Extraction separation device
By designing an extraction and separation device for fuel and material analysis, the problems of large manpower demand and radioactive exposure are solved, and the automated separation of uranium substrates is achieved, and efficiency and safety are improved.
Patent Information
- Application Number
- CN202510570220.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-06
- Publication Date
- 2025-06-03
- Estimated Expiration
- 2045-05-06
AI Technical Summary
There is a large demand for manpower in fuel and material analysis, which affects work progress and efficiency, and is prone to contamination of the laboratory environment and radioactive exposure to the human body.
An extraction and separation device is designed, including a body, a robotic arm, a liquid filling assembly, a pipetting assembly, a pressurization device and a receiving assembly, and the fully automated separation of the uranium matrix and impurity elements through collaborative work.
The automatic separation of uranium matrix in fuel components is achieved, reducing human operation errors, improving separation work efficiency, reducing labor costs, and avoiding environmental and human radiocontamination.
Smart Images

Figure CN120084622A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of extraction and separation, and more particularly, to an extraction and separation device. Background Art
[0002] The physical and chemical properties, composition content and distribution of fuel elements are closely related to the core power distribution. The content of impurity elements (such as cadmium, chromium, gadolinium, samarium, thorium, molybdenum, tin, dysprosium, europium, etc.) in the fuel will directly affect the safety performance of the reactor. Usually, chromatographic separation method is used to separate impurity elements. However, the chromatographic separation method has problems such as cumbersome process, long time consumption, high manpower requirement, which seriously affects the work progress and efficiency. In addition, fuel elements usually contain a large amount of uranium. During the manual separation process, it is not only easy to cause laboratory environment contamination, but also easy to cause human radioactive exposure.
[0003] Therefore, how to overcome the above defects has become an urgent problem to be solved. Summary of the Invention
[0004] In order to solve the technical problems of high manpower requirement in fuel and material analysis, which affects the work progress and efficiency, and is also easy to cause laboratory environment contamination and human radioactive exposure, this application proposes an extraction and separation device.
[0005] In view of this, this application proposes an extraction and separation device for the automated separation of uranium matrix in fuel and material analysis, including: a main body, on which a sample tray, a reagent bottle and an extraction column tray are arranged. The extraction column tray is provided with a plurality of separation columns, and the separation columns are used for the selective adsorption and separation of uranium matrix and impurity elements; a first robotic arm arranged on the main body; a liquid addition assembly arranged on the first robotic arm, and the liquid addition assembly is used to take liquid from the reagent bottle and perform the liquid addition operation; a pipetting assembly arranged on the first robotic arm, and the pipetting assembly is used to take samples from the sample tray and perform the sample loading operation; a second robotic arm arranged on the main body; a pressurizing device arranged on the second robotic arm, and the pressurizing device is used to perform a sealing and pressurizing operation on the separation column; a receiving assembly arranged on the main body, and the receiving assembly can move relative to the main body, and the receiving assembly is used to collect sample solutions and waste liquids.
[0006] The extraction and separation device provided by this application includes a main body, a first robotic arm, a liquid addition assembly, a pipetting assembly, a second robotic arm, a pressurizing device and a receiving assembly. Each component realizes the fully automated operation of separating uranium matrix and impurity elements through collaborative work.
[0007] Samples to be processed are stored in the sample tray, and reagents for extraction and separation are stored in the reagent bottle. Each reagent is stored separately. The extraction column tray is integrated with a plurality of separation columns, supporting batch separation and processing of samples. The separation columns are filled with specific adsorption materials (such as TBP resin or extraction resin), and selectively adsorb uranium at a specific acidity to separate impurity elements in the extraction material matrix.
[0008] The first robotic arm and the second robotic arm cooperate with each other in division of labor. The liquid addition component and the pipetting component can move with the first robotic arm, and the pressurizing device can move with the second robotic arm. The first robotic arm is responsible for liquid operations (liquid addition / pipetting / sampling / sample loading). It precisely controls the accurate addition of reagents through the liquid addition component and realizes the quantitative transfer of samples to be processed through the pipetting component. The second robotic arm accelerates the diffusion and binding of uranyl ions in the adsorption material by applying a controllable pressure to the separation column, thereby shortening the separation time.
[0009] The receiving component adopts a movable design, automatically locates according to the position of the separation column, and realizes the classified collection of sample solutions and waste liquids.
[0010] For the extraction and separation device provided by this application, all processes such as sample loading, elution, elution, reception, volume determination, and classified collection of waste liquids are automatically completed. The whole process is controlled by the first robotic arm, the second robotic arm, and a program, reducing human operation errors, improving the separation work efficiency, reducing labor costs, and avoiding environmental radioactive pollution and human radioactive damage.
[0011] In some technical solutions, optionally, the liquid addition component includes: a plurality of syringe pumps arranged on the first robotic arm, and the plurality of syringe pumps are used to draw liquid from reagent bottles and add the liquid to the separation column; activation liquid, eluent, and elution liquid are stored in the reagent bottles; a pressure regulating structure is arranged on the syringe pump and is used to control the liquid drawing speed and the liquid addition speed.
[0012] In some technical solutions, optionally, the liquid addition component further includes: a reagent pipeline group, the reagent pipeline group includes multiple pipelines, one end of each pipeline is respectively connected to the syringe pump, and each pipeline is respectively used for the addition of different reagents; a multi-way control valve is connected to all pipelines of the reagent pipeline group, and realizes the selective flow of different reagents through valve position switching.
