A high-throughput automated multispectroscopy integrated experimental method, system and medium

Abstract

The application discloses a high-throughput automatic multi-spectroscopy integrated experiment method, system and medium, and belongs to the technical field of automatic experiment and spectroscopy analysis. The method comprises the following steps: material warehouse-out and analysis driven by a general control system module, automatic preparation by a pretreatment device, transmission through a ground rail and a magnetic suspension system, automatic multi-spectroscopy parallel test, automatic recovery by a post-treatment device, and material warehouse-in and data closed loop. The experiment system integrates an automatic storage device, a multi-spectroscopy test workstation and a machine scientist interactive module, realizes full-process unmanned operation and data traceability, solves the problems of low efficiency, discrete process and incapability of cooperation with an AI system of existing spectroscopy experiments, significantly improves spectroscopy characterization efficiency, supports AI-driven intelligent research and development, and is suitable for material science, catalytic screening and chemical analysis scenes.

Description

Technical Field

[0001] This invention relates to the technical field of automated experiments and spectroscopic analysis, specifically to a high-throughput automated multi-spectral integrated experimental method, system, and medium. Background Technology

[0002] Current spectroscopic experiments heavily rely on manual operation, resulting in low efficiency and lengthy cycles for multi-sample, multi-spectral testing. The lack of unified scheduling among individual instruments hinders collaborative and parallel operations. The management of materials, consumables, and reagents depends on paper records or unstructured data, lacking digital tracking and real-time inventory monitoring, making errors prone to occur. High levels of manual intervention in sample transfer, capping, cleaning, and recycling pose risks of cross-contamination and result in poor repeatability. Furthermore, the fragmented storage of test parameters, operational logs, and spectral data fails to form a complete data loop, hindering efficient integration with AI-driven machine scientist systems, a problem that urgently needs to be addressed. Summary of the Invention

[0003] This invention proposes a high-throughput automated multi-spectral integrated experimental method, which aims to solve the technical problems of high dependence on manual operation, discrete process, difficulty in multi-device collaboration, lack of data closed loop and difficulty in connecting to AI system in existing spectroscopic experiments, resulting in low overall characterization efficiency and long R&D cycle.

[0004] A high-throughput automated multispectral integrated experimental method includes: S1. The central control system module issues experimental tasks and drives the automated warehousing device to scan and release consumables, reagents, samples and containers, and analyze consumables. S2. The pretreatment device performs solid injection, liquid transfer, dilution, ultrasonic mixing, magnetic stirring, cap opening and closing, tableting and filtration operations on the outgoing materials to complete sample preparation. S3. The tray carrying the processed sample is automatically transported to the designated spectroscopic testing workstation through a transmission system consisting of a ground-rail robotic arm and a magnetic levitation transmission line. S4. Each spectroscopic testing workstation independently completes automatic sample loading, parameter configuration, data acquisition and automatic sample unloading, realizing parallel testing of at least multiple spectroscopic methods including ultraviolet, infrared, Raman, fluorescence, circular dichroism, circular polarization, nuclear magnetic resonance, electrochemistry, photocatalysis, liquid chromatography, high-resolution mass spectrometry and gas chromatography-mass spectrometry. S5. The post-processing unit performs cleaning, drying, waste liquid treatment and material recycling operations on the tested containers and trays. S6. The recycled empty containers and pallets are automatically returned to the warehouse by the automated storage device, and the experimental parameters, operation logs, spectroscopic data and time scales are recorded throughout the process by the central control system module, forming traceable closed-loop data.

[0005] Furthermore, in S1, the automated warehousing device specifically performs QR code scanning for inbound and outbound operations and real-time inventory monitoring operations.

[0006] Furthermore, in S2, the solid sample injection is performed by a small solid sampler or a large solid sampler in conjunction with a balance positioning linear motion module; the liquid pipetting is performed by an automatic pipetting module; the ultrasonic mixing is performed by an ultrasonic mixing module; the cap opening and closing is performed by a cap opening and closing gripper; the tableting is performed by a tablet press; and the filtration is performed by a filtration device.

[0007] Furthermore, in S5, the cleaning is performed by an ultrasonic cleaner, the drying is performed by a dryer, the waste liquid treatment is performed by a liquid addition pump head, a liquid extraction pump head and a waste liquid monitoring module, and the material recycling is performed by a solid recycling unit.

[0008] Furthermore, in S4, each spectroscopic testing workstation is equipped with a dedicated robotic arm, a sample tray placement station, a cover clamp, and a rotating electric gripper to perform the automatic sample loading, testing, and unloading operations.

[0009] Furthermore, the overall control system module interacts with the automated storage device, preprocessing device, transmission system, postprocessing device, and each spectroscopic testing workstation through communication interface units that support SDK, HTTP, TCP / IP, and RS485 serial port protocols.

[0010] Furthermore, it supports high-throughput parallel testing of multiple samples, and supports mid-process material change, breakpoint continuation testing, and anomaly alarms.

[0011] Furthermore, the present invention proposes a high-throughput automated multispectral integrated experimental system, comprising: a central control software module, a storage management module, a preprocessing control module, a postprocessing control module, a transmission scheduling module, a multispectral driving module, a data management module, and a machine scientist interaction module; and an integrated experimental device for executing the high-throughput automated multispectral integrated experimental method.

[0012] Furthermore, the multi-spectral driving module supports the automatic execution of various standardized full-processes, including ultraviolet full-process, electrochemical full-process, photoreaction full-process, NMR full-process, infrared full-process, Raman full-process, liquid chromatography full-process, fluorescence full-process, circular dichroism full-process, circular polarization full-process, and mass spectrometry full-process.

