Method for automatically extracting and separating uranium matrix in uranium-containing solution

Abstract

The invention belongs to the technical field of extraction and separation of uranium matrixes in uranium solutions, aims to solve the problems of tedious operation, long time consumption, high labor intensity, poor uniform mixing effect and low extraction efficiency in the prior art, and discloses a method for automatically extracting and separating uranium matrixes in uranium-containing solutions. The automatic module performs automatic cover opening, automatic extraction agent adding, automatic cover closing, automatic vortex uniform mixing, automatic centrifugation, automatic cover opening and automatic subnatant suction into a clean sample tube, and the method is high in automation degree and extraction efficiency.

Description

Technical Field

[0001] The present application belongs to the technical field of extraction and separation of uranium matrix in uranium solution, and in particular to a method for automatically extracting and separating uranium matrix in uranium-containing solution. Background Art

[0002] At present, the existing method for extracting and separating uranium matrix from uranium-containing solution is as follows: draw sample solution into a clean extraction tube, add extractant, cover the extraction tube, shake, let stand, open the extraction tube cover, draw the upper organic phase and discard, add extractant, cover the extraction tube cover, shake, let stand, open the extraction tube cover, draw the lower aqueous phase into a clean sample tube for testing. However, this method is cumbersome, time-consuming, labor-intensive, and personnel are exposed to a large amount of organic reagents, which damages the health of operators. In addition, the amplitude of manual shaking by personnel is unstable, the repeatability of extraction is poor, and the error introduced by operation is large.

[0003] Chinese patent CN216259234U discloses a laboratory liquid-liquid automatic extraction device, which can realize the automatic operation of adding extractant, vertical oscillation up and down, and extracting extraction liquid. The extraction device has a small number of sample bottle stations and is not suitable for the extraction of large quantities of samples; the extraction efficiency of vertical movement and up and down oscillation is low. In addition, the design of the conical sample tube has defects: during the up and down oscillation process, part of the solution at the bottom of the conical sample tube may not be mixed, so when the extraction needle extracts the extraction liquid from the bottom, part of the solution that has not been completely extracted will be extracted; after the extraction is completed, it needs to stand for a certain period of time before the liquid can be taken, and the extraction efficiency is low.

[0004] Chinese patent CN217981373U discloses an extraction device for sample pretreatment, which uses an extraction column for solid-liquid extraction and uses positive pressure to generate balanced gas pressure to improve extraction quality. The device has a small number of extraction columns and is not suitable for extracting large quantities of samples; the extraction column needs to be cleaned after use before the next round of extraction operation can be performed; the extraction column has a service life, and a new extraction column needs to be prepared after a period of use.

[0005] Chinese patent CN112237754A discloses an automatic extraction device and its working method, which uses a controller to drive the valve assembly to work, and uses a syringe pump and a valve assembly to extract the solvent in the solvent bottle into the ultrasonic extraction assembly for ultrasonic extraction. After the extraction is completed, the air is pressed into the air pump and the valve assembly, so that the liquid extracted in the ultrasonic extraction assembly is pressed into the constant volume assembly for constant volume, and the sample extraction preparation process is automatically completed. The device has few extraction stations and is not suitable for the extraction of large quantities of samples; after the extraction is completed, the liquid needs to be left to stand for stratification before it can be taken.

[0006] It can be seen that the existing extraction and separation technology is to manually perform the extraction and separation throughout the process or to use machines to replace manpower in some links, such as automatically transferring solutions, automatically adding extractants, shaking with oscillators, and centrifuging with centrifuges, but manual operation is still required between each link. When the sample volume is large, the processing takes a long time, the labor intensity is high, the efficiency is low, and the personnel are exposed to a large amount of organic reagents, which damages the health of the operators. In addition, the amplitude of manual shaking by personnel is unstable, the repeatability of extraction is poor, and the error introduced by the operation is large. After extraction, it needs to stand for a certain period of time before the lower layer of clear liquid can be sucked for detection, which takes too long.

[0007] The existing liquid-liquid extraction and separation device has design defects. The vertical oscillation method has poor mixing effect and low oscillation efficiency, and the extraction effect is poor. After the extraction is completed, it needs to stand for a certain period of time before the liquid can be taken. The extraction efficiency is low, and the amount of extracted samples is small. It is not suitable for the extraction and separation of large quantities of samples.

