CN111856057A - Automatic sample injector of solid nuclear magnetic resonance spectrometer and sample injection method - Google Patents
Automatic sample injector of solid nuclear magnetic resonance spectrometer and sample injection method Download PDFInfo
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- CN111856057A CN111856057A CN202010863146.4A CN202010863146A CN111856057A CN 111856057 A CN111856057 A CN 111856057A CN 202010863146 A CN202010863146 A CN 202010863146A CN 111856057 A CN111856057 A CN 111856057A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to an automatic sample injector of a solid nuclear magnetic resonance spectrometer, which comprises: the support, be fixed with servo motor on the support, the servo motor lower extreme passes through the shaft coupling, embraces the axle of shaft regulator connection sample storehouse carousel, and the sample storehouse carousel is reconnected, and the sample storehouse lower extreme even has sample funnel pipe and Y type sample pipe side pipe and Y type sample pipe straight tube, and the storehouse is collected to the sample to the reconnection, the nuclear magnetic resonance spectrometer sample pipe at solid nuclear magnetic resonance spectrometer magnet top is connected to Y type sample pipe straight tube, and Y type sample pipe straight tube both sides are equipped with correlation formula photoelectric sensor, and photoelectric sensor and servo motor all connect the control box, have liquid crystal display panel on the control box can carry out parameter setting operation and status information display.
Description
Technical Field
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 spectrometers.
Background
The nuclear magnetic resonance testing technology is one of the important means of the analysis test and the structure identification of the contemporary substance, and the solid nuclear magnetic resonance spectrometer is mainly used for the structure analysis and the performance research of the solid substance and is widely applied to various aspects of biology, medicines, materials, chemistry, plants, petrochemical industry, foods, organic synthesis and the like.
The liquid nuclear magnetic resonance spectrometer successfully realizes automatic sample changing of an automatic sample injector at present; and the solid nuclear magnetic resonance spectrometer adopts manual sample introduction, so that the test needs to be attended, and the utilization efficiency of the equipment needs to be improved urgently.
Disclosure of Invention
The invention aims to solve the problems that: the existing solid nuclear magnetic resonance spectrometer has no automatic sample injector, and the sample cannot be replaced when the existing solid nuclear magnetic resonance spectrometer is unattended. The technical scheme of the invention is as follows:
a solid nuclear magnetic resonance spectrometer autosampler, comprising: the support, be fixed with servo motor on the support, the servo motor lower extreme passes through the shaft coupling, embraces the axle of shaft regulator connection sample storehouse carousel, and the sample storehouse carousel is reconnected, and the sample storehouse lower extreme even has sample funnel pipe and Y type sample pipe side pipe and Y type sample pipe straight tube, and the storehouse is collected to the sample to the reconnection, the nuclear magnetic resonance spectrometer sample pipe at solid nuclear magnetic resonance spectrometer magnet top is connected to Y type sample pipe straight tube, and Y type sample pipe straight tube both sides are equipped with correlation formula photoelectric sensor, and photoelectric sensor and servo motor all connect the control box, have liquid crystal display panel on the control box can carry out parameter setting operation and status information display.
Furthermore, the sample cabin is provided with a turntable positioning point and a reflection type photoelectric sensor, and the initial positioning of the sample cabin is carried out through the turntable positioning point and the reflection type photoelectric sensor.
Furthermore, the support clamps two liquid helium inlet and outlet pipes above the magnetic body of the nuclear magnetic resonance spectrometer through two liquid helium inlet and outlet pipe clamps respectively, the hoisting ring fixer and the hoisting ring of the magnetic body of the nuclear magnetic resonance spectrometer are locked through bolts, the two weight-reducing hole-digging horizontal support rods are connected to form a base of the automatic sample injector support, and the vertical support pipe is fixed on the base of the support through the support rod connector.
Furthermore, the vertical supporting tube clamp tightly holds the vertical supporting tube to fix the weight-reduction hole-digging horizontal arm, the servo motor is fixed at the tail end of the weight-reduction hole-digging horizontal arm, the display controllers of the reflection type photoelectric sensor and the correlation type photoelectric sensor are fixed on the weight-reduction hole-digging horizontal arm, the servo motor is connected with the control host through a power line and a signal line, and the control box comprises a power supply, a single chip microcomputer and a touch screen.
Furthermore, a plurality of holes are arranged on the sample bin turntable in a central rotation symmetry manner and are used for containing sample tubes.
Furthermore, the sample bin rotary disc is of a circular structure, and a plurality of sample bins are arranged in the center symmetry distribution and used for containing sample tubes; the sample bin is provided with a sample bin bottom plate sample inlet hole below, and the size of the sample bin bottom plate sample inlet hole is the same as the diameter of the sample bin.