[0013] Furthermore, the present invention proposes a computer-readable storage medium storing a computer program thereon, which, when executed by a processor, implements the steps of the high-throughput automated multispectral integrated experimental method described above.

[0014] This invention proposes a high-throughput automated multi-spectral integrated experimental method and system, achieving fully unmanned operation from material warehousing to data closure. Based on the aforementioned collaboration, testing efficiency is significantly improved, allowing multi-spectral characterization to be completed in parallel in a single experiment, greatly shortening the R&D cycle. This end-to-end digital management supports a high degree of standardization, repeatability, and traceability of materials and data, and through open multi-protocol interfaces, it achieves seamless integration with machine scientist interaction modules, forming a high-throughput screening closed loop from task input to automated execution to data output to AI re-decision, breaking through the limitations of traditional discrete experiments. Attached Figure Description

[0015] Figure 1 This is a flowchart illustrating a high-throughput automated multispectral integrated experimental method proposed in this invention. Figure 2 This is a schematic diagram of the overall architecture of the high-throughput automated multispectral integrated experimental system of the present invention; Figure 3 This is a schematic diagram of the structure of the automated warehousing device of the present invention; Figure 4 This is a schematic diagram of the module configuration structure of the preprocessing device of the present invention; Figure 5 This is a schematic diagram of the layout structure of the transmission system and multispectral testing workstation of the present invention; Figure 6 This is a schematic diagram of the module configuration structure of the post-processing device of the present invention; Figure 7 This is a schematic diagram of the communication and interaction structure between the overall control system module and each device of the present invention; Figure 8 This is a schematic diagram of the software module structure of the high-throughput automated multispectral integrated experimental system of the present invention. Detailed Implementation

[0016] refer to Figure 1 This invention proposes a high-throughput automated multispectral integrated experimental method, comprising: S1, the central control system module issues experimental tasks and drives the automated storage device to scan and release consumables, reagents, samples and containers, and analyze consumables.

[0017] Specifically, the automated storage and warehousing system includes a consumables warehouse, a reagent warehouse, a solid sample warehouse, and a container pallet warehouse. Upon outbound shipment, the automated storage and warehousing system uses a QR code scanning module to identify and register the required items. Subsequently, the warehouse management module verifies inventory and analyzes usage to ensure that materials match experimental tasks. For example, before a typical experiment, the automated storage and warehousing system scans and dispatches a hopper containing a solid sample, a reagent bottle containing acetonitrile solvent, and a set of reaction flasks and cuvettes, recording their unique identification codes. This automated material station is further subdivided into areas for storing solid samples, reagents, and consumables, reagent bottles, and liquid samples, and is equipped with an equipment usage recording module. Each pallet in the pallet warehouse has a material station pallet identification code for tracking.

[0018] In a specific implementation scenario, combined with Figure 2 and Figure 3 As shown, the central control system module sends instructions to the automated storage device. The consumables warehouse, reagent warehouse, solid sample warehouse, and container pallet warehouse in the automated storage device receive the outbound instructions and complete the consumables parsing through the QR code scanning module. Then, the outbound materials are transferred to the next process.

[0019] S2. The pretreatment device performs solid injection, liquid transfer, dilution, ultrasonic mixing, magnetic stirring, cap opening and closing, tablet pressing and filtration operations on the outgoing materials to complete sample preparation.

[0020] Specifically, this pretreatment device integrates a solid sampler, an automated pipetting module, an ultrasonic mixer, a magnetic stirrer, a tablet press, an electric gripper for opening and closing the cap, and a filtration device. These modules work together to automatically complete processes such as solid sample addition, liquid pipetting, dilution, ultrasonic mixing, magnetic stirring, tablet pressing, and filtration based on the formula file issued by the central control system module. For example, the solid sampler accurately weighs the sample powder according to a preset mass, the automated pipetting module draws a quantitative amount of acetonitrile solvent into the reaction flask, ultrasonic mixing is then used to fully dissolve the sample, and finally, the electric gripper for opening and closing the cap completes the process.

[0021] The pretreatment workstation is divided into two parts. The core configuration of the first part includes the METLER TOLEDO solvent solid sampler, gripping and capping electric gripper, robotic arm, ultrasonic instrument, multi-size pipettes (such as 10ml, 5ml, 1ml), solid sampler, solid sampler balance positioning linear motion module, material placement stage, fixed gripper, and base for placing 10ml, 20ml, 50ml, 100ml, and 500ml stock solution bottles, tip container and bottle cap. The typical operating procedure (taking UV experiment as an example) is as follows: The ground-rail robotic arm picks up a cuvette, a 1ml tip, three 10ml reaction flasks, and a 100ml stock solution bottle and places them in the corresponding positions on the pretreatment workstation; then the robotic arm uses grippers to open the 10ml bottle; next, the 10ml reaction flask is placed into the solid sampler, and the ground-rail robotic arm retrieves the powder from the powder hopper and places the powder into the solid sampler transfer station; the robotic arm picks up the powder hopper from the transfer station, places it into the solid sampler, and completes the sample addition; then the powder hopper is stored; next, the liquid addition operation is performed, adding liquid to the first row of reaction flasks; during the liquid transfer process, the robotic arm picks up 10ml... Open the cap of the 100ml stock solution bottle using the tip, lower the tip, remove the gripper, close the cap of the reaction bottle, and place the reaction bottle into the sonicator. Then, add the solution from the first row of reaction bottles to the second row of reaction bottles. Repeat this process to open all the 10ml reaction bottles that need to participate in the reaction. Finally, take a 10ml pipette and transfer the liquid from the second row of bottles into cuvettes in positions 3-9, or take 100ml of liquid into cuvettes in positions 1 and 2. After sample addition, the guide rail will transport each material to the reaction station. The second part is equipped with grippers, a filter device, a pipette, an assembly table, a window panel fabrication platform, a waste storage area, a robotic arm, and a material storage platform. In Mode 1 (LC-MS vials), the process is as follows: Place the required materials into the material storage stage (position 1 for the 10ml stock solution vial, position 2 for the LC-MS plate, and positions 3 and 4 for the syringes); place the LC vial on the LC plate onto the assembly stage; remove the gripper and place the syringe onto the filter; place the 10ml stock solution vial onto the assembly stage; start the filter; after filtration, remove the placed LC vials, stock solution vials, and syringes, discarding the syringes into the waste storage area and returning the other two to their original positions. In Mode 2 (window plate fabrication), the process is as follows: Place the required materials into the material storage stage (position 1 for the tip, position 2 for the stock solution vial, and position 3 for the window plate); the robotic arm removes the gripper and places the window plate onto the window plate platform; use a pipette to transfer the solution from the stock solution vial onto the window plate; then dry the solution; finally, remove the window plate.

