A nuclear magnetic sample loading system and method

Abstract

The application discloses a nuclear magnetic sample loading system and a sample loading method. The nuclear magnetic sample loading system comprises a rack and a material storage area, an oscillation and shaking assembly, a bottle clamping assembly, a nuclear magnetic tube assembly component, a horizontal moving assembly, a top three-axis sample loading assembly and a control system arranged on the rack. The horizontal moving assembly is loaded with a multifunctional manipulator integrating a rotating cap, pipetting and nuclear magnetic tube carrying functions. Through coordination of the control system, the equipment can automatically perform sample bottle uncapping, solvent filling, eccentric oscillation mixing, filtering and transferring, nuclear magnetic tube packaging and rotor insertion, and finally send into a spectrometer inlet by the top assembly. Through high function integration and closed-loop monitoring mechanism, the application solves the problems of low efficiency, poor consistency and safety hidden danger caused by volatile solvents in manual operation, realizes full-process automation from sample pretreatment to nuclear magnetic sample loading, and significantly improves the reliability and standardization level of high-throughput detection.

Description

Technical Field

[0001] This invention belongs to the field of nuclear magnetic resonance detection technology, and specifically relates to a nuclear magnetic resonance sample loading system and sample loading method. Background Technology

[0002] Nuclear magnetic resonance spectroscopy (NMR) is a core technology in analytical chemistry, widely used for the structural identification and quantitative analysis of organic compounds, biomolecules, and other substances. Sample preparation is a crucial step affecting the accuracy and reproducibility of NMR results, typically involving steps such as sample dissolution, vortexing, liquid transfer, filtration and purification, NMR tube loading, and rotor assembly. Currently, most laboratories still rely on manual operation to complete these procedures, resulting in the following prominent problems: Low efficiency: Manual sample processing is time-consuming, making it difficult to meet the demands of high-throughput detection, especially in large-scale screening or continuous experiments, where it becomes a bottleneck; Poor consistency: Manual operation easily introduces individual differences, such as the difficulty in standardizing parameters like mixing intensity, pipetting volume, and NMR tube sealing force, leading to data fluctuations; Risk of cross-contamination: Frequent contact with consumables such as sample vials and NMR tubes may introduce impurities, affecting detection sensitivity; Safety challenges: Some solvents are volatile or toxic, and direct exposure poses a potential threat to the health of operators. To improve automation, some semi-automatic equipment has emerged in existing technologies, such as independently operated pipetting workstations or shakers, but their functions are relatively limited, failing to achieve full integration from sample pretreatment to sample loading.

[0003] Therefore, there is an urgent need to develop a highly integrated, intelligent, and coordinated fully automated NMR sample loading system to solve the balance problem between efficiency, accuracy, and safety in existing technologies. Summary of the Invention

[0004] This invention provides an NMR sample loading system and method, aiming to solve the problems pointed out in the background art.

[0005] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: An NMR sample loading system, comprising: frame; The material storage area, oscillation and shaking assembly, several sets of bottle clamping assemblies, nuclear magnetic tube assembly assembly, horizontal movement assembly, top three-axis sample loading assembly, imaging sensor and control system are set on the frame. The horizontal moving component is equipped with a multi-functional robotic arm, which includes a capping component, a pipetting component, and a nuclear magnetic resonance tube handling component. The capping assembly includes a first vertical feeding module and a rotating electric gripper. The capping assembly cooperates with the bottle clamping assembly to open or close sample bottles, transfer bottles or solvent bottles. A mounting plate is fixedly connected to the moving end of the first vertical feed module. A horizontally set limiting plate is fixedly connected to the upper end of the mounting plate. The rotating electric claw is vertically slidably connected to the mounting plate, and a number of buffer springs are provided between the upper end of the rotating electric claw and the limiting plate. A displacement sensor is provided on the limiting plate, and a trigger plate that cooperates with the displacement sensor is provided on the upper part of the rotating electric gripper. The control system is configured to dynamically control the rotation of the rotating electric gripper and the lifting of the first vertical feed module based on the displacement signal of the trigger plate monitored by the displacement sensor, so as to achieve abnormal error correction and locking during the closing operation.

[0006] Furthermore, the control system controls the capping assembly to perform the following steps during the capping operation: Step 1: The first vertical feed module drives the rotating electric claw holding the bottle cap to descend to contact the bottle mouth and maintain a preset initial downward pressure, causing the buffer spring to contract and the trigger plate to move upward a preset distance S1; Step 2: Control the rotating electric gripper to rotate in the opposite direction and monitor the displacement change signal of the trigger plate in the vertical direction in real time; when the change signal is detected, determine that the bottle cap is aligned with the starting point of the bottle mouth thread and stop the reverse rotation; Step 3: Control the rotating electric gripper to rotate in the forward direction with a preset preload torque, while the first vertical feed module moves downward synchronously, and acquires the movement signal S of the trigger plate in real time; Step 4: If the downward depth value does not reach the preset target depth threshold, the movement signal S exceeds the preset range, and it is determined that the thread misalignment and jamming has occurred. Then, the rotary electric gripper is controlled to rotate in the opposite direction for a preset number of turns and the first vertical feed module rises synchronously. Then, the rotary electric gripper is controlled to place the bottle cap on the horizontal surface and grab it again, and returns to Step 1 until the movement signal is within the preset range or the maximum number of retries is reached during the screwing process. If all the movement signals during the screwing-in process are within the preset range, then proceed to step five; If the maximum number of retries is reached, an exception alarm will be triggered. Step 5: Increase the positive output torque of the rotating electric gripper to the rated sealing torque, and complete the cover closing operation after reaching the rated sealing torque.

[0007] Furthermore, the oscillation and mixing component is used to eccentrically oscillate and mix the bottle. The bottle clamping assembly is used to clamp the bottle and monitor whether the bottle cap has been removed; The NMR tube assembly is used in conjunction with the multifunctional robotic arm to open or close the NMR tube, insert the NMR tube containing the test liquid and solvent into the rotor before testing, and remove the NMR tube from the rotor after testing. The horizontal movement component is used to drive the multi-functional robot to move in the plane above the material storage area, the oscillation and shaking component, the bottle clamping component, and the nuclear magnetic tube assembly component. The top triaxial sample loading assembly is used to deliver the assembled NMR tube and rotor assembly into the sample loading position of the NMR spectrometer and to perform sample unloading and recovery after the detection is completed; The control system is configured to coordinate the horizontal movement component, multi-functional robotic arm, oscillation and shaking component, bottle clamping component, NMR tube assembly component and top three-axis sample loading component to complete automatic sample loading according to a preset process.

[0008] Furthermore, the material storage area includes: NMR tube rack, sample vial rack, transfer vial rack, filter head rack, and liquid retrieval head rack; each of the NMR tube rack, sample vial rack, transfer vial rack, filter head rack, and liquid retrieval head rack is divided into a feeding area and a recycling area; the feeding area is used to provide consumables to be used, and the recycling area is used to recycle consumables after use.