[0013] In some technical solutions, optionally, the pipetting component includes: a plurality of samplers arranged on the first robotic arm, and the plurality of samplers can realize the sampling and sample loading operations of multiple samples.
[0014] In some technical solutions, optionally, the number of the second robotic arms is at least two, and the at least two second robotic arms are arranged oppositely; at least one pressurizing device is arranged on each second robotic arm.
[0015] In some technical solutions, optionally, the receiving component includes a sample receiving tray and a waste liquid collection tank. The extraction and separation device further includes: a guide rail arranged below the sample receiving tray and the waste liquid collection tank, the sample receiving tray can move along the guide rail for receiving sample solutions, and the waste liquid collection tank can move along the guide rail for receiving waste liquids.
[0016] In some technical solutions, optionally, the pressurizing device includes: an air circuit disposed on the second robotic arm for adjusting the air pressure in the separation column; a sealing layer disposed on the air circuit for sealing the air circuit; and a sealing cover disposed on the second robotic arm for sealing the outer opening of the separation column.
[0017] In some technical solutions, optionally, the extraction and separation device further includes: a waste liquid bottle including a first waste liquid bottle and a second waste liquid bottle for storing different waste liquids; and a peristaltic pump disposed on the main body for pumping the waste liquid collected by the waste liquid collection tank to the waste liquid bottle.
[0018] In some technical solutions, optionally, the extraction and separation device further includes: a control system connected to the first robotic arm, the liquid adding assembly, the liquid transferring assembly, the second robotic arm, the pressurizing device, and the receiving assembly, and the control system is capable of sending control instructions to the first robotic arm, the liquid adding assembly, the liquid transferring assembly, the second robotic arm, the pressurizing device, and the receiving assembly.
[0019] In some technical solutions, optionally, the first robotic arm and the second robotic arm are two-axis robotic arms, and the surfaces of the first robotic arm and the second robotic arm are coated with an anti-corrosion material layer.
[0020] Compared with the prior art, the present application has the following technical effects: The extraction and separation device provided by the present application can automatically extract and separate impurity elements in fuel elements, and is used to realize the automatic separation of uranium matrix in various fuel and material analyses. Based on a high-precision injection pump, activation liquid, eluent, and elution liquid are accurately added, and a pipette gun type liquid transferring and adding module is used for the full transfer and sampling of the sample solution. The gun head is automatically picked and removed, realizing the automatic completion of the whole process such as automatic sampling, elution, elution, reception, constant volume, and waste liquid classification collection.
[0021] The additional aspects and advantages of the present application will become apparent in the following description section or be learned through the practice of the present application. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] The above and / or additional aspects and advantages of the present application will become apparent and be readily understood from the description of the embodiments in conjunction with the following drawings, in which: Figure 1 The structural schematic diagram of the extraction and separation device according to an embodiment of the present application is shown; Figure 2 The system flow path schematic diagram of the extraction and separation device according to an embodiment of the present application is shown; Figure 3 The structural schematic diagram of the extraction and separation device according to another embodiment of the present application is shown; Figure 4Shows a schematic structural diagram of a first robotic arm according to an embodiment of the present application; Figure 5 Shows a schematic diagram of the sample loading state of the first robotic arm according to an embodiment of the present application; Figure 6 Shows a schematic structural diagram of a receiving component according to an embodiment of the present application; Figure 7 Shows a schematic structural diagram of a waste tip box of the receiving component according to an embodiment of the present application; Figure 8 Shows Figure 3 A schematic structural diagram of the open lid state of the extraction and separation device of the illustrated embodiment; Figure 9 Shows an elution curve diagram of the automatic separation of uranium matrix by the extraction and separation device according to an embodiment of the present application.
[0023] Wherein, Figures 1 to 8 The corresponding relationship between the reference numerals and the component names in the figure is as follows: 100 extraction and separation device, 110 main body, 112 sample tray, 114 reagent bottle, 116 extraction column tray, 118 tip box, 119 waste tip box, 120 first robotic arm, 130 liquid addition component, 132 injection pump, 136 reagent pipeline group, 138 multi-way control valve, 140 pipetting component, 142 sampler, 150 second robotic arm, 160 pressurizing device, 166 sealing cover, 170 receiving component, 172 sample receiving tray, 174 waste liquid collection tank, 180 guide rail, 190 peristaltic pump, 192 waste liquid bottle. Detailed implementation manners
[0024] In order to more clearly understand the above objects, features and advantages of the present application, the present application will be further described in detail below with reference to the drawings and specific implementation manners. It should be noted that, without conflict, the embodiments of the present application and the features in the embodiments can be combined with each other.
[0025] Many specific details are set forth in the following description in order to fully understand the present application. However, the present application may also be implemented in other ways different from those described herein. Therefore, the protection scope of the present application is not limited by the specific embodiments disclosed below.
[0026] Next, refer to Figures 1 to 9 Describe the extraction and separation device 100 according to some embodiments of the present application.