Furthermore, the sample funnel conduit is connected with the Y-shaped sample conduit straight pipe through a Y-shaped sample conduit side pipe; the upper end and the lower end of the sample conduit straight pipe are both provided with openings, the size of each opening is larger than the diameter of the sample conduit, and the sample conduit straight pipe is positioned in the center of the collection bin.
Furthermore, the collecting bin is a cylindrical cavity and comprises a collecting bin top plate, a collecting bin side surface, a collecting bin bottom plate and a collecting bin sample outlet, wherein a collecting bin buffer cushion is arranged on the collecting bin bottom plate; the side surface of the collecting bin is provided with a side surface sliding door.
Furthermore, the Y-shaped sample conduit is connected with the sample tube conduit of the nuclear magnetic resonance spectrometer, and the inner diameters of the joints are the same, so that the inner wall is ensured to be smooth; and an air blowing device is arranged below the sample tube guide tube of the nuclear magnetic resonance spectrometer and is used for ejecting the sample tube.
According to another aspect of the present invention, an automatic sample injection method for a solid nuclear magnetic resonance spectrometer is provided, which includes the following steps:
step 2, sequentially placing sample tubes No. 1-6 into a sample bin, pressing a 'start' button by a liquid crystal panel of a host computer, rotating a servo motor by a fixed angle to enable the sample bin No. 1 to be aligned with a sample inlet hole of a bottom plate of the sample bin, and enabling the sample tubes No. 1 to enter sample tube guide tubes at the top of a nuclear magnetic resonance spectrometer through a sample funnel guide tube, a Y-shaped sample guide tube side tube and a Y-shaped sample guide tube straight tube; when the sample tube passes through the Y-shaped sample tube straight tube, the correlation photoelectric sensor transmits a signal to the host, and the sample tube enters to finish the action;
step 4, after the host computer receives the signals of the correlation type photoelectric sensor twice in sequence, the servo motor rotates a fixed angle, so that the No. 2 sample bin aligns to the sample inlet hole of the sample bin bottom plate, the No. 2 sample tube enters the nuclear magnetic resonance spectrometer, and the sample tube entering action and the collecting action are repeated;
step 5, when the servo motor rotates for a fixed angle and does not receive the signal of the correlation type photoelectric sensor within preset time, feeding back 'sample introduction is finished';
and 6, when all samples are tested, laterally sliding the side sliding door of the collection bin, taking out all sample tubes, and closing the side sliding door of the collection bin to finish all actions.
Has the advantages that:
the invention adopts a servo motor to control the disc type sample bin, can accurately control the rotation angle of the sample bin, ensures that a sample tube to be tested can slide into the rotor guide tube at the top of the magnet of the solid nuclear magnetic resonance spectrometer from the sample bin through the Y-shaped sample guide tube side tube and finally enters the nuclear magnetic resonance probe, and the sample tube after being tested is pushed from the nuclear magnetic resonance probe by compressed gas to enter the collection bin through the rotor guide tube and the Y-shaped sample guide tube straight tube. After various parameters are set, the solid nuclear magnetic spectrometer can be in an unattended state and works automatically, the detection speed of a sample is greatly improved, the utilization efficiency of equipment is improved, and the contradiction between the machine-hour shortage of the equipment and the scientific research requirement is greatly relieved. The use efficiency of the nuclear magnetic resonance spectrometer is improved, and the manpower for operation is saved.
Drawings
FIG. 1: the automatic sample injector is structurally schematic;
FIG. 2: and an enlarged view of the joint of the Y-shaped sample conduit and the sample tube conduit of the nuclear magnetic resonance spectrometer.
FIG. 3 is a schematic diagram of the autosampler cradle.
Description of reference numerals:
1 servo motor, 2 shaft coupling, 3 shaft holding regulator, 4 sample cabin turntable shaft, 5 sample cabin turntable, 6 sample cabin, 7 sample tube, 8 turntable positioning point, 9 sample cabin bottom plate, 10 reflection type photoelectric sensor, 11 sample cabin bottom plate sample inlet hole, 12 sample funnel conduit, 13Y type sample conduit side tube, 14 collection cabin top plate, 15 collection cabin buffer cushion, 16 collection cabin side sliding door, 17 collection cabin side, 18 collection cabin bottom plate, 19 collection cabin sample outlet, 20 correlation type photoelectric sensor, 21Y type sample conduit straight tube, 22 nuclear magnetic resonance spectrometer sample conduit, 23 nuclear magnetic resonance spectrometer magnet liquid helium inlet tube, 24 nuclear magnetic resonance spectrometer magnet hoisting ring, 25 liquid helium inlet and outlet pipe clamp, 26 hoisting ring fixer, 27 weight reducing hole digging horizontal support rod, 28 support rod connector, 29 vertical support tube, 30 vertical support tube clamp, 31 lightening the hole digging horizontal arm.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person skilled in the art based on the embodiments of the present invention belong to the protection scope of the present invention without creative efforts.