[0009] Furthermore, the pipetting assembly includes a second vertical feed module and a pipette, used for adding, retrieving, and transferring liquid between sample vials, transfer vials, and NMR tubes; The NMR tube handling assembly includes a third vertical feed module and an electric gripper, used to pick up and place NMR tubes from the NMR tube rack and deliver the NMR tubes to the NMR tube assembly assembly, and to remove used NMR tubes from the NMR tube assembly assembly and deliver them to the recycling area. The first vertical feed module, the second vertical feed module, and the third vertical feed module are fixedly connected to one side of the mounting back plate. The mounting back plate is fixedly connected to the moving end of the horizontal moving component. The first vertical feed module, the second vertical feed module, and the third vertical feed module respectively drive the capping assembly, the pipetting assembly, and the NMR tube transport assembly to move independently in the vertical direction.

[0010] Furthermore, the lower part of the rotating electric claw is provided with a capping working head, including a turntable and telescopic rods symmetrically arranged on both sides of the turntable. The ends of the telescopic rods are respectively fixedly connected to a pair of spaced capping contacts through extension plates.

[0011] Furthermore, the bottle clamping assembly includes: a second support base plate, a bottle cap placement plate, a bottle pneumatic gripper, and a bottle cap in-position sensor; The second support base plate is fixedly connected to the frame. The bottle cap placement plate and the bottle body pneumatic gripper are respectively arranged on both sides of the second support base plate, and the bottle cap placement plate is located above the bottle body pneumatic gripper. The bottle cap placement plate has a bottle body clearance hole and a bottle cap placement slot. The gripping position of the bottle body pneumatic gripper is located below the bottle body clearance hole. The bottle cap in-place sensor is located at the bottom of the bottle cap placement slot to monitor whether the bottle cap is accurately placed after opening or removed before closing.

[0012] Furthermore, the nuclear magnetic tube assembly includes: a rotor servo motor, a rotary indexing plate, a mounting bracket, guide grippers, a telescopic cylinder, and fixed pneumatic grippers; The rotor servo motor is fixedly connected to the frame, and its output end is fixedly connected to the rotating indexing plate coaxially. The rotating indexing plate has multiple rotor placement slots around its circumference. The mounting bracket is fixedly connected to the frame and is located on one side of the rotor servo motor. The guide gripper, telescopic cylinder, and fixed pneumatic gripper are all fixed on the mounting bracket. The guide gripper is used to provide end guidance during the insertion of the nuclear magnetic tube into the rotor. The moving end of the telescopic cylinder is fixedly connected to a slot plate. The telescopic cylinder cooperates with the slot plate to fix the rotor during the removal of the nuclear magnetic tube from the rotor. The fixed pneumatic gripper works in conjunction with the NMR tube handling assembly to open and close the NMR tube. A rotor presence sensor and a nuclear magnetic tube presence sensor are provided on one side of the rotating indexing disk, and a nuclear magnetic tube positioning sensor is provided at the bottom of the rotating indexing disk to detect whether the insertion depth of the nuclear magnetic tube and the rotor meets the standard.

[0013] Furthermore, the top three-axis sample loading assembly includes: a second longitudinal feed module, a second transverse feed module, and a fourth vertical feed module, wherein a sample loading pneumatic gripper is fixedly connected to the moving end of the fourth vertical feed module. The second longitudinal feed module and the second transverse feed module are mounted on the top edge of the frame and their travel covers the NMR tube assembly and the external NMR spectrometer inlet.

[0014] Furthermore, this application also provides a sample loading method using an NMR sample loading system, employing the NMR sample loading system described above, comprising the following steps: S1: In the material storage area, complete the preparation for the installation of NMR tubes, sample vials, transfer bottles, solvent bottles, filter heads, and liquid dispensing heads. S2: The capping assembly of the multi-functional robotic arm opens the sample bottle and solvent bottle; the pipetting assembly draws a preset volume of solvent from the solvent bottle and adds it to the sample bottle before tightening the sample bottle cap; S3: Place the sample vial in the shaking assembly and perform eccentric shaking to mix; S4: Use an imaging sensor to determine the dissolved impurities in the mixed sample; if it is determined that the impurities are not dissolved, return to step S3 to continue mixing; if it is determined that there are impurities, proceed to step S5 for filtration and transfer; if it is determined that there are no impurities and the impurities have been dissolved, proceed to step S6. S5: The pipetting assembly filters the sample solution through the filter head into the transfer bottle; S6: The NMR tube handling assembly takes the NMR tube from the NMR tube rack to the NMR tube assembly assembly and opens the cap; the pipetting assembly transfers the sample solution to the NMR tube and closes the cap. S7: The NMR tube handling assembly inserts the NMR tube into the rotor of the NMR tube assembly assembly; S8: The top three-axis sample loading assembly sends the assembled NMR tube rotor assembly into the NMR spectrometer to complete the sample loading; after the test is completed, the sample is unloaded and returned to the recycling station.

[0015] Compared with the prior art, the present invention has the following technical effects: 1. This invention integrates all steps, including sample opening, solvent addition, oscillation mixing, liquid transfer, filtration, NMR tube opening and closing, rotor insertion and removal, and instrument sample loading and unloading, into a single device through the coordinated operation of a horizontal moving component, a multi-functional robotic arm, a top three-axis sample loading component, and a control system. This greatly reduces manual intervention, avoids result fluctuations caused by operator differences, and is particularly suitable for high-throughput detection scenarios, ensuring data reliability and reproducibility.

[0016] 2. The multifunctional robotic arm in this invention integrates three major functional modules—capping, pipetting, and NMR tube handling—onto a single mounting backplate, and is driven by a horizontal movement component to move within a plane. Each functional module is driven by an independent vertical feed module, allowing for independent or sequential operation. This design avoids the complexity of configuring a separate robotic arm for each function, resulting in a compact structure, reduced cost and equipment size, while ensuring that all operations can be completed smoothly and continuously within a single work cycle.

[0017] 3. Before the capping assembly of this invention is tightened in the forward direction, an initial downward pressure is applied and the electric gripper is controlled to reverse. The vertical displacement change signal generated by the trigger plate when the thread start point crosses the pitch gap is used to accurately locate the thread alignment point. This biomimetic tooth-finding action fundamentally eliminates hard thread misalignment and stripping phenomena in high-throughput operations. Combined with real-time linkage comparison of descent depth and movement signals, the system can autonomously determine that thread misalignment has occurred when the target depth has not been reached and the sensor signal is abnormal. At this time, the system does not directly crash and stop, but initiates a closed-loop error correction mechanism of reversing the rotation, synchronously rising, placing the gripper again, and realigning. This effectively solves the pain point of frequent manual reset caused by occasional jamming in automated equipment, and greatly improves the throughput and trouble-free operation time of the equipment.

[0018] 4. The NMR tube assembly component in this invention achieves multi-station operation through a rotating indexing plate. Combined with guide grippers, telescopic cylinders, fixed pneumatic grippers, and various sensors, it enables automatic opening and closing of the NMR tube cap and precise alignment and depth control during the insertion and removal of the NMR tube and rotor. This solves the core pain points of easy damage to the NMR tube and inconsistent insertion depth affecting spectrum quality in manual operation, ensuring standardization and success rate in the sample loading process, and reducing data fluctuations caused by manual operation. Attached Figure Description

[0019] Figure 1 This is an overall isometric view of an NMR sample loading system described in this invention; Figure 2 This is an isometric view of an NMR sample loading system without an outer cover, as described in this invention. Figure 3 This is a schematic diagram of the overall multifunctional robotic arm of the nuclear magnetic resonance sample loading system described in this invention; Figure 4 This is a schematic diagram of the capping assembly of an NMR sample loading system according to the present invention; Figure 5 This is a schematic diagram of the pipetting assembly and the nuclear magnetic resonance tube transport assembly of an NMR sample loading system according to the present invention; Figure 6 This is a schematic diagram of a bottle clamping assembly of an NMR sample loading system according to the present invention; Figure 7 This is an exploded schematic diagram of the bottle clamping assembly of an NMR sample loading system according to the present invention; Figure 8 This is a schematic diagram of the overall oscillation and mixing component of an NMR sample loading system according to the present invention; Figure 9 This is an isometric view of the nuclear magnetic resonance tube assembly of a nuclear magnetic resonance sample loading system according to the present invention; Figure 10 This is a side view of the nuclear magnetic resonance tube assembly of a nuclear magnetic resonance sample loading system according to the present invention; Figure 11 This is an isometric view of the top three-axis sample loading assembly of an NMR sample loading system according to the present invention.