[0027] As Figure 1 、 Figure 3 And Figure 8As shown in the figure, the present application proposes an extraction and separation device 100 for the automated separation of uranium matrix in fuel and material analysis, including: a main body 110, on which a sample tray 112, reagent bottles 114 and an extraction column tray 116 are arranged. The extraction column tray 116 is provided with a plurality of separation columns, which are used for the selective adsorption and separation of uranium matrix and impurity elements; a first robotic arm 120, arranged on the main body 110; a liquid addition assembly 130, arranged on the first robotic arm 120, and the liquid addition assembly 130 is used to take liquid from the reagent bottle 114 and perform the liquid addition operation; a pipetting assembly 140, arranged on the first robotic arm 120, and the pipetting assembly 140 is used to take samples from the sample tray 112 and perform the sample loading operation; a second robotic arm 150, arranged on the main body 110; a pressurizing device 160, arranged on the second robotic arm 150, and the pressurizing device 160 is used to perform a sealing and pressurizing operation on the separation column; a receiving assembly 170, arranged on the main body 110, and the receiving assembly 170 can move relative to the main body 110, and the receiving assembly 170 is used to collect sample solutions and waste liquids.
[0028] The extraction and separation device 100 provided by the present application includes a main body 110, a first robotic arm 120, a liquid addition assembly 130, a pipetting assembly 140, a second robotic arm 150, a pressurizing device 160 and a receiving assembly 170. Each component realizes the fully automated operation of uranium matrix separation through collaborative work.
[0029] Samples to be processed are stored in the sample tray 112, and reagents for extraction and separation are stored in the reagent bottles 114. Each reagent is stored separately. The extraction column tray 116 is integrated with a plurality of separation columns, supporting batch separation processing of samples. The separation columns are filled with specific adsorption materials (such as TBP resin or extraction resin), and selectively adsorb uranium at a specific acidity to separate impurity elements in the extraction material matrix.
[0030] The first robotic arm 120 and the second robotic arm 150 cooperate with each other. The liquid addition assembly 130 and the pipetting assembly 140 can move with the first robotic arm 120, and the pressurizing device 160 can move with the second robotic arm 150. The first robotic arm 120 is responsible for liquid operations (liquid addition / pipetting / sampling / sample loading), accurately controlling the accurate addition of reagents through the liquid addition assembly 130, and realizing the quantitative transfer of samples to be processed through the pipetting assembly 140; the second robotic arm 150 accelerates the diffusion and binding of uranyl ions in the adsorption material by applying a controllable pressure to the separation column, shortening the separation time.
[0031] The receiving assembly 170 adopts a movable design, automatically locates according to the position of the separation column, and realizes the classified collection of sample solutions and waste liquids.
[0032] The extraction and separation device 100 provided by this application can automatically complete the entire process, including sample loading, elution, elution, reception, volume determination, and waste liquid classification collection. The whole process is completed by the first robotic arm 120, the second robotic arm 150, and program control, reducing human operation errors, improving separation work efficiency, reducing labor costs, and avoiding environmental radioactive pollution and human radioactive damage.
[0033] In some embodiments, optionally, as Figure 2 shown, the liquid addition assembly 130 includes: a plurality of syringe pumps 132 disposed on the first robotic arm 120. The plurality of syringe pumps 132 are used to draw liquid from the reagent bottle 114 and add the liquid to the separation column. The reagent bottle 114 stores an activation solution, an eluent, and an elution solution. A pressure regulating structure is disposed on the syringe pump 132 for controlling the liquid drawing speed and the liquid addition speed.
[0034] In this embodiment, the liquid addition assembly 130 includes a plurality of syringe pumps 132 and a pressure regulating structure. The reagent bottle 114 stores an activation solution, an eluent, and an elution solution. The delivery process of the reagent is accurately controlled by the syringe pump 132 and the pressure regulating structure to ensure the efficiency and reliability of uranium matrix separation.
[0035] Each syringe pump 132 can independently control the addition of different reagents (such as activation solution, eluent, elution solution) through different lines, avoiding cross-contamination between different reagents.
[0036] By adjusting the pressure output of the pressure regulating structure (such as pneumatic drive or electric plunger), accurate control of the liquid drawing speed (drawing liquid from the reagent bottle 114) and the liquid addition speed (injecting liquid into the separation column) is achieved.
[0037] The pressure regulating structure can integrate a pressure sensor to real-time monitor the pipeline resistance, automatically adjust the pressurization parameters, and prevent the risk of liquid leakage caused by pipeline blockage or too high column pressure.
[0038] The interior of the reagent bottle 114 adopts an independent liquid storage design, and the reagent type and expiration date are identified through labels or two-dimensional codes to achieve automatic identification and scheduling. When the reagent remaining amount is lower than the threshold, the system automatically triggers an alarm and generates a replenishment list.
[0039] For easily deteriorated reagents, the reagent bottle 114 can integrate a micro refrigeration module to maintain the storage environment temperature and extend the service life of the reagent.
[0040] Through the mobility of the first robotic arm 120, the accuracy of the syringe pump 132, and the controllability of the pressure regulating structure, the liquid addition assembly 130 realizes the full automation and intelligence of the separation process, significantly improving the reliability, repeatability, and analysis throughput of uranium matrix analysis.
[0041] In some embodiments, optionally, as Figure 2As shown, the liquid addition assembly 130 further includes: a reagent pipeline group 136, which includes multiple pipelines. One end of each pipeline is respectively connected to the injection pump 132, and each pipeline is used for adding different reagents; a multi-way control valve 138, which is connected to all the pipelines of the reagent pipeline group 136, and realizes the selective flow of different reagents through valve position switching.
[0042] In this embodiment, the liquid addition assembly 130 further includes a reagent pipeline group 136 and a multi-way control valve 138. The reagent pipeline group 136 includes multiple pipelines, which can realize the parallel management of multiple reagents.
[0043] The number of the reagent pipeline groups 136 is the same as the number of the injection pumps 132. Each pipeline of a single reagent pipeline group 136 is independently connected to a specific reagent storage tank in the reagent bottle 114, forming a physically isolated liquid channel, which can avoid cross-contamination between different reagents.