Referring to fig. 1, according to an embodiment of the present invention, there is provided a solid-state nmr spectrometer autosampler including: a servo motor 1 is fixed on the bracket (shown in figure 3), the lower end of the servo motor 1 is connected with a shaft 4 of a sample bin rotary disc through a coupler 2 and a shaft-holding regulator 3 and is connected with a sample bin rotary disc 5, a sample bin 6 is provided with a rotary disc positioning point 8 and a reflection type photoelectric sensor 10, the initial positioning of the sample bin can be carried out through the rotary disc positioning point and the reflection type photoelectric sensor 10, the lower end of the sample bin 6 is connected with a sample funnel guide pipe 12, a Y-shaped sample guide pipe side pipe 13 and a Y-shaped sample guide pipe straight pipe 21, the Y-shaped sample guide pipe straight pipe 21 is connected with a nuclear magnetic resonance spectrometer sample guide pipe 22 at the top of a solid nuclear magnetic resonance spectrometer magnet, and the enlarged view of figure 2 is that the connection part of the Y-; two sides of the Y-shaped sample conduit straight pipe 21 are provided with opposite photoelectric sensors 20, the photoelectric sensors and the servo motor are both connected with a control box, and a liquid crystal panel is arranged on the control box and can be used for parameter setting operation, state information display and the like.
The sample bin rotary disc is of a circular structure, and a plurality of sample bins 6 are arranged in the center symmetry manner and are used for containing sample tubes 7; a sample inlet hole 11 of the bottom plate of the sample bin is arranged below the sample bin, and the size of the sample inlet hole is the same as the diameter of the sample bin 6;
the sample funnel conduit 12 is connected with a Y-shaped sample conduit straight pipe 21 through a Y-shaped sample conduit side pipe 13; the upper end and the lower end of the sample conduit straight pipe 21 are both provided with openings, the size of the openings is larger than the diameter of the sample conduit, and the sample conduit straight pipe 21 is positioned in the center of the collection bin;
the collecting bin is a cylindrical cavity and comprises a collecting bin top plate 14, a collecting bin side surface 17, a collecting bin bottom plate 18 and a collecting bin sample outlet 19, wherein a collecting bin buffer cushion 15 is arranged on the collecting bin bottom plate; a side sliding door 16 is arranged on the side surface 17 of the collection bin;
referring to fig. 2, the Y-shaped sample conduit is connected with the sample conduit 22 of the nuclear magnetic resonance spectrometer, and the inner diameters of the joints are the same, so that the inner wall is smooth; an air blowing device is arranged below the sample tube guide tube 22 of the nuclear magnetic resonance spectrometer and is used for ejecting the sample tube 7;
the automatic sample injector bracket respectively clamps two liquid helium inlet and outlet pipes 23 above a nuclear magnetic resonance spectrometer magnet through two liquid helium inlet and outlet pipe clamps 25, a lifting ring fixer 26 and the nuclear magnetic resonance spectrometer magnet lifting ring 24 are locked through bolts, the three points are directly connected through two weight-reducing hole-digging horizontal support rods 27 to form a base of the automatic sample injector bracket, a vertical support pipe 29 is fixed on the base of the bracket through a support rod connector 28, a vertical support pipe clamp 30 tightly holds the vertical support pipe 29 to fix a weight-reducing hole-digging horizontal arm 31, a servo motor 1 in a graph 1 is fixed at the tail end of the weight-reducing hole-digging horizontal arm 31, a display controller of a reflection type photoelectric sensor 10 and an opposite type photoelectric sensor 20 in the graph 1 are fixed on the weight-reducing hole-digging horizontal arm 31, the servo motor 1 is connected with a control host through a power line and a signal line, and a power supply, a single chip microcomputer, The touch screen controls the machine to reset and start to sample through prefabricated software, and checks the running state, reports error information and the like.