[0020] In the picture: 1. Rack; 2. Material storage area; 201. NMR tube rack; 202. Sample vial rack; 203. Transfer vial rack; 204. Filter head rack; 205. Liquid dispensing head rack; 3. Oscillating and shaking component; 4. Bottle clamping assembly; 401. Second support base plate; 402. Bottle cap placement plate; 4021. Bottle body clearance hole; 4022. Bottle cap placement slot; 403. Bottle body pneumatic gripper; 404. Bottle cap in-position sensor; 5. Nuclear magnetic tube assembly assembly; 501. Rotor servo motor; 502. Rotary indexing plate; 503. Rotor placement slot; 504. Mounting bracket; 505. Guide gripper; 506. Telescopic cylinder; 5061. Slot plate; 507. Rotor in-place sensor; 508. Nuclear magnetic tube in-place sensor; 509. Fixed pneumatic gripper; 510. Protective tube; 511. Nuclear magnetic tube positioning sensor; 6. Horizontal movement component; 601. First longitudinal feed module; 602. First transverse feed module; 7. Multifunctional robotic arm; 701. Mounting backplate; 702. Capping assembly; 7021. First vertical feed module; 7022. Mounting plate; 7023. Rotary electric gripper; 7024. Limiting plate; 7025. Buffer spring; 7026. Displacement sensor; 7027. Trigger plate; 7028, Capping head; 70281, Turntable; 70282, Telescopic rod; 70283, Extension plate; 70284, Capping contact; 703. Pipetting assembly; 7031. Second vertical feed module; 7032. Pipette; 704. Nuclear magnetic tube handling assembly; 7041. Third vertical feed module; 7042. Electric gripper; 8. Top three-axis sample loading assembly; 801. Second longitudinal feed module; 802. Second transverse feed module; 803. Fourth vertical feed module; 804. Sample loading pneumatic gripper. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with specific embodiments of the present application and with reference to the accompanying drawings.

[0022] like Figure 1-5 As shown, an NMR sample loading system includes: Rack 1; The following components are set on the frame 1: material storage area 2, oscillation and shaking assembly 3, several sets of bottle clamping assemblies 4, nuclear magnetic tube assembly 5, horizontal movement assembly 6, top three-axis sample loading assembly 8, and imaging sensor and control system. The horizontal moving component 6 is equipped with a multi-functional robotic arm 7, which includes a capping component 702, a pipetting component 703, and a nuclear magnetic resonance tube handling component 704. The capping assembly 702 includes a first vertical feeding module 7021 and a rotating electric gripper 7023. The capping assembly 702 cooperates with the bottle body clamping assembly 4 to open or close sample bottles, transfer bottles or solvent bottles. A mounting plate 7022 is fixedly connected to the moving end of the first vertical feed module 7021. A horizontally set limiting plate 7024 is fixedly connected to the upper end of the mounting plate 7022. The rotating electric gripper 7023 is vertically slidably connected to the mounting plate 7022. A plurality of buffer springs 7025 are provided between the upper end of the rotating electric gripper 7023 and the limiting plate 7024. The limiting plate 7024 is provided with a displacement sensor 7026, and the upper part of the rotating electric claw 7023 is provided with a trigger plate 7027 that cooperates with the displacement sensor 7026. The control system is configured to dynamically control the rotation of the rotating electric gripper 7023 and the lifting of the first vertical feed module 7021 based on the displacement signal of the trigger plate 7027 monitored by the displacement sensor 7026, so as to achieve abnormal error correction and locking during the closing operation.

[0023] In one specific embodiment, the control system controls the capping assembly 702 to perform the following steps during the capping operation: Step 1: The first vertical feed module 7021 drives the rotating electric claw 7023 holding the bottle cap to descend to contact the bottle mouth and maintain a preset initial downward pressure, causing the buffer spring 7025 to contract and the trigger plate 7027 to move upward a preset distance S1. Step 2: Control the rotating electric gripper 7023 to rotate in the opposite direction, and monitor the vertical displacement change signal of the trigger plate 7027 in real time; when the change signal is detected, determine that the bottle cap is aligned with the starting point of the bottle mouth thread, and stop the reverse rotation; Step 3: Control the rotating electric gripper 7023 to rotate in the forward direction with a preset preload torque, while the first vertical feed module 7021 moves downward synchronously, and the movement signal S of the trigger plate 7027 is acquired in real time; Step 4: If the downward depth value does not reach the preset target depth threshold, the movement signal S exceeds the preset range, and it is determined that a thread misalignment jam has occurred. Then, the rotary electric gripper 7023 is controlled to rotate in the opposite direction for a preset number of turns, and the first vertical feed module 7021 rises synchronously. Then, the rotary electric gripper 7023 is controlled to place the bottle cap on the horizontal surface and grab it again, and return to Step 1 until the movement signal is within the preset range or the maximum number of retries is reached during the screwing process. If all the movement signals during the screwing-in process are within the preset range, then proceed to step five; If the maximum number of retries is reached, an exception alarm will be triggered. Step 5: Increase the positive output torque of the rotary electric gripper 7023 to the rated sealing torque, and complete the cover closing operation after reaching the rated sealing torque.

[0024] Traditional automated capping often uses unidirectional force tightening, which easily damages the threads. The capping assembly 702 of this application applies an initial downward pressure and controls the electric gripper to reverse direction before the actual forward tightening. It uses the sudden vertical displacement signal generated by the trigger plate when the thread start point crosses the pitch gap to precisely locate the thread alignment point. This biomimetic thread-finding action fundamentally eliminates misalignment and stripping in high-throughput operations.

[0025] By combining real-time comparison of downlink depth and motion signals, the system can autonomously determine that thread misalignment has occurred when the target depth has not been reached and the sensor signal is abnormal. Instead of immediately crashing and shutting down, the system initiates a closed-loop error correction mechanism involving reversing the thread, synchronous ascent, repositioning, and realigning. This effectively solves the pain point of frequent manual resets required by occasional jamming in automated equipment, significantly improving the throughput and trouble-free operating time of the equipment during continuous operation.

[0026] In one specific embodiment, in order to ensure that the bottle cap has sufficient adhesion to fall into the starting point of the thread during the subsequent "reverse tooth finding" without causing thread wear due to excessive pressure, the initial contraction amount of the buffer spring 7025, i.e. the preset distance S1 of the trigger plate moving upward, is set to a value related to the pitch P.

[0027] Preferred setting: S1 = 1.0P - 1.5P.