[0044] The number of pipelines can be flexibly expanded according to requirements, supporting the parallel use of more types of reagents and adapting to complex separation processes.
[0045] The multi-way control valve 138 can accurately control the flow direction of the reagent. By rotating the valve core or electromagnetic drive, the multi-way control valve 138 can switch the valve position, connect the target reagent pipeline to the separation column, and keep other pipelines closed.
[0046] If a certain pipeline is blocked or leaks, the multi-way control valve 138 can immediately close this passage and trigger an alarm to prevent the contamination from spreading to other reagents or the separation column.
[0047] Through the synergistic effect of the reagent pipeline group 136 and the multi-way control valve 138, accurate control of reagent delivery, high automation of the process, and significant improvement of the analysis throughput are achieved.
[0048] In some embodiments, optionally, as Figure 1 、 Figure 4 and Figure 5 shown, the liquid transfer assembly 140 includes: a multi-channel sampler 142, which is arranged on the first robotic arm 120, and the multi-channel sampler 142 can realize the sampling and loading operations of multiple samples.
[0049] In this embodiment, the liquid transfer assembly 140 includes a multi-channel sampler 142. The multi-channel sampler 142 can load multiple pipette tips at one time and synchronously aspirate the samples in the sample tray 112. After sampling, the first robotic arm 120 directly moves above the separation column to achieve seamless connection of "sampling - moving - loading".
[0050] Relying on the closed-loop control system of the first robotic arm 120, the sampling pipette tips can be accurately positioned to avoid liquid droplet residue or cross-contamination. As Figure 7As shown, after sample loading is completed, automatic tip ejection can be achieved. It is driven and controlled by a motor to automatically control the tip ejection action, with small mechanical stress and stable structure. The discarded tips can be automatically placed into the waste tip box 119.
[0051] Through the cooperation of the multi-channel sampler 142 and the first robotic arm 120, the efficiency, accuracy, and process automation of sample processing are achieved.
[0052] In some embodiments, optionally, as Figure 1 shown, the number of the second robotic arms 150 is at least two, and at least two second robotic arms 150 are arranged oppositely; at least one pressurizing device 160 is arranged on each second robotic arm 150.
[0053] In this embodiment, the number of the second robotic arms 150 is at least two, and at least one pressurizing device 160 is arranged on each second robotic arm 150.
[0054] At least two second robotic arms 150 are arranged oppositely and can be independently applied to different extraction column trays 116. This doubles the throughput of a multi-column separation system (such as a 4-column or 8-column system) and improves the analysis throughput.
[0055] The oppositely arranged robotic arms can form a "mirror" motion trajectory in a limited space, reducing the risk of collision between the robotic arms while expanding the operation coverage.
[0056] Each second robotic arm 150 is equipped with at least one pressurizing device 160, and the pressurizing device 160 can independently adjust the working pressure of the corresponding separation column. The pressurizing device 160 supports programmed pressure changes to adapt to the requirements of the separation process. Through the cooperation and independent pressure control of at least two second robotic arms 150, the efficiency, flexibility, and scalability of the separation system are achieved.
[0057] In some embodiments, optionally, as Figure 1 and Figure 6 shown, the receiving component 170 includes a sample receiving tray 172 and a waste liquid collection tank 174. The extraction and separation device 100 further includes: a guide rail 180, which is arranged below the sample receiving tray 172 and the waste liquid collection tank 174. The sample receiving tray 172 can move along the guide rail 180 for receiving the sample solution, and the waste liquid collection tank 174 can move along the guide rail 180 for receiving the waste liquid.
[0058] In this embodiment, the receiving component 170 includes a sample receiving tray 172 and a waste liquid collection tank 174. A guide rail 180 is provided below the sample receiving tray 172 and the waste liquid collection tank 174. The sample receiving tray 172 moves along the guide rail 180 and can be accurately positioned at the sample solution output position. The waste liquid collection tank 174 moves along the guide rail 180 and dynamically adjusts its position according to the waste liquid generation rate. Each separation column is allocated an independent waste liquid tank to avoid cross-contamination. The waste liquid tank is equipped with a weighing sensor or an infrared liquid level gauge to monitor the waste liquid volume in real time. When the preset threshold is reached, a reminder is issued.
[0059] Automatic waste liquid management reduces the risk of manual contact with harmful reagents and decreases the probability of laboratory accidents. The sample receiving tray 172 and the waste liquid collection tank 174 can be moved to the edge of the device in the non-working state, facilitating device maintenance. Through the design of the guide rail 180 type receiving component 170, flexible management, intelligent monitoring, and efficient processing of samples and waste liquid are achieved.
[0060] In some embodiments, optionally, as Figure 1 and Figure 3 shown, the pressurizing device 160 includes: a gas path provided in the second robotic arm 150 for adjusting the air pressure inside the separation column; a sealing layer provided in the gas path for sealing the gas path; and a sealing cover 166 provided in the second robotic arm 150 for sealing the outer opening of the separation column.
[0061] In this embodiment, the pressurizing device 160 includes a gas path, a sealing layer, and a sealing cover 166. The gas path adjusts the gas flow through a solenoid valve or a proportional valve to achieve precise control of the pressure inside the separation column. The gas path sealing layer forms a compression seal at the gas path interface to prevent gas leakage, ensure pressure stability, and avoid pressure fluctuations affecting the separation effect.