[0022] In a specific implementation scenario, such as Figure 4 As shown, after receiving the material from the automated storage device, the pretreatment unit uses a solid sampler, an automatic liquid transfer module, an ultrasonic mixer, a magnetic stirrer, a tablet press, an electric gripper for opening and closing the lid, and a filter device to perform the pretreatment operation, and outputs the prepared sample tray to the transmission system.

[0023] S3. The tray carrying the processed sample is automatically transported to the designated spectroscopic testing workstation via a transmission system consisting of a ground-rail robotic arm and a magnetic levitation transmission line.

[0024] Specifically, the transfer system includes a first-level ground-rail robotic arm, a second-level ground-rail robotic arm, and a magnetic levitation transport line. The first robotic arm is responsible for picking up a pallet from the pre-processing station and transferring it to the transfer area. The magnetic levitation transport line then quickly and smoothly transports the pallet to the waiting area of ​​the designated spectroscopic workstation. Finally, the second robotic arm precisely places the pallet onto the sample station of the workstation. The working area of ​​the first ground-rail robotic arm covers the solid hopper transfer area, the reagent bottle transfer area, and the pallet transfer area. The second ground-rail and robotic arm also have pallet transfer stations for secondary material transfer and connection.

[0025] In a specific implementation scenario, combined with Figure 5 As shown, the transmission system consists of a ground-rail robotic arm and a magnetic levitation transmission line. The ground-rail robotic arm picks up a tray from the pre-processing station and hands it over to the magnetic levitation transmission line, which then transports the tray to each spectroscopic testing workstation.

[0026] S4. Each spectroscopic testing workstation independently completes automatic sample loading, parameter configuration, data acquisition, and automatic sample unloading, enabling parallel testing of at least multiple spectroscopic methods, including ultraviolet, infrared, Raman, fluorescence, circular dichroism, circular polarization, nuclear magnetic resonance, electrochemical, photocatalysis, liquid chromatography, high-resolution mass spectrometry, and gas chromatography-mass spectrometry.

[0027] Specifically, for example, in a UV spectrometer workstation, a dedicated robotic arm picks up a single cuvette from the sample tray and places it into the instrument's measurement chamber. The instrument automatically configures parameters such as the scanning wavelength range and begins data acquisition. After acquisition is complete, the robotic arm returns the sample to the tray. Throughout the process, multiple workstations, including UV, IR, Raman, and NMR, can perform tests simultaneously without interference.

[0028] In addition, each workstation has a detailed operating procedure: The infrared spectrometer workstation is equipped with an IRTracer-100 spectrometer, a tablet press, tablet press clamps, an alcohol cleaning module, and a material storage platform. Its operating modes include: Mode 1 (Liquid Mode): Place a tip in position 1 of the material storage platform, a 10ml reaction flask in position 2, and a cotton swab in position 3; the robotic arm retrieves the rotating clamps, uses a cotton swab dipped in alcohol to clean the detection platform, and then dries it with the swab; subsequently, it retrieves the tip, uses a pipette, and drops the solution from the reaction flask onto the detection platform, inserts it into the instrument for detection, and repeats the detection cycle; after each detection, it needs to be cleaned and dried again with a cotton swab. Mode 2 (Tablet Mode): Place the tablet in position 2; the robotic arm uses the clamps to place it in the tablet press slot, starts the tablet press, inserts the tablet into the instrument for detection, and removes the tablet after detection. Mode 3 (Window Plate Mode): Place the window plate in position 2; the robotic arm retrieves the window plate and inserts it into the instrument for detection. The liquid chromatography workstation is equipped with a robotic arm, rotary grippers, fixed grippers, a waste storage area, a material placement stage, rinsing tanks (positions 1 and 2), and a suction head. The procedure is as follows: place the liquid chromatography material tray on the storage stage, remove the rotary grippers, the instrument door automatically opens, place the material tray into the instrument, place the vial on the storage stage and open the cap, and remove the material tray after analysis. The photoreaction and electrochemical workstation integrates an electrolytic cell (positions 1 and 2), electrode holders (positions 1 and 2), photoreaction grippers, electrochemical grippers, a photoreaction material placement stage, an electrochemical material placement stage, photoreaction measurement equipment, and an electrochemical workstation. The photoreaction procedure is as follows: remove the grippers to open the instrument, place the analyte into the instrument, close the door to start the reaction, and remove the vial after the reaction is complete. The electrochemical process is as follows: Place the suction head into the material bottle, open the bottle, and draw liquid into the electrolytic cell; place the material into the gripper, and use the robotic arm to rub the electrode (removing the oxide layer). Place the electrode into the electrolytic cell and draw liquid into the cell again; drain the liquid after draining (equivalent to cleaning the electrolytic cell); then inject cleaning solution into the cleaning tank, and inject cleaning solution into the electrolytic cell again, then drain; begin the reaction; after detection, empty the electrolytic cell; finally, close the material cover, and the process ends. The UV spectrometer workstation is equipped with a dedicated robotic arm and material placement stage. The process is as follows: the robotic arm opens the instrument cover, places the material in, closes the cover, and performs detection; after detection, remove the material, and repeat this cycle.