[0028] This spring compression energy storage design provides a gentle axial thrust. During the reverse rotation in step two, when the bottle mouth aligns with the starting point of the cap's thread, the cap will instantly fall into the thread groove under the spring force, resulting in a small downward displacement Δd, typically 0.2P-0.5P. The displacement sensor 7026 captures this abrupt displacement difference; S changes abruptly from S1 to S1-Δd, thus accurately determining that the threads are aligned.

[0029] In the forward screwing stage of step three, to prevent stripping caused by forceful screwing, the control system adopts an equidistant follow-up control method. That is, the downward linear movement speed v of the first vertical feed module 7021, the rotational speed n of the rotating electric gripper 7023, and the cap pitch P have the following relationship: v = n × P; For every one revolution of the rotary gripper 7023 in the forward direction, the first vertical feed module 7021 descends by a pitch P. This constant pitch descent ensures that the axial force exerted on the cap by the vertical module during screwing is close to zero, allowing it to screw in completely following the natural guidance of the thread. The movement signal S of the trigger plate 7027 remains essentially unchanged during the capping process.

[0030] During an ideal and smooth screwing process, the speed at which the bottle cap descends is exactly the same as the speed at which the first vertical feed module 7021 descends, so the deformation of the buffer spring 7025 should remain constant.

[0031] At this time, the reference movement signal of the trigger board 7027 remains in the aligned state, that is, S0=S1-Δd; The default safety range is set to: [S0-0.2P, S0+0.2P]; If S > S0 + 0.2P is detected when the descent depth is below the target, it physically means that the first vertical feed module 7021 is descending at the predetermined speed, but the bottle cap fails to screw into the bottle mouth due to a misaligned screw thread, causing the buffer spring 7025 to be further abnormally compressed. The control system detects this out-of-tolerance signal, confirms the misaligned screw thread jamming, and immediately triggers the reverse uncoiling and retry mechanism in step four. This determination based on relative pitch displacement is more sensitive than relying solely on a torque sensor, allowing for intervention and protection in the early stages of jamming.

[0032] like Figure 1-3 As shown, the oscillating and mixing component 3 is used to eccentrically oscillate and mix the bottle. The bottle clamping assembly 4 is used to clamp the bottle and monitor whether the bottle cap has been removed; The NMR tube assembly 5 is used in conjunction with the multifunctional robotic arm 7 to open or close the NMR tube, insert the NMR tube containing the test liquid and solvent into the rotor before testing, and remove the NMR tube from the rotor after testing. The horizontal movement component 6 is used to drive the multi-functional robotic arm 7 to move in the plane above the material storage area 2, the oscillation and shaking component 3, the bottle clamping component 4, and the nuclear magnetic tube assembly component 5; for example Figure 2As shown, the horizontal moving component 6 includes a first longitudinal feeding module 601 and a first transverse feeding module 602. The first transverse feeding module 602 is disposed on the moving end of the first longitudinal feeding module 601, and the multi-functional robot 7 is disposed on the moving end of the first transverse feeding module 602. The first longitudinal feeding module 601 and the first transverse feeding module 602 cooperate to drive the multi-functional robot 7 to move in the horizontal direction. The top triaxial sample loading assembly 8 is used to send the assembled NMR tube and rotor assembly into the sample loading position of the NMR spectrometer and to perform sample unloading and recovery after the detection is completed; The control system is configured to coordinate the horizontal movement component 6, the multi-functional robotic arm 7, the oscillation and mixing component 3, the bottle clamping component 4, the NMR tube assembly component 5, and the top triaxial sample loading component 8 to automatically load samples according to a preset process. This device integrates all steps such as sample opening, solvent addition, oscillation and mixing, liquid transfer, filtration, NMR tube opening and closing, rotor insertion and removal, and instrument sample loading and unloading into one device. This greatly reduces manual intervention, avoids result fluctuations caused by operator differences, and is particularly suitable for high-throughput detection scenarios, ensuring data reliability and reproducibility.

[0033] like Figure 2 As shown, the material storage area 2 includes: NMR tube rack 201, sample bottle rack 202, transfer bottle rack 203, filter head rack 204, and liquid collection head rack 205; the NMR tube rack 201, sample bottle rack 202, transfer bottle rack 203, filter head rack 204, and liquid collection head rack 205 are all divided into a feeding area and a recycling area; the feeding area is used to provide consumables to be used, and the recycling area is used to recycle consumables after use.

[0034] In this embodiment, as Figure 2 As shown, the material storage area 2 is used for the centralized arrangement and orderly management of consumables required for the entire sample loading process. It includes NMR tube rack 201, sample bottle rack 202, transfer bottle rack 203, filter head rack 204, and liquid collection head rack 205. Each of the above racks is divided into a supply area and a recycling area. The supply area is used to place consumables to be used, and the recycling area is used to collect consumables after use, reducing the risk of mis-collection and cross-contamination caused by mixed storage of consumables.

[0035] like Figure 3-5 As shown, the pipetting assembly 703 includes a second vertical feed module 7031 and a pipette 7032, used for adding, taking and transferring liquids between sample vials, transfer vials and NMR tubes; In one specific embodiment, to adapt to automated operation, the pipette 7032 preferably adopts a disposable dispensing tip solution commonly used in the art, which cooperates with the dispensing tip holder 205 to achieve automatic loading and unloading. Specifically, the lower end of the pipette 7032 is provided with a standardized nozzle, such as a conical insertion interface or an equivalent standard interface, and the upper end of the disposable dispensing tip forms a matching conical hole or sleeve section. During tip installation, a sealed connection is formed by axial compression. This structure is a mature and universal structure in the field of pipetting workstations, facilitating reliable sealing and quick replacement.

[0036] When the dispensing head needs to be used, the horizontal moving component 6 moves the pipetting assembly 703 above the feeding area of ​​the dispensing head holder 205. The second vertical feeding module 7031 drives the pipette 7032 to move downwards vertically, aligning the nozzle with the axis of the dispensing head and inserting it into the upper conical hole of the dispensing head. It then continues to press down until the preset pressing stroke is reached, thus completing the dispensing head assembly. To achieve post-use recycling, the pipette 7032 can be equipped with a common type of sleeve or ejector ring in the art: it can slide axially on the outside of the pipette 7032, with the lower end of the sleeve aligned with the upper flange or step of the dispensing head. During dispensing, the sleeve moves downwards driven by a small push rod such as an electric push rod, cylinder, or cam mechanism, pressing against the flange of the dispensing head, pushing the dispensing head off the conical surface of the nozzle, and the dispensing head falls into the recycling area of ​​the dispensing head holder 205, thereby achieving consumable recycling.

[0037] When a filter head needs to be installed at the lower end of the liquid dispensing head for filtering sample liquid, the filter head may include a filter housing, a filter membrane, and upstream and downstream interfaces: the upstream interface is a plug-in interface that matches the end of the liquid dispensing head, such as a conical plug-in interface; the downstream outlet is a drop outlet, which facilitates controlled dripping by aligning with the mouth of the transfer bottle or inserting into the mouth area of ​​the transfer bottle. The above interface type is a mature and common connection method in this field, which can ensure sealing and repeatable positioning without adding complex mechanisms.

