CN212674949U - Automatic sample injector of solid nuclear magnetic resonance spectrometer - Google Patents

Abstract

The utility model relates to a solid nuclear magnetic resonance spectrometer autosampler, include: 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

Automatic sample injector of solid nuclear magnetic resonance spectrometer

Technical Field

The utility model 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.

SUMMERY OF THE UTILITY MODEL

The utility model discloses a problem that solve is: 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 utility model is that:

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.

Has the advantages that:

the utility model discloses a servo motor control device disk sample storehouse can the rotatory angle in accurate control sample storehouse, guarantees that the sample cell that awaits measuring can follow the sample storehouse and slide the rotor pipe at solid nuclear magnetic resonance spectrometer magnet top in Y type sample pipe side tube, finally gets into the nuclear magnetic resonance probe, and the sample cell that the test was accomplished is promoted by compressed gas from the nuclear magnetic probe and is got into through rotor pipe and Y type sample pipe straight tube and collect the storehouse. 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 structure schematic diagram of the automatic sample injector of the utility model;

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 solution 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 some embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any inventive work belong to the protection scope of the present invention based on the embodiments of the present invention.

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 utility model discloses a program of establishment in the control host computer controls the sample cell of this auto-sampler and gets into the probe of nuclear magnetic resonance spectrometer to collect the sample cell that pops out from the spectrometer probe after the test is accomplished. The detailed process is as follows:

step 1, a reset button is pressed through a touch screen of a control host, a servo motor (1) rotates, a sample bin rotary disc (5) is driven to rotate through a coupler (2), a shaft holding regulator (3) and a shaft (4) of the sample bin rotary disc, when a white rotary disc positioning point (8) is opposite to a reflection type photoelectric sensor (10), light rays emitted by the reflection type photoelectric sensor (10) are reflected back through the white rotary disc positioning point (8), the host receives a signal of the reflection type photoelectric sensor (10) and rotates for a preset angle, a sample inlet hole (11) of a sample bin bottom plate is aligned to a sample bin No. 0 (6), and reset action is completed;

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 3, after the nuclear magnetic resonance spectrometer completes the test, the compressed gas pushes the sample tube (7) to enter the collection bin from the nuclear magnetic resonance probe through the sample tube guide tube (22) and the Y-shaped sample guide tube straight tube (21) and from the sample outlet (19) of the collection bin, the sample tube rebounds for a plurality of times through the buffer pads (15) on the top surface and the bottom surface of the collection bin and falls into the collection bin, when the sample tube (7) passes through the Y-shaped sample guide tube straight tube (21), the correlation type photoelectric sensor (20) transmits the signal to the host again, and the sample tube collection action is completed;

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 invention have been described above to facilitate the understanding of the invention by those skilled in the art, it should be understood that the invention is not limited to the scope of the embodiments, and that various changes will become apparent to those skilled in the art once they are within the spirit and scope of the invention as defined and defined in the appended claims.

Claims (9)

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, characterized in that the vertical support tube clamper tightly holds the vertical support tube and fixes the weight-reducing hole-digging horizontal arm, the servo motor is fixed at the end of the weight-reducing hole-digging horizontal arm, the display controllers of the reflective photoelectric sensor and the correlation photoelectric sensor are fixed on the weight-reducing 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 singlechip 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.

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