[0062] The separation column sealing cover 166 is provided at the end of the robotic arm and is realized through pneumatic or electric drive. After moving to the position of the separation column, it can quickly dock with the column opening of the separation column to complete the sealing. The automatic opening and closing of the sealing cover 166 reduces the risk of manual contact with the high-temperature and high-pressure column body. Through the dynamic control of the gas path and the double-sealing design, the efficiency, safety, and scalability of the separation system are achieved.
[0063] As Figure 8 shown, in some embodiments, optionally, the extraction and separation device 100 further includes: a waste liquid bottle 192, the waste liquid bottle 192 includes a first waste liquid bottle and a second waste liquid bottle for storing different waste liquids; a peristaltic pump 190 provided in the main body 110, and the peristaltic pump 190 is used to pump the waste liquid collected by the waste liquid collection tank 174 to the waste liquid bottle 192.
[0064] In this embodiment, the extraction and separation device 100 further includes: a waste liquid bottle 192 and a peristaltic pump 190. The waste liquid bottle 192 is made of corrosion-resistant material. The waste liquid bottle 192 is internally provided with a capacitive or ultrasonic liquid level sensor. When the waste liquid volume approaches the capacity threshold, the warning system is automatically triggered to notify the operator to replace the waste liquid bottle 192.
[0065] Specifically, the first waste liquid bottle is used to store uranium-containing waste liquid, and the second waste liquid bottle is used to store uranium-free waste liquid, so as to realize the separate discharge of uranium-containing waste liquid and uranium-free waste liquid, and minimize radioactive waste.
[0066] The peristaltic pump 190 generates negative pressure by compressing the elastic hose, and pumps the waste liquid from the collection tank to the waste liquid bottle 192, avoiding direct contact between the pump body and the corrosive waste liquid and extending the service life of the equipment. By adjusting the pump head speed or the inner diameter of the hose, precise control of the waste liquid flow rate can be achieved.
[0067] The peristaltic pump 190 is equipped with a one-way valve to prevent the waste liquid from flowing back to the collection tank when the machine stops, ensuring the one-way flow of the waste liquid. Through the safe storage of the waste liquid bottle 192 and the precise delivery of the peristaltic pump 190, the efficiency, safety and compliance of waste liquid management are realized.
[0068] In some embodiments, optionally, the extraction and separation device 100 further includes: a control system, which is connected to the first robotic arm 120, the liquid adding assembly 130, the pipetting assembly 140, the second robotic arm 150, the pressurizing device 160 and the receiving assembly 170. The control system can send control instructions to the first robotic arm 120, the liquid adding assembly 130, the pipetting assembly 140, the second robotic arm 150, the pressurizing device 160 and the receiving assembly 170.
[0069] In this embodiment, the extraction and separation device 100 further includes: a control system, which is controlled by a computer program, has high control precision, good stability and is very convenient to operate and use.
[0070] The control system can realize the coordinated control of multiple components, full-process automation, and coordinate the actions of the first robotic arm 120 (sample transfer), the liquid adding assembly 130 (reagent addition), the pipetting assembly 140 (accurate sampling), the second robotic arm 150 (separation column pressurization operation), the pressurizing device 160 (pressure regulation) and the receiving assembly 170 (sample / waste liquid collection).
[0071] The control system adopts a dynamic scheduling algorithm to adjust the action timing in real time according to the operating states of each component. For example, while the liquid adding assembly 130 injects the reagent, the first robotic arm 120 pre-loads the next sample to reduce the waiting time.
[0072] Collect the operating parameters of each component in real time (such as the position of the robotic arm, the pressure value, the liquid level height), and display the system status through the dashboard interface. Pressure warning: When the pressure in the separation column exceeds the set threshold, an alarm is automatically triggered and the experiment is paused; Liquid level monitoring: When the waste liquid collection tank 174 is close to full, it automatically switches to the standby tank position. Precisely control the actions of each component (such as the positioning accuracy of the robotic arm, the pressure control accuracy). Through the integrated design of the control system, the high automation, intelligence and informatization of the pressurizing device 160 are realized.
[0073] In some embodiments, optionally, the first robotic arm 120 and the second robotic arm 150 are two-axis robotic arms, and the surfaces of the first robotic arm 120 and the second robotic arm 150 are coated with an anti-corrosion material layer.
[0074] In this embodiment, the two-axis robotic arm can be driven by a stepper motor or a servo motor to achieve precise positioning in a set plane (for example: a horizontal plane). The precise positioning and motion optimization of the two-axis robotic arm improve the transfer speed of samples and reagents, meeting the requirements of high-throughput separation.
[0075] The control system uses a path planning algorithm to avoid collisions during the movement of multiple robotic arms and improve the action efficiency. The first robotic arm 120 and the second robotic arm 150 are integrally coated with a PVC (polyvinyl chloride) anti-corrosion material, which can effectively avoid the corrosion of acid solution.
[0076] Through the precise motion control of the two-axis robotic arm and the chemical protection of the anti-corrosion material layer, the high efficiency, stability and durability of the separation system are realized.
[0077] In a specific embodiment, as Figure 2 shown, the system flow path uses eight high-precision syringe pumps 132 (P1, P2... P8) to perform liquid addition and liquid transfer operations, and the liquid path tubes are made of 1 / 8 PTFE (polytetrafluoroethylene) tubes; Pressurization is carried out by providing gas through a separate gas path. The P1-P8 syringe pumps 132 use 10-ml syringes to provide power for liquid suction. The multi-way control valve 138 is used to switch reagents such as activation liquid, elution liquid and washing liquid. The flow rate through the column is controlled by the gas path.