[0038] Filter head installation steps: First, the pipette 7032 is taken from the dispensing head holder 205 and a disposable dispensing head is assembled as described above; The horizontal moving component 6 moves the liquid transfer component 703 to above the feeding area of ​​the filter head frame 204; the second vertical feeding module 7031 moves down so that the end of the assembled liquid taking head is aligned with the upstream interface of the filter head. Continue pressing down to complete the insertion, so that the filter head and the liquid dispensing head form a connected and sealed filtration channel. Assembly consistency can be ensured by controlling the insertion stroke.

[0039] After filtration is completed, the filter head is given priority for direct recycling as a disposable consumable: the pipetting assembly 703 moves to the filter head holder 204 recycling area, and the filter head is removed and put into the recycling area by lifting it off or pushing the filter head shoulder with the sleeve; subsequently, the liquid collection head can also be disposed of in the liquid collection head holder 205 recycling area as needed.

[0040] The NMR tube handling assembly 704 includes a third vertical feeding module 7041 and an electric gripper 7042, which are used to pick up and place NMR tubes from the NMR tube rack 201 and deliver the NMR tubes to the NMR tube assembly assembly 5, and to remove used NMR tubes from the NMR tube assembly assembly 5 and deliver them to the recycling area. The first vertical feed module 7021, the second vertical feed module 7031, and the third vertical feed module 7041 are fixedly connected to one side of the mounting back plate 701. The mounting back plate 701 is fixedly connected to the moving end of the horizontal moving component 6. The first vertical feed module 7021, the second vertical feed module 7031, and the third vertical feed module 7041 respectively drive the capping component 702, the pipetting component 703, and the NMR tube transport component 704 to move independently in the vertical direction.

[0041] The multi-functional robotic arm 7 integrates three major functional modules—capping, pipetting, and NMR tube handling—on a single mounting backplate 701, and is driven by the horizontal moving component 6 to move within a plane. Each functional module is driven by an independent vertical feed module, allowing for independent or sequential operation. This design avoids the complexity of configuring a separate robotic arm for each function, resulting in a compact structure, reduced cost and equipment size, while ensuring that all operations can be completed smoothly and continuously within a single work cycle.

[0042] like Figure 4 As shown, the lower part of the rotating electric gripper 7023 is provided with a capping working head 7028, which includes a turntable 70281 and telescopic rods 70282 symmetrically arranged on both sides of the turntable 70281. The ends of the telescopic rods 70282 are respectively fixedly connected to a pair of spaced capping contacts 70284 through extension plates 70283.

[0043] Specifically, the turntable 70281 is connected to the output end of the rotating electric gripper 7023 and rotates synchronously with it, thereby transmitting the torque of the rotating electric gripper 7023 to the capping contact 70284; the telescopic rods 70282 on both sides are arranged symmetrically to provide radial extension stroke for the capping contact 70284, so that the contact can automatically fit and form a clamping force when it contacts the outer periphery of the bottle cap, avoiding unilateral force and slippage caused by the diameter tolerance or positioning deviation of the bottle cap, and making the capping working head 7028 suitable for bottle caps of different diameters.

[0044] In the specific working process, the first vertical feed module 7021 drives the rotating electric gripper 7023 to move the capping head 7028 downward in the vertical direction. When the capping head 7028 descends to the preset height position corresponding to the bottle cap, the two telescopic rods 70282 on both sides retract radially inward, so that the four capping contacts 70284 simultaneously move towards the outer periphery of the bottle cap and clamp around the bottle cap, thereby completing the centering and stable clamping of the bottle cap. Subsequently, the turntable 70281 rotates under the drive of the rotating electric gripper 7023, and transmits torque to the bottle cap through the four capping contacts 70284 to realize the opening or closing operation of the bottle cap.

[0045] like Figure 8 As shown, the oscillation and shaking component 3 is used to eccentrically oscillate and mix the bottle. Mature oscillation and shaking equipment on the market can be selected according to actual needs. In one specific embodiment, the oscillation and shaking assembly 3 includes: a first support base plate, an oscillation motor, and an oscillation tray; The first support base plate is fixedly connected to the frame 1, the oscillating motor is fixedly connected to the lower part of the first support base plate, and the output end passes through the first support base plate and is fixedly connected to an eccentric transmission shaft. The upper surface of the oscillation tray is provided with multiple bottle placement holes, the side wall is connected to the first support base plate by a return spring, and a transmission rod is provided at the bottom. An eccentric drive shaft has an eccentric circular hole in the middle, and a drive rod is inserted into the eccentric circular hole. When the eccentric drive shaft rotates, it drives the drive rod through the eccentric circular hole, and the drive rod drives the oscillating tray to oscillate. A protective housing is provided on the outside of the oscillating tray, and the protective housing is fixedly connected to the frame 1.

[0046] Specifically, the first support base plate is fixedly connected to the frame 1, serving as the mounting base for the oscillation mechanism. The oscillation motor is fixedly mounted on the lower part of the first support base plate, with its output end passing through the first support base plate and fixedly connected to the eccentric transmission shaft, thereby transmitting the motor's rotational motion to the eccentric transmission mechanism. The oscillation tray is used to support the bottles to be mixed, and its upper surface is provided with multiple bottle placement holes for limiting and positioning sample bottles and transfer bottles. The side wall of the oscillation tray is connected to the first support base plate through a return spring, enabling the oscillation tray to automatically return to center after being excited by oscillation and suppressing abnormal amplitude diffusion. At the same time, a transmission rod is provided at the lower part of the oscillation tray to cooperate with the eccentric structure of the eccentric transmission shaft to achieve oscillation drive.

[0047] An eccentric drive shaft has an eccentric circular hole in its center, into which a transmission rod is inserted. When the eccentric drive shaft rotates with the oscillating motor, the eccentric circular hole undergoes periodic eccentric motion relative to the center of the shaft, thereby driving the transmission rod to oscillate back and forth. The transmission rod then drives the oscillating tray to generate eccentric oscillation, achieving uniform mixing of the bottles. To improve operational safety and isolate the oscillation area, a protective shell is installed on the outside of the oscillating tray. The protective shell is fixedly connected to the frame 1 and serves to cover and protect the oscillating tray and transmission components.

[0048] like Figure 6-7 As shown, the bottle clamping assembly 4 includes: a second support base plate 401, a bottle cap placement plate 402, a bottle pneumatic gripper 403, and a bottle cap in-position sensor 404. The second support base plate 401 is fixedly connected to the frame 1. The bottle cap placement plate 402 and the bottle body pneumatic gripper 403 are respectively arranged on both sides of the second support base plate 401, and the bottle cap placement plate 402 is located above the bottle body pneumatic gripper 403. The bottle cap placement plate 402 is provided with a bottle body clearance hole 4021 and a bottle cap placement groove 4022. The clamping position of the bottle body pneumatic gripper 403 is located below the bottle body clearance hole 4021. The bottle cap in place sensor 404 is located at the bottom of the bottle cap placement groove 4022 and is used to monitor whether the bottle cap is accurately placed after opening or removed before closing.

[0049] Specifically, the second support base plate 401 is fixedly connected to the frame 1 to provide an installation reference for the bottle cap placement plate 402 and the bottle body pneumatic gripper 403. The bottle cap placement plate 402 and the bottle body pneumatic gripper 403 are respectively arranged on both sides of the second support base plate 401, and the bottle cap placement plate 402 is located above the bottle body pneumatic gripper 403, so that while the bottle body is clamped and positioned below, the bottle cap can be temporarily stored and retrieved nearby above, reducing the horizontal transport distance.

