the Y-shaped sample conduit straight tube (21), the opposing photoelectric sensor (20) transmits the signal to the host again, and the sample tube collection action is completed;

[0039] Step 4: After the host receives signals from the two opposing photoelectric sensors (20) in sequence, the servo motor (1) rotates at a fixed angle so that the No. 2 sample chamber (6) is aligned with the sample chamber bottom plate sample inlet hole (12), and the No. 2 sample tube (7) enters the nuclear magnetic resonance spectrometer, and the sample tube entry action and collection action are repeated;

[0040] Step 5: When the servo motor (1) rotates a fixed angle and does not receive a signal from the through-beam photoelectric sensor (20) within a certain period of time, a "sample injection end" signal is fed back.

[0041] Step 6: When all samples have been tested, the side sliding door (16) of the collection chamber can be slid sideways to take out all sample tubes (7), and the side sliding door (16) of the collection chamber is closed, and all actions are completed.

[0042] Although the above describes the illustrative specific embodiments of the present invention to facilitate those skilled in the art to understand the present invention, and it should be clear that the present invention is not limited to the scope of the specific embodiments, for those of ordinary skill in the art, as long as various changes are within the spirit and scope of the present invention as defined and determined by the attached claims, these changes are obvious, and all inventions and creations using the concept of the present invention are protected.

Claims

1. A solid-state nuclear magnetic resonance spectrometer automatic sampling method, characterized in that: The steps include: Step 1. Press the "Reset" button on the LCD panel of the host, and the servo motor will rotate. The sample bin turntable will rotate through the coupling, the shaft regulator, and the shaft of the sample bin turntable. When the white turntable positioning point is facing the reflective photoelectric sensor, the light emitted by the reflective photoelectric sensor is reflected back through the white turntable positioning point. The host receives the signal from the reflective photoelectric sensor and then rotates a preset angle to align the sample bin bottom plate injection hole with the No. 0 sample bin. The reset action is completed. Step 2, put sample tubes No. 1 to 6 into the sample bin in sequence, press the "Start" button on the LCD panel of the host, and the servo motor rotates a fixed angle to align the No. 1 sample bin with the sample inlet hole on the bottom plate of the sample bin. Sample tube No. 1 enters the sample tube conduit on the top of the nuclear magnetic resonance spectrometer through the sample funnel conduit, the Y-type sample conduit side tube, and the Y-type sample conduit straight tube; when the sample tube passes through the Y-type sample conduit straight tube, the opposing photoelectric sensor transmits a signal to the host, and the sample tube entry action is completed; Step 3, after the nuclear magnetic resonance spectrometer completes the test, the compressed gas pushes the sample tube from the nuclear magnetic resonance probe through the sample tube guide tube, the Y-shaped sample guide tube straight tube, and enters the collection bin from the sample outlet of the collection bin, bounces off the cushions on the top and bottom of the collection bin several times, and falls into the collection bin. When the sample tube passes through the Y-shaped sample guide tube straight tube, the opposing photoelectric sensor transmits the signal to the host again, and the sample tube collection action is completed; Step 4, when the host receives the signals of the two opposing photoelectric sensors in sequence, the servo motor rotates a fixed angle to align the No. 2 sample chamber with the sample inlet hole on the bottom plate of the sample chamber, and the No. 2 sample tube enters the nuclear magnetic resonance spectrometer, and the sample tube entry action and collection action are repeated; Step 5: When the servo motor rotates a fixed angle and does not receive a signal from the photoelectric sensor within a predetermined time, the "injection is completed" signal is fed back; Step 6: When all samples have been tested, slide the side sliding door of the collection chamber sideways, take out all sample tubes, and close the side sliding door of the collection chamber. All actions are completed.

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