The invention controls the sample tube of the automatic sample injector to enter the probe of the nuclear magnetic resonance spectrometer through the program programmed in the control host, and collects the sample tube ejected from the probe of the spectrometer after the test is finished. The detailed process is as follows:
and 2, sequentially putting No. 1-6 sample tubes (7) into a sample bin (6), pressing a 'start' button by a touch screen of a control host, rotating a servo motor (1) by a fixed angle to enable the No. 1 sample bin (6) to be aligned with a sample inlet hole (11) of a sample bin bottom plate, and enabling the No. 1 sample tubes (7) to enter a sample tube guide tube (22) at the top of the nuclear magnetic resonance spectrometer through a sample funnel guide tube (12), a Y-shaped sample guide tube side tube (13) and a Y-shaped sample guide tube straight tube (21). When the sample tube (7) passes through the Y-shaped sample tube straight tube (21), the correlation photoelectric sensor (20) transmits a signal to the host, and the sample tube enters to finish the action;
step 4, after the host computer receives signals of the correlation type photoelectric sensor (20) twice in sequence, the servo motor (1) rotates for a fixed angle, so that the No. 2 sample bin (6) is aligned to the sample bin bottom plate sample inlet hole (12), the No. 2 sample tube (7) enters the nuclear magnetic resonance spectrometer, and the sample tube entering action and the collecting action are repeated;
and 5, when the servo motor (1) rotates for a fixed angle and does not receive a signal of the correlation type photoelectric sensor (20) within a certain time, feeding back 'sample introduction end'.
And 6, when all samples are tested, laterally sliding the collection bin side sliding door (16), taking out all sample tubes (7), closing the collection bin side sliding door (16), and finishing all actions.
Although illustrative embodiments of the present invention have been described above to facilitate the understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but various changes may be apparent to those skilled in the art, and it is intended that all inventive concepts utilizing the inventive concepts set forth herein be protected without departing from the spirit and scope of the present invention as defined and limited by the appended claims.
Claims (10)
1. A solid-state nmr spectrometer autosampler, comprising:
the support, be fixed with servo motor on the support, the servo motor lower extreme passes through the shaft coupling, embraces the axle of shaft regulator connection sample storehouse carousel, and the sample storehouse carousel is reconnected, and the sample storehouse lower extreme even has sample funnel pipe and Y type sample pipe side pipe and Y type sample pipe straight tube, and the storehouse is collected to the sample to the reconnection, the nuclear magnetic resonance spectrometer sample pipe at solid nuclear magnetic resonance spectrometer magnet top is connected to Y type sample pipe straight tube, and Y type sample pipe straight tube both sides are equipped with correlation formula photoelectric sensor, and photoelectric sensor and servo motor all connect the control box, have liquid crystal display panel on the control box can carry out parameter setting operation and status information display.
2. The autosampler of a solid state nmr spectrometer according to claim 1, wherein the sample chamber is provided with a turntable location and a reflective photo sensor, and the initial positioning of the sample chamber is performed by the turntable location and the reflective photo sensor.
3. The autosampler of a solid nmr spectrometer according to claim 1, wherein the holder is adapted to hold two liquid helium inlet and outlet tubes above the nmr spectrometer magnet by two liquid helium inlet and outlet tube clamps, the ring holder is bolted to the ring holder of the nmr spectrometer magnet, the two weight-reducing slotted horizontal support rods are connected to form a base of the autosampler holder, and the vertical support tubes are fixed to the holder base by a support rod connector.
4. The automatic sample injector of the solid nuclear magnetic resonance spectrometer according to claim 3, wherein the vertical support tube clamper tightly holds the vertical support tube and fixes the weight-reduction hole-digging horizontal arm, the servo motor is fixed at the end of the weight-reduction hole-digging horizontal arm, the display controllers of the reflective photoelectric sensor and the correlation photoelectric sensor are fixed on the weight-reduction hole-digging horizontal arm, the servo motor is connected with the control host through a power line and a signal line, and the control box comprises a power supply, a single chip microcomputer and a touch screen.
5. The autosampler of solid nmr spectrometer according to claim 1, wherein the sample compartment carousel has a plurality of holes arranged in a central rotational symmetry for receiving sample tubes.
6. The autosampler of solid nmr spectrometer according to claim 1, wherein the sample compartment carousel is of a circular structure, and a plurality of sample compartments are arranged in a central symmetrical distribution for holding sample tubes; the sample bin is provided with a sample bin bottom plate sample inlet hole below, and the size of the sample bin bottom plate sample inlet hole is the same as the diameter of the sample bin.
7. The autosampler of a solid-state nmr spectrometer according to claim 1, wherein the sample funnel conduit is connected to the Y-sample conduit straight conduit via a Y-sample conduit side conduit; the upper end and the lower end of the sample conduit straight pipe are both provided with openings, the size of each opening is larger than the diameter of the sample conduit, and the sample conduit straight pipe is positioned in the center of the collection bin.