[0050] Furthermore, the bottle cap placement plate 402 is provided with a bottle body clearance hole 4021 and a bottle cap placement groove 4022. The bottle body clearance hole 4021 is used to provide space for the upper part of the bottle body when clamping the bottle body, so as to avoid interference between the bottle body and the placement plate. The clamping position of the bottle body pneumatic gripper 403 is located below the bottle body clearance hole 4021, so that the bottle body can maintain axial stability after the gripper clamps it, which facilitates the screw cap assembly 702 to perform screwing operation at the bottle mouth position.

[0051] The cap placement slot 4022 is used to limit the placement of the cap after it has been opened. A cap presence sensor 404 is located at the bottom of the cap placement slot 4022 and is used to monitor whether the cap has been accurately placed after opening and whether it has been removed before closing, thus providing a process interlock signal to the control system. For example, when the sensor detects that the cap is not in place, subsequent processes such as pipetting or shaking can be prohibited. When preparing to close the cap, if the sensor still detects that the cap is in the slot, the capping assembly 702 is allowed to remove the cap and close it; otherwise, a missing cap or abnormal cap removal is indicated. Optionally, the cap presence sensor 404 can be a commonly used sensor such as a photoelectric / proximity / pressure contact, and the cap placement slot 4022 can be equipped with a guide chamfer or limiting step to improve the consistency of cap placement and reduce the risk of misplacement.

[0052] like Figure 9-10 As shown, the nuclear magnetic tube assembly assembly 5 includes: a rotor servo motor 501, a rotary indexing plate 502, a mounting bracket 504, a guide gripper 505, a telescopic cylinder 506, and a fixed pneumatic gripper 509. The rotor servo motor 501 is fixedly connected to the frame 1, and its output end is fixedly connected to the rotating indexing plate 502 on the same axis. The rotating indexing plate 502 is provided with a plurality of rotor placement slots 503 around its circumference. Mounting bracket 504 is fixedly connected to frame 1 and is located on one side of rotor servo motor 501. Guide gripper 505, telescopic cylinder 506 and fixed pneumatic gripper 509 are all fixed on mounting bracket 504. Guide gripper 505 is used to provide end guidance during the insertion of nuclear magnetic tube into rotor. The moving end of telescopic cylinder 506 is fixedly connected to slot plate 5061. Telescopic cylinder 506 cooperates with slot plate 5061 to fix rotor during the removal of nuclear magnetic tube from rotor. The fixed pneumatic gripper 509 cooperates with the nuclear magnetic tube handling assembly 704 to perform opening and closing operations on the nuclear magnetic tube. A rotor presence sensor 507 and a nuclear magnetic tube presence sensor 508 are provided on one side of the rotating indexing disk 502, and a nuclear magnetic tube positioning sensor 511 is provided at the lower part of the rotating indexing disk 502 to detect whether the insertion depth of the nuclear magnetic tube and the rotor meets the standard.

[0053] Specifically, the rotor servo motor 501 is fixedly connected to the frame 1, and its output end is coaxially fixedly connected to the rotating indexing plate 502. The rotating indexing plate 502 has multiple rotor placement slots 503 arranged around its circumference for array-type bearing and indexing positioning of multiple rotors. Through angle control of the rotor servo motor 501, the rotating indexing plate 502 can rotate the target rotor placement slot 503 to a preset assembly position, realizing rotor loading positioning and station switching. The guide gripper 505 provides end-point guidance during the insertion of the nuclear magnetic tube into the rotor, ensuring the nuclear magnetic tube maintains a stable posture when entering the rotor hole and reducing the risk of misalignment and scratching.

[0054] The moving end of the telescopic cylinder 506 is fixedly connected to the slot plate 5061. The telescopic cylinder 506 cooperates with the slot plate 5061 to limit and fix the rotor during the process of pulling out the nuclear magnetic tube: when the nuclear magnetic tube needs to be pulled out, the slot plate 5061 extends and forms a lock with the upper surface of the rotor, thereby ensuring that the rotor will not be pulled out along with the nuclear magnetic tube when the nuclear magnetic tube is pulled out.

[0055] The fixed pneumatic gripper 509 cooperates with the NMR tube handling assembly 704 to open or close the NMR tube. That is, after the NMR tube is delivered to the NMR tube assembly station, the fixed pneumatic gripper 509 clamps and fixes the NMR tube body, and the NMR tube handling assembly 704 clamps the NMR tube cap and moves it up and down to realize the opening and closing of the NMR tube.

[0056] To enable process status monitoring, a rotor in-place sensor 507 and a nuclear magnetic tube in-place sensor 508 are installed on one side of the rotary indexing plate 502 to detect whether the rotor and nuclear magnetic tube are in the preset assembly position, respectively; a nuclear magnetic tube positioning sensor 511 is installed at the bottom of the rotary indexing plate 502 to detect whether the insertion depth of the nuclear magnetic tube and the rotor meets the requirements, so as to avoid assembly abnormalities caused by insufficient insertion or over-insertion.

[0057] Optionally, as shown in the appendix Figure 9-10 As shown, a protective tube 510 can also be installed in the nuclear magnetic resonance tube assembly area to provide isolation protection and guidance shielding for the nuclear magnetic resonance tube opening and closing operation position, reducing the risk of accidental collision and liquid splashing.

[0058] like Figure 11 As shown, the top three-axis sample loading assembly 8 includes: a second longitudinal feed module 801, a second transverse feed module 802 and a fourth vertical feed module 803, and a sample loading pneumatic gripper 804 is fixedly connected to the moving end of the fourth vertical feed module 803. The second longitudinal feed module 801 and the second transverse feed module 802 are mounted on the top edge of the frame 1 and their travel covers the NMR tube assembly 5 and the external NMR spectrometer inlet.

[0059] Specifically, the second longitudinal feed module 801 and the second transverse feed module 802 are mounted on the top edge of the frame 1. Together, they form a top XY moving plane, ensuring their travel covers the NMR tube assembly 5 and the external NMR spectrometer inlet. This guarantees that the pneumatic gripper 804 can complete spatial transfer between the assembly station and the spectrometer inlet. The pneumatic gripper 804 is used to hold the assembled NMR tube rotor assembly and, under the coordination of the control system, executes the sample loading step: sending the assembled NMR tube rotor assembly into the NMR spectrometer for sample loading, and after testing, retrieving the sample back to the recovery station to achieve a fully automated closed-loop process.

[0060] In the specific embodiments of this application, the types of various feeding modules can be determined according to actual needs, and can be, for example, linear motor-slider guide rail module, lead screw guide rail-slider guide rail module, etc. The embodiments of this application do not limit this.