[0008] The extraction column used in the existing solid-liquid extraction method has a service life. After a period of use, a new extraction column needs to be prepared. The operation is cumbersome and the extraction efficiency is low. It is not suitable for the extraction and separation of large quantities of samples. Summary of the invention

[0009] The purpose of the present application is to overcome the defects of the prior art and provide a method for automatically extracting and separating uranium matrix from uranium-containing solution, which solves the problems of the prior art such as complicated operation, long time consumption, high labor intensity, poor mixing effect and low extraction efficiency. The method has high automation degree and high extraction efficiency.

[0010] In order to achieve the above objectives, this application provides the following technical solutions:

[0011] Step 1: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the first position of the decapping machine, and the mechanical arm of the decapping machine unscrews the tube cap;

[0012] Step 2: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the sample loading rack;

[0013] Step 3: Add the extractant with a high-precision syringe pump;

[0014] Step 4: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the first position of the decapping machine, and the mechanical arm of the decapping machine tightens the tube cap;

[0015] Step 5: Move the robotic arm to pick up the centrifuge tube containing the sample solution and place it on the vortex oscillator, and wait for vortexing;

[0016] Step 6: Repeat the above five steps until there are six centrifuge tubes containing sample solutions on the vortex oscillator, and vortex;

[0017] Step 7: Move the mechanical arm to pick up the centrifuge tubes containing the sample solution from the vortex oscillator in turn and place them in the centrifuge position for centrifugation;

[0018] Step 8: After centrifugation is completed, the mobile robot arm sequentially picks up the centrifuge tubes containing the sample solution from the centrifuge position and puts them on the centrifuge tube input rack;

[0019] Step 9: Repeat the above eight steps until all centrifuge tubes in the centrifuge tube input racks 1, 2, and 3 are extracted;

[0020] Step 10: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the first position of the decapping machine, and the mechanical arm of the decapping machine unscrews the tube cap;

[0021] Step 11: Move the mechanical arm to pick up the empty centrifuge tube on the output rack to the second position of the decapping machine, and the mechanical arm of the second decapping machine unscrews the tube cap;

[0022] Step 12: The mechanical arm pipette obtains a pipette from the pipette box, and draws the lower layer of water from the centrifuge tube containing the sample solution into the empty centrifuge tube of the second decapping machine;

[0023] Step 13: The mechanical arm pipette moves to the top of the pipette waste port and pushes out the pipette;

[0024] Step 14: The mechanical arm of the decapping machine 1 tightens the tube cap; the mechanical arm of the decapping machine 2 tightens the tube cap;

[0025] Step 15: Move the mechanical arm to clamp the centrifuge tube containing the sample solution from the first position of the decapping machine to the input rack;

[0026] Step 16: The robotic arm clamps the centrifuge tube containing the solution to be tested from the second position of the capping machine to the output rack;

[0027] Step 17: Repeat steps 10 to 16 until the separation of the uranium matrix of all sample solutions in the centrifuge tubes containing the solution to be tested in racks 1, 2, and 3 is completed.

[0028] In some embodiments, six centrifuge tube racks are used, three of which contain centrifuge tubes containing sample solutions, and the other three contain empty centrifuge tubes.

[0029] In some embodiments, each centrifuge tube rack has 48 holes arranged in a 12*4 pattern.

[0030] In some embodiments, the method can process 144 samples at a time.

[0031] In some embodiments, when the number of samples is ≤48, the centrifuge tube rack containing the sample solution is placed in the sample input rack 1, and the empty centrifuge tube rack is placed in the sample output rack 1;

[0032] When the number of samples is ≤96, place the centrifuge tube racks containing sample solutions in sample input rack 1 and sample input rack 2, and place the empty centrifuge tube racks in sample output rack 1 and sample output rack 2;

[0033] When the number of samples is ≤144, place the centrifuge tube racks containing sample solutions on sample input rack one, sample input rack two, and sample input rack three, and place the empty centrifuge tube racks on sample output rack one, sample output rack two, and sample output rack three.

[0034] In some embodiments, the fully automatic extraction and separation system is started, the air compressor is turned on, and the pressure gauge pressure of the fully automatic extraction and separation system is set to be ≥6 bar.

[0035] In some embodiments, 4.5 mL of extractant is added to the syringe pump.