[0078] As Figure 1 shown, the present application uses one first robotic arm 120 and two second robotic arms 150, and all three robotic arms are two-axis robotic arms. The robotic arms are integrally coated with a PVC anti-corrosion material, which can effectively avoid the corrosion of acid solution.
[0079] The first robotic arm 120 integrates a liquid addition module (liquid addition component 130) and a pipetting module (pipetting component 140). Among them, the liquid addition module includes 8 injection pump pipelines and a sealed pressure regulation and speed control structure (pressure regulation structure). The 8 pipelines independently add reagents, can support the independent addition of different reagents such as eluent and eluate, and can achieve the overall or individual liquid addition function. The liquid-contact materials are all PTFE materials, which can resist strong acids (HNO 3 , HCL, HF, HCLO 4 , etc.); the injection pump 132 can ensure the accuracy of liquid addition. The syringe specification is 10 ml, and the liquid addition accuracy is better than 10 ml ± 0.1 ml.
[0080] The pipetting module integrates an 8-channel automatic sampler, which realizes functions such as automatic piercing and retracting of the pipette tip, automatic sampling, sample loading, and the addition of various activation liquids, eluents, and eluates in the separation column. The sampler 142 is arranged at the end of the first robotic arm 120 and can be accurately transferred into the sample tube along with the first robotic arm 120 to perform simultaneous sampling and sample loading operations on 8 samples, ensuring the sample processing efficiency. It avoids the occurrence of cross-contamination between samples. The device is designed with an automatic pipette tip ejection structure, which is driven and controlled by a motor to automatically control the pipette tip ejection action. It has small mechanical stress and a stable structure, and the waste pipette tips can be automatically placed into the waste pipette tip box 119.
[0081] The pressurizing device 160 arranged on the second robotic arm 150 is equipped with an air circuit and a sealing ring, and adjusts the air pressure to achieve flow rate control. It has a polyurethane sealing cover and an outer port seal to prevent cross-contamination. The design of the seal can ensure that the column always maintains a pressurized state during the extraction process.
[0082] The sample tray 112 is made of anti-corrosion plastic material, with guaranteed strength, light weight and reliability. Each tray has a total of 16 sample receiving tubes, and 8 samples can be stored in a single row, corresponding to the automatic sampling and sample loading channels. The sample tray 112 is designed to be inclined, and the sample tubes can be placed obliquely to ensure all transfer during the sample transfer process and reduce sample loss.
[0083] The extraction column tray 116 is processed and made of anti-corrosion plastic material, and can hold 16 separation columns (8 in a single tray, with a total of 2 trays designed). The separation columns can be inserted from above, which is convenient for replacing the separation columns. The specific size specifications of the separation columns can be customized according to actual requirements. The storage separation column tray is designed with a universal size interface, and the unified placement position, and the number of single-row channels is the same as that of the pipette tip box 118, the sample tray 112, etc.
[0084] The sample solution and waste liquid receiving adopt a horizontally movable design, with a horizontal movement guide rail 180 designed. The whole is driven by a motor to move horizontally, so as to realize the receiving of the sample solution and waste liquid, and can automatically move to the lower part of the separation column according to the set process. The sample receiving tray 172 has a total of 16 positions and 2 trays, adopting a single-tray 8-position design. Each row can store 8 sample receiving tubes, and the sample receiving tubes are 25-milliliter volumetric flasks. After the sample solution is received, the whole tray can be taken away manually for volume fixing.
[0085] On both sides of the sample receiving tray 172, waste liquid collection troughs 174 are provided. The bottom end of each trough is connected to a waste liquid collection barrel. The waste liquid collection trough 174 is made of corrosion-resistant material and can be discharged to a designated waste liquid bottle through a peristaltic pump, realizing the functions of automatic waste liquid collection and transfer, and meeting the requirements of the laboratory waste liquid management regulations. The waste liquid collection trough 174 has a certain inclination angle, so that the waste liquid can be discharged into the waste liquid collection barrel even when the amount of waste liquid is small. In addition, a reagent rinsing waste liquid level is provided, and this waste liquid level is a fixed position. The volume of each waste liquid collection trough 174 is about 200 milliliters.
[0086] The control system is controlled by a computer program, with high control precision, good stability, and very convenient operation and use.
[0087] Verification method of the extraction and separation device 100: First, prepare a simulated solution containing elements such as Fe, Mn, Co, Ni, Cu, Zn, Ba, Cr, V, Ti, Mo, Mg, Pb, Al, etc., and verify the elution curve of the automatic extraction and separation device for separating the simulated solution. The experimental results are as Figure 9 shown. From the experimental results, as the elution volume increases, each element is eluted from the separation column, and all elements reach the maximum elution amount when the elution volume is 4 mL. When the elution volume increases to 10 mL, most elements have been eluted. The experimental results show that the extraction and separation device 100 can effectively separate impurity elements.