[0061] This application also provides a sample loading method using an NMR sample loading system, employing the NMR sample loading system described above. Includes the following steps: S1: In material storage area 2, complete the preparation for loading NMR tubes, sample vials, transfer bottles, solvent bottles, filter heads, and liquid dispensing heads onto the instrument; S2: The capping assembly 702 of the multi-functional robotic arm 7 opens the sample bottle and solvent bottle; the pipetting assembly 703 draws a preset volume of solvent from the solvent bottle and adds it to the sample bottle, then tightens the sample bottle cap. S3: Place the sample vial in the shaking assembly 3 and perform eccentric shaking to mix; S4: Use an imaging sensor to determine the dissolved impurities in the mixed sample; if it is determined that the impurities are not dissolved, return to step S3 to continue mixing; if it is determined that there are impurities, proceed to step S5 for filtration and transfer; if it is determined that there are no impurities and the impurities have been dissolved, proceed to step S6. S5: The pipetting assembly 703 filters the sample solution through the filter head into the transfer bottle; S6: The NMR tube handling assembly 704 takes the NMR tube from the NMR tube rack 201 to the NMR tube assembly 5 and opens the cap; the pipetting assembly 703 transfers the sample solution to the NMR tube and closes the cap. S7: The NMR tube transport assembly 704 inserts the NMR tube into the rotor of the NMR tube assembly assembly 5; S8: The top three-axis sample loading assembly 8 sends the assembled NMR tube rotor assembly into the NMR spectrometer to complete the sample loading; after the test is completed, the sample is unloaded and returned to the recycling station.

[0062] Further, optionally, the imaging sensor is used to determine the dissolution state and impurity state of the mixed sample. It can be set on the frame 1 to form an independent imaging detection station. The imaging detection station is located near the oscillation and mixing component 3 and within the range of motion of the multi-functional robot 7. The imaging detection station includes an imaging sensor and a light source component that works with it, and a light shield can be set to reduce ambient light interference. After completing the eccentric oscillation mixing in step S3, the multi-functional robot 7 transfers the sample bottle to the imaging detection station. The control system is configured to stop the oscillation of the sample bottle and let it stand for a preset time before imaging acquisition to reduce the influence of liquid surface fluctuations and bubbles on imaging. Then, the imaging sensor takes pictures of the liquid in the sample bottle and outputs them to the control system. Optionally, the imaging sensor can also be fixedly installed above or to the side of the oscillating and shaking assembly 3, with the lens aimed at the bottle placement hole area of ​​the oscillating tray, and an observation window or opening structure provided on the protective housing to meet the requirements of image acquisition; further optionally, the imaging detection adopts a lateral transmission arrangement, that is, an imaging sensor is set on one side of the bottle and a backlight plate is set on the other side to obtain a transmission image, thereby improving the sensitivity of identification of suspended particles, flocculent matter and sedimentation boundary; Furthermore, the control system is configured to determine the sample's three states—"undissolved / with impurities / without impurities and dissolved"—based on images acquired by the imaging sensor. Preferably, the liquid area located in the lower part of the bottle is selected as the determination area in the image, and a preset area near the bottom of the bottle can be further selected as the sedimentation detection area. The control system can perform preprocessing such as grayscale normalization and background correction on the determination area to reduce the impact of bottle wall thickness and changes in illumination. When the judgment area is generally turbid or has insufficient transmittance, the control system determines that the sample is undissolved based on a comparison of preset turbidity indicators, such as the mean gray value, gray value variance, contrast, or transmission intensity of the judgment area with a threshold, and controls the process to return to step S3 for further mixing. When the judgment area contains particles, flocculent matter, or bottom sedimentation characteristics, the control system determines that the sample contains impurities based on a comparison of preset impurity indicators, such as the number of connected domains of particles, total area, maximum size, or the proportion of sedimentation area with a threshold, and controls the process to proceed to step S5 for filtration and transfer. When the judgment area meets the clarity condition and the impurity indicators are below the threshold, the control system determines that the sample is free of impurities and has dissolved, and controls the process to proceed to step S6 for NMR tube sample addition and capping. Optionally, the control system can use multi-frame acquisition to obtain the median or acquire images before and after settling for comparison to suppress the influence of reflection, bubbles, and occasional suspended matter on the judgment results, thereby improving the stability and consistency of the judgment.

[0063] The above description is only a preferred embodiment of the present invention. It should be noted that those skilled in the art can make several modifications and improvements without departing from the inventive concept of the present invention, and these all fall within the protection scope of the present invention.

Claims

1. An NMR sample loading system, characterized in that, include: Rack (1); The following components are set on the frame (1): material storage area (2), oscillation and shaking assembly (3), several sets of bottle clamping assemblies (4), nuclear magnetic tube assembly assembly (5), horizontal movement assembly (6), top three-axis sample loading assembly (8), and imaging sensor and control system. The horizontal moving component (6) is provided with a multi-functional manipulator (7), which includes a capping component (702), a pipetting component (703), and a nuclear magnetic resonance tube handling component (704). The capping assembly (702) includes a first vertical feed module (7021) and a rotary electric gripper (7023). The capping assembly (702) cooperates with the bottle clamping assembly (4) to open or close sample bottles, transfer bottles or solvent bottles. A mounting plate (7022) is fixedly connected to the moving end of the first vertical feed module (7021). A horizontally set limiting plate (7024) is fixedly connected to the upper end of the mounting plate (7022). The rotating electric gripper (7023) is vertically slidably connected to the mounting plate (7022). A plurality of buffer springs (7025) are provided between the upper end of the rotating electric gripper (7023) and the limiting plate (7024). The limiting plate (7024) is provided with a displacement sensor (7026), and the upper part of the rotating electric gripper (7023) is provided with a trigger plate (7027) that cooperates with the displacement sensor (7026). The control system is configured to dynamically control the rotation of the rotating electric gripper (7023) and the lifting of the first vertical feed module (7021) based on the displacement signal of the trigger plate (7027) monitored by the displacement sensor (7026), so as to realize abnormal error correction and locking in the closing operation. The control system controls the capping assembly (702) to perform the following steps during the capping operation: Step 1: The first vertical feed module (7021) drives the rotating electric claw (7023) holding the bottle cap to descend to contact the bottle mouth and maintain a preset initial downward pressure, causing the buffer spring (7025) to contract and the trigger plate (7027) to move upward a preset distance S1; Step 2: Control the rotating electric gripper (7023) to rotate in the opposite direction and monitor the vertical displacement change signal of the trigger plate (7027) in real time; when the change signal is detected, determine that the bottle cap is aligned with the starting point of the bottle mouth thread and stop the reverse rotation; Step 3: Control the rotating electric gripper (7023) to rotate in the forward direction with a preset preload torque, while the first vertical feed module (7021) moves downward synchronously, and the movement signal S of the trigger plate (7027) is acquired in real time; Step 4: If the downward depth value does not reach the preset target depth threshold, the movement signal S exceeds the preset range, and it is determined that a thread misalignment jam has occurred. Then, the rotary electric gripper (7023) is controlled to rotate in the opposite direction for a preset number of turns, and the first vertical feed module (7021) rises synchronously. Then, the rotary electric gripper (7023) is controlled to place the bottle cap on the horizontal surface and grab it again, and returns to Step 1 until the movement signal is within the preset range or the maximum number of retries is reached during the screwing process. If all the movement signals during the screwing-in process are within the preset range, then proceed to step five; If the maximum number of retries is reached, an exception alarm will be triggered. Step 5: Increase the positive output torque of the rotating electric gripper (7023) to the rated sealing torque, and complete the cover closing operation after reaching the rated sealing torque.