8. The automatic sample injector of the solid nuclear magnetic resonance spectrometer according to claim 1, wherein the collection bin is a cylindrical cavity comprising a collection bin top plate, a collection bin side surface, a collection bin bottom plate and a collection bin sample outlet, and a collection bin buffer pad is arranged on the collection bin bottom plate; the side surface of the collecting bin is provided with a side surface sliding door.
9. The automatic sample injector of the solid nuclear magnetic resonance spectrometer according to claim 1, characterized in that the Y-shaped sample conduit is connected with the sample tube conduit of the nuclear magnetic resonance spectrometer, and the inner diameters of the joints are the same, so as to ensure smooth inner wall; and an air blowing device is arranged below the sample tube guide tube of the nuclear magnetic resonance spectrometer and is used for ejecting the sample tube.
10. An automatic sample introduction method of a solid nuclear magnetic resonance spectrometer is characterized by comprising the following steps:
step 1, a reset button is pressed through a liquid crystal panel of a host, a servo motor rotates, a sample bin rotary disc is driven to rotate through a shaft coupling, a shaft holding regulator and a shaft of the sample bin rotary disc, when a white rotary disc positioning point is opposite to a reflection type photoelectric sensor, light rays emitted by the reflection type photoelectric sensor are reflected back through the white rotary disc positioning point, the host receives a signal of the reflection type photoelectric sensor and rotates a preset angle, so that a sample inlet hole of a bottom plate of the sample bin is aligned with a sample bin No. 0, and the reset action is finished;
step 2, sequentially placing sample tubes No. 1-6 into a sample bin, pressing a 'start' button by a liquid crystal panel of a host computer, rotating a servo motor by a fixed angle to enable the sample bin No. 1 to be aligned with a sample inlet hole of a bottom plate of the sample bin, and enabling the sample tubes No. 1 to enter sample tube guide tubes at the top of a nuclear magnetic resonance spectrometer through a sample funnel guide tube, a Y-shaped sample guide tube side tube and a Y-shaped sample guide tube straight tube; when the sample tube passes through the Y-shaped sample tube straight tube, the correlation photoelectric sensor transmits a signal to the host, and the sample tube enters to finish the action;
step 3, after the nuclear magnetic resonance spectrometer completes the test, the compressed gas pushes the sample tube to enter the collection bin from the nuclear magnetic resonance probe through the sample tube guide tube and the Y-shaped sample guide tube straight tube, the sample tube enters the collection bin from the sample outlet of the collection bin, rebounds for a plurality of times through the cushion pads on the top surface and the bottom surface of the collection bin and falls into the collection bin, when the sample tube passes through the Y-shaped sample guide tube straight tube, the correlation photoelectric sensor transmits the signal to the host again, and the sample tube collection action is completed;
step 4, after the host computer receives the signals of the correlation type photoelectric sensor twice in sequence, the servo motor rotates a fixed angle, so that the No. 2 sample bin aligns to the sample inlet hole of the sample bin bottom plate, the No. 2 sample tube enters the nuclear magnetic resonance spectrometer, and the sample tube entering action and the collecting action are repeated;
step 5, when the servo motor rotates for a fixed angle and does not receive the signal of the correlation type photoelectric sensor within preset time, feeding back 'sample introduction is finished';
and 6, when all samples are tested, laterally sliding the side sliding door of the collection bin, taking out all sample tubes, and closing the side sliding door of the collection bin to finish all actions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010863146.4A CN111856057A (en) | 2020-08-25 | 2020-08-25 | Automatic sample injector of solid nuclear magnetic resonance spectrometer and sample injection method |
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| CN202010863146.4A CN111856057A (en) | 2020-08-25 | 2020-08-25 | Automatic sample injector of solid nuclear magnetic resonance spectrometer and sample injection method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376197A (en) * | 2021-05-10 | 2021-09-10 | 兰立生物科技(苏州)有限公司 | Nuclear magnetic resonance-based kidney cancer detection system and working method thereof |
| CN113970568A (en) * | 2021-10-14 | 2022-01-25 | 厦门大学 | Automatic sample changing device and method for nuclear magnetic resonance spectrometer |
-
2020
- 2020-08-25 CN CN202010863146.4A patent/CN111856057A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376197A (en) * | 2021-05-10 | 2021-09-10 | 兰立生物科技(苏州)有限公司 | Nuclear magnetic resonance-based kidney cancer detection system and working method thereof |
| CN113970568A (en) * | 2021-10-14 | 2022-01-25 | 厦门大学 | Automatic sample changing device and method for nuclear magnetic resonance spectrometer |
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