[0088] The extraction column tray 116 places 16 separation columns (single-tray 8 positions, a total of 2 trays designed), namely extraction column tray A and extraction column tray B. The following is the automated operation logic of the extraction and separation device 100 provided by this application for batch processing 16 samples: (1) Preparation: Laboratory operators place the samples to be processed in the designated sample rack, edit the separation method in the system software, including activation liquid, eluent, eluate, elution volume, elution volume, position of the sample tray 112, waste liquid classification collection, and corresponding column passing flow rate, etc., and start the process; (2) Drainage: When the system is powered on, the pressurization module (pressurization device 160) is lifted, and the liquid in the separation column is drained into the waste liquid collection trough 174 and waits for activation; (3) Activation of extraction column tray A: The system automatically sucks the corresponding activation liquid (3M HNO3 That is, a nitric acid solution of 3 mol / L), and the set activation liquid is simultaneously added to the 8 columns on the extraction column tray A. At the same time, the waste liquid collection tank 174 at the bottom moves to the target waste liquid level to automatically collect the activation liquid; (4) Sealing and pressurizing the extraction column tray A: After the sample loading is completed, the pressurizing device 160 moves above the extraction column tray A for sealing, and air is introduced for pressurization to accelerate activation; (5) Activation of the extraction column tray B: At the same time, the system sucks the corresponding activation liquid through the injection pump 132, and the set activation liquid is simultaneously added to the 8 columns on the extraction column tray B. At the same time, the waste liquid collection tank 174 at the bottom moves to the target waste liquid level to automatically collect the activation liquid; (6) Sealing and pressurizing the extraction column tray B: After the sample loading is completed, the pressurizing device 160 moves above the extraction column tray B for sealing, and air is introduced for pressurization to accelerate activation; (7) Sample loading on the extraction column tray A: After the activation is completed, the pressurizing device 160 is removed, the first robotic arm 120 carries the liquid addition assembly 130 to transfer to the clean tip box 118, automatically picks up the tips, and then transfers to the sample tray 112, simultaneously aspirates 8 samples and transfers them above the separation column for automatic sample loading; (8) Sealing the extraction column tray A: The pressurizing device 160 moves above the extraction column tray A for sealing; (9) Sample loading on the extraction column tray B: After the activation is completed, the pressurizing device 160 is removed, the first robotic arm 120 carries the liquid addition assembly 130 to transfer to the clean tip box 118, automatically picks up the tips, and then transfers to the sample tray 112, simultaneously aspirates 8 samples and transfers them above the separation column for automatic sample loading; (10) Sealing the extraction column tray B: The pressurizing device 160 moves above the extraction column tray B for sealing; (11) Discarding the tips: After the sample loading is completed, the first robotic arm 120 carries the liquid addition assembly 130 to retract the tips to the waste tip box 119; (12) Elution and reception of the extraction column tray A: According to the set process, after a certain time, the sample receiving tube automatically transfers below the separation column, and the liquid addition assembly 130 adds eluent (3M HNO 3 ) for elution, and approximately 15 mL of the sample solution is correspondingly received; (13) Elution and reception of the extraction column tray B: According to the set process, after a certain time, the sample receiving tube automatically transfers below the separation column, and the liquid addition assembly 130 adds liquid for elution, and approximately 15 mL of the sample solution is correspondingly received; (14) Elution and waste discharge of the extraction column tray A: The corresponding eluent is sucked through the injection pump 132, and the set eluent is simultaneously added to the 8 columns on the extraction column tray A. At the same time, the waste liquid classification collection tray at the bottom moves to the target waste liquid level to automatically collect the waste liquid; (15)Sealing of Extraction Column Tray A: After the rinsing is completed, the pressurizing device 160 moves above the extraction column tray A for sealing; (16)Elution and Waste Discharge of Extraction Column Tray B: The corresponding eluent is aspirated by the syringe pump 132, and the set eluent is simultaneously added to the 8 columns on the extraction column tray B. At the same time, the waste liquid classification collection tray at the bottom moves to the target waste liquid level to automatically collect the waste liquid; (17)Sealing of Extraction Column Tray B: After the rinsing is completed, the pressurizing device 160 moves above the extraction column tray B for sealing; (18)End: After all processes are completed, the sealing cover 166 presses above the column to keep the separation column in a moist state, ensuring that the separation column is sealed without leakage, and the system enters the standby state.
[0089] In summary, the present invention uniquely establishes an extraction separation device 100 for the automated separation of uranium matrix in fuel and material analysis, having the following beneficial effects: 1. The present invention provides an automatic extraction separation device 100 for the automated separation of uranium matrix in fuel analysis, which is used to achieve the automated separation of uranium matrix in various fuel and material analyses and can efficiently separate and extract impurity elements in the material matrix.
[0090] 2. The extraction separation device 100 accurately adds the activation solution, rinsing solution, and eluent based on the high-precision syringe pump 132, and uses the pipetting component 140 in the form of a pipette and the liquid addition module to perform the full transfer and sampling of the sample solution, automatically picking up and removing the pipette tips, realizing the automatic completion of the entire process such as automatic sampling, rinsing, elution, receiving, volume fixation, and waste liquid classification collection.
[0091] 3. The extraction separation device 100 includes a liquid addition component 130, a pipetting component 140, and two independent pressurizing devices 160. Among them, the liquid addition component 130 executes the liquid addition and sampling processes. The first robotic arm 120 automatically picks up the pipette tip, and the syringe pump 132 ensures the liquid suction accuracy, simulating the form of a pipette to perform the full transfer of the sample, which can ensure no cross-contamination of the sample, and uses the high-precision syringe pump 132 to perform processes such as activation, rinsing, and elution of the separation column; the pressurizing device 160 includes a sealing layer and a gas path. The sealing layer uses polyurethane material to ensure the sealing effect, and the independent gas path is used to pressurize and control the flow rate, which can seal and pressurize the extraction column tray 116.