2. The NMR sample loading system according to claim 1, characterized in that, The oscillating and mixing component (3) is used to eccentrically oscillate and mix the bottle. The bottle clamping assembly (4) is used to clamp the bottle and monitor whether the bottle cap has been removed; The nuclear magnetic resonance tube assembly (5) is used to cooperate with the multifunctional robot (7) to open or close the nuclear magnetic resonance tube, insert the nuclear magnetic resonance tube containing the test liquid and solvent into the rotor before the test, and remove the nuclear magnetic resonance tube from the rotor after the test. The horizontal moving component (6) is used to drive the multi-functional robot (7) to move in the plane above the material storage area (2), the oscillation and shaking component (3), the bottle clamping component (4), and the nuclear magnetic tube assembly component (5); The top triaxial sample loading assembly (8) is used to send the assembled nuclear magnetic tube and rotor assembly into the sample loading position of the nuclear magnetic resonance spectrometer and to perform sample unloading and recovery after the detection is completed; The control system is configured to coordinate the horizontal movement component (6), the multi-functional robotic arm (7), the oscillation and shaking component (3), the bottle clamping component (4), the nuclear magnetic tube assembly component (5), and the top three-axis sample loading component (8) to complete the automatic sample loading according to the preset process.

3. The NMR sample loading system according to claim 2, characterized in that, The material storage area (2) includes: NMR tube rack (201), sample bottle rack (202), transfer bottle rack (203), filter head rack (204), and liquid collection head rack (205); the NMR tube rack (201), sample bottle rack (202), transfer bottle rack (203), filter head rack (204), and liquid collection head rack (205) are all divided into a material supply area and a recycling area; the material supply area is used to provide consumables to be used, and the recycling area is used to recycle consumables after use.

4. The NMR sample loading system according to claim 3, characterized in that, The pipetting assembly (703) includes a second vertical feed module (7031) and a pipette (7032) for adding, taking and transferring liquids between sample vials, transfer vials and NMR tubes; The NMR tube handling assembly (704) includes a third vertical feed module (7041) and an electric gripper (7042) for picking up and placing NMR tubes from the NMR tube rack (201) and delivering the NMR tubes to the NMR tube assembly assembly (5), and removing used NMR tubes from the NMR tube assembly assembly (5) and delivering them to the recycling area; The first vertical feed module (7021), the second vertical feed module (7031) and the third vertical feed module (7041) are fixedly connected to one side of the mounting back plate (701). The mounting back plate (701) is fixedly connected to the moving end of the horizontal moving component (6). The first vertical feed module (7021), the second vertical feed module (7031) and the third vertical feed module (7041) drive the capping component (702), the pipetting component (703) and the NMR tube transport component (704) to move independently in the vertical direction, respectively.

5. The NMR sample loading system according to claim 4, characterized in that, The lower part of the rotating electric gripper (7023) is provided with a capping working head (7028), which includes a turntable (70281) and telescopic rods (70282) symmetrically arranged on both sides of the turntable (70281). The ends of the telescopic rods (70282) are respectively fixedly connected to a pair of spaced capping contacts (70284) through extension plates (70283).

6. The NMR sample loading system according to claim 5, characterized in that, The bottle clamping assembly (4) includes: a second support base plate (401), a bottle cap placement plate (402), a bottle pneumatic gripper (403), and a bottle cap in-place sensor (404). The second support base plate (401) is fixedly connected to the frame (1), the bottle cap placement plate (402) and the bottle body pneumatic gripper (403) are respectively arranged on both sides of the second support base plate (401), and the bottle cap placement plate (402) is located above the bottle body pneumatic gripper (403); The bottle cap placement plate (402) is provided with a bottle body clearance hole (4021) and a bottle cap placement groove (4022). The clamping position of the bottle body pneumatic gripper (403) is located below the bottle body clearance hole (4021). The bottle cap in-place sensor (404) is located at the bottom of the bottle cap placement groove (4022) and is used to monitor whether the bottle cap is accurately placed after opening or removed before closing.

7. The NMR sample loading system according to claim 6, characterized in that, The nuclear magnetic tube assembly (5) includes: a rotor servo motor (501), a rotary indexing plate (502), a mounting bracket (504), a guide gripper (505), a telescopic cylinder (506), and a fixed pneumatic gripper (509). The rotor servo motor (501) is fixedly connected to the frame (1), and its output end is fixedly connected to the rotating indexing plate (502) on the same axis. The rotating indexing plate (502) has multiple rotor placement slots (503) around its circumference. The mounting bracket (504) is fixedly connected to the frame (1) and is located on one side of the rotor servo motor (501). The guide gripper (505), telescopic cylinder (506) and fixed pneumatic gripper (509) are all fixed on the mounting bracket (504). The guide gripper (505) is used to provide end guidance during the insertion of the nuclear magnetic tube into the rotor. The moving end of the telescopic cylinder (506) is fixedly connected to the slot plate (5061). The telescopic cylinder (506) cooperates with the slot plate (5061) to fix the rotor during the removal of the nuclear magnetic tube from the rotor. The fixed pneumatic gripper (509) cooperates with the nuclear magnetic tube handling assembly (704) to perform opening and closing operations on the nuclear magnetic tube; A rotor in-situ sensor (507) and a nuclear magnetic tube in-situ sensor (508) are provided on one side of the rotating indexing disk (502), and a nuclear magnetic tube positioning sensor (511) is provided at the lower part of the rotating indexing disk (502) to detect whether the insertion depth of the nuclear magnetic tube and the rotor meets the standard.

8. The NMR sample loading system according to claim 7, characterized in that, The top three-axis sample loading assembly (8) includes: a second longitudinal feed module (801), a second transverse feed module (802) and a fourth vertical feed module (803), wherein a sample loading pneumatic gripper (804) is fixedly connected to the moving end of the fourth vertical feed module (803). The second longitudinal feed module (801) and the second transverse feed module (802) are mounted on the top edge of the frame (1) and their travel covers the nuclear magnetic tube assembly (5) and the external nuclear magnetic resonance spectrometer inlet.

9. A sample loading method for an NMR sample loading system, employing the NMR sample loading system according to any one of claims 1-8, characterized in that, Includes the following steps: S1: In the material storage area (2), complete the preparation for the installation of NMR tubes, sample bottles, transfer bottles, solvent bottles, filter heads and liquid dispensing heads. S2: The capping assembly (702) of the multi-functional robotic arm (7) opens the sample bottle and the solvent bottle; the pipetting assembly (703) draws a preset volume of solvent from the solvent bottle and adds it to the sample bottle, then tightens the sample bottle cap; S3: Place the sample vial in the shaking assembly (3) and perform eccentric shaking to mix; S4: Use an imaging sensor to determine the dissolved impurities in the mixed sample; if it is determined that they are not dissolved, return to step S3 to continue mixing. If impurities are detected, proceed to step S5 for filtration and transfer. If it is determined that there are no impurities and the solution has been dissolved, then proceed to step S6; S5: The pipetting assembly (703) filters the sample solution through the filter head into the transfer bottle; S6: The NMR tube handling assembly (704) takes the NMR tube from the NMR tube rack (201) to the NMR tube assembly assembly (5) and opens the cap; the pipetting assembly (703) transfers the sample solution to the NMR tube and closes the cap; S7: The NMR tube transport assembly (704) inserts the NMR tube into the rotor of the NMR tube assembly assembly (5); S8: The top three-axis sample loading assembly (8) sends the assembled nuclear magnetic tube rotor assembly into the nuclear magnetic resonance spectrometer to complete the sample loading; after the test is completed, the sample is unloaded and recycled to the recycling station.

Images