[0029] The Raman spectrometer workstation is equipped with a moving guide rail, laser source (laser emitter), source controller, HORIBA dedicated motion controller, CCD camera, HR550 imaging spectrometer, and magnetic levitation tray. The procedure is as follows: the magnetic levitation tray carries the sample to be measured, aligns with the laser, and starts the measurement. After measuring one aperture, the tray moves again to align the other apertures with the laser for further measurement. The circular dichroism (CD) spectrometer workstation is equipped with a dedicated robotic arm, circular dichroism grippers, fixed grippers, a waste disposal area, and a material placement stage. The procedure is as follows: remove the grippers, open the instrument door, place the sample, close the instrument door, and start the detection; repeat this cycle to measure all samples, and then remove the sample after detection. The high-resolution mass spectrometer workstation is equipped with high-quality grippers, a robotic arm, and a material placement stage. The procedure is as follows: remove the grippers, pull out the drawer, place the sample on the drawer, push the drawer back to close the door, and then perform the detection; after detection, remove the sample. The Circular Polarization Spectrometer (CPL) workstation is equipped with a robotic arm for loading and unloading CPL samples. The process is as follows: the robotic arm on the ground rail (position 2) picks up the sample, opens the instrument door, places the sample in for testing, and removes the sample after testing. This process is repeated. The NMR workstation uses an HT Spinsolve 80 UTRAMultiX magritek benchtop NMR spectrometer, equipped with an NMR tube assembly station (containing 10 stations), an NMR workstation robotic arm, NMR tube clamping components, and NMR tubes. The complex process is as follows: NMR tube No. 1 is placed on assembly station No. 10, and the clamps on assembly station No. 10 open the lid; the robotic arm drives pipette No. 3 to add the test reagent; clamping jaw No. 8 clamps the NMR tube with added reagent and places it on position No. 6; expansion tube No. 2 is placed on position No. 6, and the NMR tube is pushed to the bottom of the expansion tube using the top tube No. 7, and then pushed onto the NMR tube; after NMR testing, the process is reversed to return the NMR tube to position No. 1. The fluorescence spectrometer workstation is equipped with a dedicated robotic arm and sample tray placement station. The workflow is as follows: the robotic arm opens the instrument cover, the material is placed in, the cover is closed for detection, the material is removed after detection, and this process is repeated. The gas chromatography-mass spectrometry (GC-MS) workstation consists of EWAI brand equipment. The entire platform has a compact layout, with the pretreatment and posttreatment workstations located in the center. Above are instruments such as LC-MS, CPL circular polarization analyzer, benchtop NMR, fluorescence spectrometer, and GC-MS, while below are instruments such as circular dichroism analyzer, UV-Vis analyzer, electrochemical analyzer, Raman analyzer, LC-MS, and IR analyzer, together forming a complete analytical testing chain.

[0030] In a specific implementation scenario, such as Figure 5 As shown, each spectroscopic testing workstation receives the tray delivered by the transmission system and independently completes automatic sample loading, parameter configuration, data acquisition, and automatic sample unloading. Each spectroscopic testing workstation runs in parallel and outputs the completed container.

[0031] S5. The post-processing unit performs cleaning, drying, waste liquid treatment, and material recycling operations on the tested containers and trays.

[0032] Specifically, the post-processing unit includes an ultrasonic cleaner, a dryer, a liquid dispensing pump head, a liquid extraction pump head, and a waste liquid monitoring module. Containers are fed into the ultrasonic cleaner, cleaned in the cleaning solution, and then dried in the dryer. The waste liquid after cleaning is discharged by the liquid extraction pump head, and its discharge rate is monitored. The dried empty containers and trays are recycled to a designated location. The post-processing workstation is equipped with a dryer, a robotic arm, a liquid extraction pump head, a cleaning solution module, an ultrasonic cleaner, a water tank, and a reagent bottle placement structure. The standard operating procedure is as follows: the robotic arm picks up the liquid dispensing pump head, extracts the liquid from the bottle, retains the cuvette bottle, places it in the ultrasonic cleaner for cleaning, then places it in the dryer for drying, and finally returns the cuvette bottle to its original position.

[0033] In a specific implementation scenario, such as Figure 6 As shown, the post-processing unit uses an ultrasonic cleaner, dryer, liquid adding pump head, liquid drawing pump head and waste liquid monitoring module to process the tested containers and pallets, and outputs the recovered materials to the automated storage device.

[0034] S6. The recycled empty containers and pallets are automatically returned to the warehouse by the automated storage device, and the experimental parameters, operation logs, spectroscopic data and time scales are recorded throughout the process by the central control system module, forming traceable closed-loop data.

[0035] Specifically, upon return to the warehouse, the QR code scanning module scans the container and pallet information again to update the inventory. The central control system module records all process parameters from S1 to S5, including pipetting volume, sonication time, instrument settings, operation logs, and raw spectral data for each spectroscopic study, forming a complete experimental data package with timestamps, thus achieving a closed-loop data transmission chain.