[0092] 4. An automated separation method for uranium matrix in fuel and material analysis based on the automatic extraction separation device 100 is established.
[0093] An extraction separation device for automatic separation of uranium matrix in fuel and material analysis established by the present invention can be directly applied to the automatic separation of uranium matrix in fuel and material analysis, realizing the automatic control of the sample separation process, liberating manpower, improving efficiency, reducing environmental and human pollution, and enhancing safety.
[0094] In this application, the term "a plurality of" refers to two or more, unless otherwise clearly defined. Terms such as "installed", "connected", "connected to", "fixed" and the like should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; "connected" can be a direct connection or an indirect connection through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.
[0095] In the description of this specification, the description of terms such as "one embodiment", "some embodiments", "specific embodiments" and the like means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of this application. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0096] The above are only the preferred embodiments of this application and are not used to limit this application. For those skilled in the art, this application can have various changes and modifications. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of this application shall be included within the protection scope of this application.
Claims
1. An extraction and separation device (100) for automated separation of uranium matrix in fuel and material analysis, characterized in that: include: A body (110), wherein a sample tray (112), a reagent bottle (114) and an extraction column tray (116) are arranged on the body (110), and a plurality of separation columns are arranged on the extraction column tray (116), wherein the separation columns are used for selective adsorption and separation of uranium matrix and impurity elements; A first mechanical arm (120), disposed on the body (110); A liquid adding component (130), arranged on the first mechanical arm (120), the liquid adding component (130) being used to take liquid from the reagent bottle (114) and perform a liquid adding operation; A liquid transfer component (140) is arranged on the first mechanical arm (120), and the liquid transfer component (140) is used to take samples from the sample tray (112) and perform a sample loading operation; A second mechanical arm (150), disposed on the body (110); A pressurizing device (160), arranged on the second mechanical arm (150), the pressurizing device (160) being used to perform a sealing and pressurizing operation on the separation column; A receiving component (170) is disposed on the main body (110); the receiving component (170) is movable relative to the main body (110); and the receiving component (170) is used to collect sample solutions and waste liquids.
2. The extraction separation device (100) according to claim 1, characterized in that: The liquid adding component (130) comprises: a plurality of injection pumps (132) disposed on the first mechanical arm (120), the plurality of injection pumps (132) being used to take liquid from the reagent bottle (114) and add liquid to the separation column; the reagent bottle (114) stores an activation liquid, a washing liquid and an eluent; A pressure regulating structure is provided on the injection pump (132) and is used to control the liquid extraction speed and the liquid addition speed.
3. The extraction separation device (100) according to claim 2, characterized in that: The liquid adding component (130) further includes: A reagent pipeline group (136), the reagent pipeline group (136) comprising a plurality of pipelines, one end of each pipeline being connected to the injection pump (132), and each pipeline being used for adding a different reagent; The multi-way control valve (138) is connected to all pipelines of the reagent pipeline group (136) and realizes the selective circulation of different reagents by switching the valve position.
4. The extraction separation device (100) according to claim 1, characterized in that: The pipetting assembly (140) comprises: A plurality of samplers (142) are arranged on the first mechanical arm (120), and the plurality of samplers (142) can realize sampling and loading operations of a plurality of samples.
5. The extraction separation device (100) according to claim 1, characterized in that: The number of the second mechanical arms (150) is at least two, and the at least two second mechanical arms (150) are arranged opposite to each other; At least one of the pressurizing devices (160) is provided on each of the second mechanical arms (150).
6. The extraction separation device (100) according to claim 1, characterized in that: The receiving component (170) comprises a sample receiving tray (172) and a waste liquid collection tank (174), and the extraction and separation device (100) further comprises: The guide rail (180) is disposed below the sample receiving tray (172) and the waste liquid collecting tank (174); the sample receiving tray (172) can move along the guide rail (180) to receive the sample solution; and the waste liquid collecting tank (174) can move along the guide rail (180) to receive the waste liquid.
7. The extraction separation device (100) according to any one of claims 1 to 6, characterized in that: The pressurizing device (160) comprises: an air circuit, arranged on the second mechanical arm (150), for adjusting the air pressure in the separation column; A sealing layer, disposed on the gas path, and used to seal the gas path; A sealing cover (166) is provided on the second mechanical arm (150) and is used to seal the outer opening of the separation column.
8. The extraction separation device (100) according to any one of claims 1 to 6, characterized in that: Also includes: A waste liquid bottle (192), the waste liquid bottle (192) comprising a first waste liquid bottle and a second waste liquid bottle, the first waste liquid bottle and the second waste liquid bottle being used to store different waste liquids; A peristaltic pump (190) is disposed on the main body (110), and the peristaltic pump (190) is used to pump the waste liquid collected by the waste liquid collection tank (174) to the waste liquid bottle (192).
9. The extraction separation device (100) according to any one of claims 1 to 6, characterized in that: Also includes: A control system is connected to the first robotic arm (120), the liquid adding component (130), the pipetting component (140), the second robotic arm (150), the pressurizing device (160) and the receiving component (170), and the control system is capable of issuing control instructions to the first robotic arm (120), the liquid adding component (130), the pipetting component (140), the second robotic arm (150), the pressurizing device (160) and the receiving component (170).
10. The extraction separation device (100) according to any one of claims 1 to 6, characterized in that: The first mechanical arm (120) and the second mechanical arm (150) are two-axis mechanical arms, and surfaces of the first mechanical arm (120) and the second mechanical arm (150) are coated with an anti-corrosion material layer.
Citation Information
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