[0036] By constructing a complete process from automated logistics to pre-processing to parallel testing to post-processing to data closure, the core problems of traditional experimental processes—discreteness, excessive manual intervention, and fragmented data—are solved, thus forming a high-throughput, standardized experimental closure that collaborates with AI systems.

[0037] Furthermore, the automated warehousing equipment specifically performs QR code scanning for inbound and outbound operations and real-time inventory monitoring.

[0038] Specifically, in S1, the automated warehousing device performs the functions of scanning QR codes for inbound and outbound goods and real-time inventory monitoring. For example, when the automated warehousing device needs to issue a pallet, it first sends an instruction to the pallet warehouse, where an automated mechanical device moves the pallet to the scanning station. A fixed QR code scanner at the station reads the QR code on the bottom of the pallet, and the automated warehousing device parses the pallet's size, material, and current status. Simultaneously, the inventory monitoring module updates the pallet's inventory quantity and location information in real time, ensuring the accuracy of the inventory data. The process is similar for reagent bottles and solid sample hoppers. Each unit is associated with its unique QR code and information such as batch number, remaining quantity, and expiration date in the system database, ensuring full digitalization and traceability of material flow. Precise digital outbound and inventory management is the foundation for building a fully automated closed-loop system, avoiding process interruptions caused by material errors and ensuring the reliability of the experimental closed loop.

[0039] In a specific implementation scenario, such as Figure 3 As shown, when the automated warehousing device performs a return operation, it scans the information again through the QR code scanning module, and the warehouse management module updates the inventory.

[0040] Furthermore, in S2, the solid sample introduction is performed by a small solid sampler or a large solid sampler in conjunction with a balance positioning linear motion module; the liquid pipetting is performed by an automatic pipetting module; the ultrasonic mixing is performed by an ultrasonic mixing module; the cap opening and closing is performed by a cap opening and closing gripper; the tableting is performed by a tablet press; and the filtration is performed by a filtration device.

[0041] Specifically, the pretreatment unit integrates multiple actuators. The solid sampler is divided into a small solid sampler and a large solid sampler with a balance positioning linear motion module, used for accurately weighing and adding powder samples of different particle sizes. The automated pipetting module uses multi-channel pipette tips to accurately aspirate and dispense liquid reagents. The ultrasonic mixing module accelerates sample dissolution or homogenization. The tablet press compresses powder samples into tablets suitable for infrared and other spectral tests. The cap-opening gripper automatically grasps the reaction bottle cap and performs the screwing action. The filtration device filters the mixture using a syringe-type filter to remove insoluble particles. A mechanical quick-change tray allows the pretreatment unit to quickly switch between different end effectors according to task requirements, such as switching from a pipette tip to a cap-opening gripper. This modular, quickly switchable architecture enables the processing of multiple sample types. Precise and automated pretreatment ensures consistent sample quality, a prerequisite for the accuracy and repeatability of subsequent spectroscopic test data, and strongly supports the efficient operation of high-throughput parallel testing. The solid sampler balance positioning linear motion module and multi-specification pipettes equipped in the pretreatment workstation are specific implementations of the above modules.

[0042] In a specific implementation scenario, such as Figure 4 As shown, the pretreatment device integrates a small or large solid sampler with a balance positioning linear motion module, an automatic liquid transfer module, an ultrasonic mixing module, a cap-opening gripper, a tablet press, and a filtration device to perform related operations in coordination.

[0043] Furthermore, in S5, the cleaning is performed by an ultrasonic cleaner, the drying is performed by a dryer, the waste liquid treatment is performed by a liquid addition pump head, a liquid extraction pump head and a waste liquid monitoring module, and the material recycling is performed by a solid recycling unit.

[0044] Specifically, in S5, the post-processing unit comprises multiple modules. An ultrasonic cleaner efficiently cleans the inner and outer walls of containers such as reaction flasks, cuvettes, and NMR tubes using high-frequency vibration. A dryer rapidly removes moisture from the surfaces of the cleaned containers using hot air or infrared heating. A liquid injection pump and a liquid extraction pump are used to inject cleaning solution into the cleaning tank and discharge waste liquid into the processing pipeline, respectively. The cleaning solution system automatically manages the concentration and replacement cycle of the cleaning solution. A waste liquid monitoring module monitors the level and type of waste liquid in the waste liquid tank in real time and triggers discharge or warning signals. A solids collector collects discarded solid samples or filter residue after testing. The storage and monitoring module manages the cleaned and dried containers, preparing them for future use or return to storage. This achieves automated cleaning, drying, and recycling of containers, eliminating manual intervention. The automated post-processing process is a key link in achieving a continuous, high-throughput experimental closed loop, ensuring the reusability of containers and consumables and avoiding the delays and contamination risks introduced by manual cleaning. The liquid addition pump head, liquid extraction pump head, ultrasonic cleaning instrument, dryer, and reagent bottle placement structure configured in the post-processing workstation are the specific devices for performing the aforementioned cleaning, drying, and waste liquid treatment.

[0045] In a specific implementation scenario, such as Figure 6 As shown, the cleaning in the post-processing unit is performed by an ultrasonic cleaner, the drying is performed by a dryer, the waste liquid treatment is performed by a liquid addition pump head, a liquid extraction pump head and a waste liquid monitoring module, and the material recovery is performed by a solid recovery unit.

[0046] Furthermore, in S4, each spectroscopic testing workstation is equipped with a dedicated robotic arm, a sample tray placement station, a cover opening and closing gripper, and a rotating electric gripper to perform the automatic sample loading, testing, and unloading operations.

[0047] Specifically, to ensure fully automated testing, each spectroscopic workstation is equipped with a dedicated robotic arm, a sample tray placement station, a cap-opening gripper, and a rotating electric gripper. For example, in the NMR spectrometer workstation, after the sample tray is transferred to the workstation, the dedicated robotic arm first uses the rotating electric gripper to pick up an empty NMR tube and place it in the NMR tube slot of the sample injector. The robotic arm then switches to the cap-opening gripper and unscrews the reaction flask cap. The robotic arm then switches back to the rotating electric gripper to remove the NMR tube from the sample injector and insert it into the reaction flask, using negative pressure or capillary action to draw the sample solution into the NMR tube. After sample loading is complete, the robotic arm returns the NMR tube to the sample injector, and the workstation automatically starts the NMR test. After the test is completed, the robotic arm removes the NMR tube and discards it into the waste bin, completing the automated sample loading process. This process is implemented in similar ways on other workstations, including liquid chromatography and mass spectrometry workstations, but adapted to different container sizes, and will not be elaborated further. This achieves complete automation and unmanned operation of sample loading and unloading on different spectroscopic workstations. Automated sample loading and unloading is a key technology for breaking down the barriers between individual instruments and integrating them into a unified automated closed loop, making parallel testing of multiple spectrometers possible. The rotating grippers used in infrared spectrometer workstations for liquid mode operations, the fixed grippers used in tablet mode, and the rotating electrostatic grippers and fixed grippers used in liquid chromatography workstations for holding vials are all specific manifestations of this principle in different workstations.

[0048] In a specific implementation scenario, such as Figure 5 As shown, each spectroscopic testing workstation is equipped with a dedicated robotic arm, a sample tray placement station, a cover opening and closing gripper, and a rotating electric gripper to perform the automatic sample loading, testing, and unloading operations.

[0049] Furthermore, the overall control system module interacts with the automated storage device, preprocessing device, transmission system, postprocessing device, and each spectroscopic testing workstation through communication interface units that support SDK, HTTP, TCP / IP, and RS485 serial port protocols.

[0050] Specifically, to enable command issuance and status feedback between the central control system module and lower-level devices, including automated warehousing equipment, robotic arms at various workstations, and spectroscopic instruments, the communication interface unit integrates multiple protocols. For instruments with advanced programming interfaces, the SDK protocol is used for deep integration, directly calling their internal functions to set parameters and read data. For upper-level computer systems that support network communication, HTTP or TCP / IP protocols are used for data interaction. For older devices or those that only support serial communication, RS485 serial port protocol is used for conversion and communication. This multi-protocol support architecture ensures that devices from different manufacturers and eras can be incorporated into a unified control network. The unified communication interface is the nerve center for the central control system module to schedule the entire process of hardware and form an integrated closed-loop system, enabling devices with different protocols and eras to work collaboratively and achieving synchronous issuance of process commands and real-time collection of data feedback.

[0051] In a specific implementation scenario, such as Figure 7 As shown, the central control system module interacts with the automated storage device, preprocessing device, transmission system, postprocessing device, and various spectroscopic testing workstations through communication interface units that support SDK, HTTP, TCP / IP, and RS485 serial port protocols.

[0052] Furthermore, the high-throughput automated multispectral integrated experimental method supports high-throughput parallel testing of multiple samples, and supports mid-process material change, breakpoint continuation testing, and anomaly alarm.

[0053] The high-throughput automated multi-spectral integrated experimental method described in this invention supports high-throughput parallel testing of multiple samples. Through the scheduling algorithm of the central control system module, different samples can be assigned to different workstations for simultaneous processing. For example, when a batch of samples needs to undergo both infrared and Raman testing simultaneously, the experimental system divides the samples into two groups: one group is sent to the infrared workstation via a transmission system, and the other group is sent to the Raman workstation, with both groups executing in parallel. Furthermore, the experimental system supports mid-process material change and breakpoint continuation functions. When an abnormal result is found for a test sample, subsequent testing of that sample can be paused, other samples can be processed first, and the unfinished testing can continue after a new sample is added. The experimental system also has an anomaly alarm mechanism. When equipment malfunctions, consumables are insufficient, or data is abnormal, an alarm is automatically issued and a log is recorded, thereby significantly improving the working efficiency and robustness of the experimental system. It can handle non-ideal situations, and its high-throughput parallelism and anomaly handling capabilities are key to the experimental system's transition from a prototype to a practical and reliable commercial product. Existing automated systems are mostly rigid production lines; a problem in one link will cause the entire system to shut down. This invention, by introducing dynamic scheduling, mid-process material replacement, and breakpoint continuation testing mechanisms, endows the experimental system with the ability to handle unexpected events. This is a deepening of the unmanned closed-loop concept, enabling the closed loop to continue operating in more complex and realistic R&D environments. Its technical effects are significant.

[0054] In a specific implementation scenario, combined with Figure 2 and Figure 8 As shown, the system supports high-throughput parallel testing of multiple samples, and supports mid-process material change, breakpoint continuation testing, and anomaly alarms. Through the collaboration of various modules, it can achieve continuous operation under non-ideal conditions.

[0055] Furthermore, the present invention also proposes a high-throughput automated multispectral integrated experimental system, comprising: a central control software module, a storage management module, a preprocessing control module, a postprocessing control module, a transmission scheduling module, a multispectral driving module, a data management module, and a machine scientist interaction module; and an integrated experimental device for executing the high-throughput automated multispectral integrated experimental method.

[0056] Specifically, the experimental system consists of a central control software module, a storage management module, a pre-processing control module, a post-processing control module, a transmission scheduling module, a multi-spectral drive module, a data management module, and a machine scientist interaction module, as well as the aforementioned integrated experimental device. The central control software module, as the core brain of the experimental system, is responsible for task creation and template management, supports graphical process arrangement and simulation operation, and has priority scheduling and system-wide status monitoring functions. The storage management module digitally manages the inventory and location of containers, pallets, reagents, and consumables, corresponding to various items such as solid test samples, reagents, and consumables in the automated material station. The pre-processing control module and the post-processing control module precisely coordinate the sample preparation and cleaning processes, respectively controlling the specific operation of the pre-processing workstation and the post-processing workstation. The transmission scheduling module plans the optimal path for the ground-rail robotic arm and the magnetic levitation transmission line, and coordinates their actions. Its scheduling objects include ground-rail robotic arm No. 1, ground rail No. 2, and the robotic arm, as well as the solid hopper transfer area, reagent bottle transfer area, and pallet transfer station they serve. The multi-spectral drive module provides unified control, parameter distribution, and result collection for various spectroscopic instruments. Its driving range includes all functional workstations such as infrared, liquid chromatography, photoreactive gas chromatography and electrochemistry, ultraviolet, Raman, circular dichroism, high-resolution mass spectrometry, circular polarization, nuclear magnetic resonance, fluorescence, and gas chromatography-mass spectrometry. The data management module is responsible for the storage, querying, and exporting of spectra, logs, and time-series data. The machine scientist interaction module receives experimental instructions from external AI systems through multi-protocol interfaces and provides feedback on experimental results. Its modular design enables closed-loop management from task distribution to data feedback. The integration of these software modules and hardware devices constitutes the physical and logical entity for achieving a high-throughput, automated, and AI-coordinated experimental closed loop. Unlike the decentralized, fragmented, stand-alone automation of existing technologies, this invention constructs a software-to-hardware collaborative architecture including a machine scientist interaction module. It embeds AI decision-making logic into the beginning (task distribution) and end (result feedback) of the experimental process, forming a closed loop from AI-designed experiments to automatic system execution and data feedback to AI. This fundamental difference in architecture makes this experimental system not only an automation tool, but also an intelligent platform that can collaborate with AI and achieve self-iterative research and development. The effects it brings are unparalleled by existing automation solutions and discrete systems.

[0057] In a specific implementation scenario, such as Figure 8 As shown, the high-throughput automated multispectral integrated experimental system includes a central control software module, a storage management module, a preprocessing control module, a postprocessing control module, a transmission scheduling module, a multispectral driving module, a data management module, and a machine scientist interaction module.

[0058] Furthermore, the multi-spectral driving module supports the automatic execution of various standardized full-processes, including ultraviolet full-process, electrochemical full-process, photoreaction full-process, NMR full-process, infrared full-process, Raman full-process, liquid chromatography full-process, fluorescence full-process, circular dichroism full-process, circular polarization full-process, and mass spectrometry full-process.

[0059] Specifically, this experimental system supports the automated execution of various standardized full-process workflows. Each full-process workflow corresponds to a preset standardized formula, which defines the specific parameters for each step from S1 to S6, including pipetting volume, ultrasonic time, tablet pressure, test wavelength range, and cleaning procedure. Users only need to select the desired workflow type and specify the sample, and the experimental system can automatically complete all operations. For example, after selecting the UV full-process workflow, the experimental system will automatically configure the pipetting volume, select the appropriate cuvette, set the scanning range and integration time of the UV spectrometer, and execute the preset cleaning scheme. The standardized full-process design greatly simplifies the operation and ensures the reproducibility of experimental results across different batches. Standardized full-process workflows are essential for achieving high-throughput, unmanned operation. It encapsulates complex, multi-step experimental processes into a one-click executable formula, eliminating the operational variability of manually configured parameters, and making the output of the entire closed-loop process highly consistent and predictable. For example: In the UV workflow, after sample preparation via pretreatment, it is magnetically levitated to the UV measurement station, then magnetically levitated to the HPLC station for opening and other operations. A ground-rail system takes a cuvette to the HPLC station for capping, and finally, the ground-rail system takes the cuvette to the post-processing cleaning station. In the electrochemical workflow, after pretreatment solution preparation, a ground-rail system takes a 100mL reaction flask tray to the magnetic levitation system, which then takes it to the electrochemical station. After measurement, the magnetic levitation system takes the tray to the post-processing cleaning station. In the photoreaction workflow, an 8mL reaction flask is taken from the ground-rail system to the pretreatment solution preparation station, then magnetically levitated to the HPLC station for capping, and finally to the post-processing cleaning station. In the NMR workflow, consumables such as tip tubes, stock solution bottles, and NMR tubes are shipped out in batches. In the infrared workflow, the coordinated scheduling of materials such as tip tubes and swabs is involved, with multiple transfers between different workstations via ground-rail and magnetic levitation systems. In the Raman workflow, the magnetic levitation system directly delivers the sample tray to the Raman spectroscopy station for measurement. In the complete liquid chromatography (LC) workflow, reaction flask trays, stock solution bottles, LC bottles, and syringes are shipped out in three batches, with pretreatment solution preparation and injection processes alternating. In the complete fluorescence and circular polarization (CNP) workflows, after the pretreatment tip and stock solution bottle are shipped out, the cuvette transport path involves coordination between the CNP station and the LC station. In the complete circular polarization workflow, after pretreatment solution preparation, the cuvettes undergo multiple steps including opening and closing the cap, magnetic levitation transport, opening the cap at the LC station, and post-processing cleaning. In the complete mass spectrometry (MS) workflow, reaction flask trays, stock solution bottles, mass spectrometer bottles, and syringes are also shipped out in batches, with magnetic levitation and ground rails handling transport between the mass spectrometry station, pretreatment, and post-processing stations.

[0060] In a specific implementation scenario, such as Figure 8 As shown, the multi-spectral driving module supports the automatic execution of various standardized full-processes, including ultraviolet full-process, electrochemical full-process, photoreaction full-process, NMR full-process, infrared full-process, Raman full-process, liquid chromatography full-process, fluorescence full-process, circular dichroism full-process, circular polarization full-process, and mass spectrometry full-process.

[0061] The present invention also proposes a computer-readable storage medium storing a computer program thereon, which, when executed by a processor, implements the steps of the high-throughput automated multispectral integrated experimental method described above.

[0062] Specifically, a computer-readable storage medium stores a computer program that, when executed by a processor, implements the steps of the aforementioned high-throughput automated multispectral integrated experimental method. This storage medium includes a hard disk, a solid-state drive, a server cluster storage array, or cloud storage space. When the program runs on a central control computer or server, it loads and executes all steps S1 to S6 of the aforementioned high-throughput automated multispectral integrated experimental method, driving the automated storage device, pre-processing device, transmission system, multispectral testing workstation, and post-processing device to work collaboratively, achieving fully automated and intelligent operation.

[0063] In a specific implementation scenario, combined with Figure 2 and Figure 7 As shown, when the program on the computer-readable storage medium is executed by the processor, the drive control system module and various hardware devices work together to execute the above-mentioned full process steps.

[0064] The above are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A high-throughput automated multispectral integrated experimental method, characterized in that, include: S1. The central control system module issues experimental tasks and drives the automated warehousing device to scan and release consumables, reagents, samples and containers, and analyze consumables. S2. The pretreatment device performs solid injection, liquid transfer, dilution, ultrasonic mixing, cap opening and closing, tablet pressing and filtration operations on the outgoing materials to complete sample preparation. S3. The tray carrying the processed sample is automatically transported to the designated spectroscopic testing workstation through a transmission system consisting of a ground-rail robotic arm and a magnetic levitation transmission line. S4. Each spectroscopic testing workstation independently completes automatic sample loading, parameter configuration, data acquisition and automatic sample unloading, realizing parallel testing of at least multiple spectroscopic methods including ultraviolet, infrared, Raman, fluorescence, circular dichroism, circular polarization, nuclear magnetic resonance, electrochemistry, photocatalysis, liquid chromatography, high-resolution mass spectrometry and gas chromatography-mass spectrometry. S5. The post-processing unit performs cleaning, drying, waste liquid treatment and material recycling operations on the tested containers and trays. S6. The recycled empty containers and pallets are automatically returned to the warehouse by the automated storage device, and the experimental parameters, operation logs, spectroscopic data and time scales are recorded throughout the process by the central control system module, forming traceable closed-loop data.

2. The high-throughput automated multispectral integrated experimental method according to claim 1, characterized in that, In S1, the automated warehousing device specifically performs QR code scanning for inbound and outbound operations and real-time inventory monitoring operations.

3. The high-throughput automated multispectral integrated experimental method according to claim 1, characterized in that, In step S2, the solid sample injection is performed by a small solid sampler or a large solid sampler in conjunction with a balance positioning linear motion module; the liquid pipetting is performed by an automatic pipetting module; the ultrasonic mixing is performed by an ultrasonic mixing module; the cap opening and closing is performed by a cap opening and closing gripper; the tableting is performed by a tablet press; and the filtration is performed by a filtration device.

4. The high-throughput automated multispectral integrated experimental method according to claim 1, characterized in that, In step S5, the cleaning is performed by an ultrasonic cleaner, the drying is performed by a dryer, the waste liquid treatment is performed by a liquid addition pump head, a liquid extraction pump head and a waste liquid monitoring module, and the material recycling is performed by a solid recycling unit.

5. The high-throughput automated multispectral integrated experimental method according to claim 1, characterized in that, In S4, each spectroscopic testing workstation is equipped with a dedicated robotic arm, a sample tray placement station, a cover opening and closing gripper, and a rotating electric gripper to perform the automatic sample loading, automatic sample testing, and automatic sample unloading operations.

6. The high-throughput automated multispectral integrated experimental method according to claim 1, characterized in that, The central control system module interacts with the automated storage device, preprocessing device, transmission system, postprocessing device, and each spectroscopic testing workstation via communication interface units that support SDK, HTTP, TCP / IP, and RS485 serial port protocols.

7. The high-throughput automated multispectral integrated experimental method according to claim 1, characterized in that, It supports high-throughput parallel testing of multiple samples, and also supports mid-process material change, breakpoint continuation testing, and anomaly alarms.

8. A high-throughput automated multispectral integrated experimental system, characterized in that, include: The system includes a central control software module, a warehouse management module, a pre-processing control module, a post-processing control module, a transmission scheduling module, a multi-spectral drive module, a data management module, and a machine scientist interaction module. And an integrated experimental apparatus for performing the high-throughput automated multispectral integrated experimental method according to any one of claims 1 to 7.

9. The experimental system according to claim 8, characterized in that, The multi-spectral driving module supports the automatic execution of various standardized full-processes, including ultraviolet full-process, electrochemical full-process, photoreaction full-process, NMR full-process, infrared full-process, Raman full-process, liquid chromatography full-process, fluorescence full-process, circular dichroism full-process, circular polarization full-process, and mass spectrometry full-process.

10. A computer-readable storage medium having a computer program stored thereon, which, when executed by a processor, implements the steps of the high-throughput automated multispectral integrated experimental method as described in any one of claims 1 to 7.

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