[0036] In some embodiments, the mobile robot arm places the centrifuge tube containing the sample solution on a vortex oscillator, the vortex rotation speed is (2200-2400) r / min, and the vortex time is (40-60) s.

[0037] In some embodiments, after vortex oscillation, the centrifuge automatically opens its lid, and the mobile robotic arm moves 45° vectorially to place the centrifuge tubes containing sample solutions into the centrifuge holes one by one. The centrifuge automatically closes its lid, the centrifuge speed is (6000-8000) r / min, and the centrifugation time is (100-120) s.

[0038] In some embodiments, the robotic pipette obtains the pipette from the pipette rack, moves to a place of the decapping machine, inserts it into the centrifuge tube containing the sample solution, absorbs the lower aqueous phase solution, moves the robotic pipette to the top of the empty centrifuge tube, and the tip of the pipette is located below the tube mouth of the empty centrifuge tube, and all the absorbed lower aqueous phase solution is released, moves the robotic pipette to the pipette waste port on the pipette box, pushes out the pipette, the robotic arms of decapping machine one and decapping machine two tighten the tube cap, and move the robotic arm to put the centrifuge tube back to the input rack and the output rack.

[0039] Compared with the prior art, the method for automatically extracting and separating uranium matrix from uranium-containing solution provided in the present application has the following beneficial effects:

[0040] The method realizes full process automation. According to the method, personnel only need to pour the sample solution into the centrifuge tube and cover the tube cap. After starting the extraction and separation program, the mobile robot arm replaces manpower to clamp the centrifuge tube, and the automation module automatically unscrews the tube cap, automatically adds the extraction agent, automatically tightens the tube cap, automatically vortexes and mixes, automatically centrifuges, automatically unscrews the tube cap, automatically draws the lower layer of clear liquid into a clean centrifuge tube, and automatically tightens the tube cap.

[0041] This method uses vortex oscillation instead of vertical oscillation. The maximum vortex speed can reach 2500r / min, the recommended vortex speed is (2200~2400)r / min, and the vortex time is (40~60)s, which ensures that the extractant and the sample solution are fully contacted and mixed, avoiding human error, achieving effective mixing and better extraction repeatability.

[0042] This method uses centrifugation instead of static stratification. The centrifuge is adapted to robot arm operation, and no human intervention is required during the entire operation process, including automatic opening and closing of the cover after centrifugation is started, 45° vector movement to complete the non-destructive insertion and removal of centrifuge tubes, and accurate identification of the sequence of each centrifuge tube. The centrifugal speed is (6000-8000) r / min, and the centrifugal time is (100-120) s, which shortens the processing time, has a good extraction effect, obvious stratification, and improves the detection efficiency and detection repeatability.

[0043] Furthermore, by selecting appropriate centrifuge tube specifications, amount of extractant added, vortex speed and vortex time, centrifuge speed and time, liquid sampling depth and liquid sampling volume, an automated method for fully automatic extraction and separation of uranium matrix in uranium-containing solution is achieved.

[0044] By statistically calculating the efficiency of the automation module, the detection efficiency and detection flux are obtained. The specific calculation content is shown in Table 1:

[0045] Table 1 Automation efficiency calculation table

[0046]

[0047] The extraction and separation of uranium matrix in 96 uranium-containing sample solutions can be completed every 6 hours. The sample position is 144, and 144 samples can be processed at one time. No human operation is required throughout the process, which saves labor. By adding vortex oscillation and centrifugation on the basis of simulating manual operation, the number of extractions is effectively reduced, the extraction efficiency is improved, and human errors are eliminated, the detection accuracy of samples is improved, and the rework rate is reduced. At the same time, standard substances are used for inspection and verification. The results of the automatic extraction procedure meet the detection requirements and can be extended to various types of uranium-containing samples and automatic extraction processes involving extraction operations. At the same time, it has market value for the promotion and use of automatic extraction of uranium-containing samples in many units in the industry.

[0048] Furthermore, by using a vortex oscillation module for oscillation, the vortex rotation speed can reach up to 2500r / min, and the recommended speed is (2200~2400)r / min. Compared with manual oscillation or vertical oscillation of an oscillator, vortex oscillation has higher mixing efficiency and better mixing effect, which effectively reduces the number of extractions, improves the extraction efficiency, avoids the problem of poor repeatability caused by unstable amplitude of manual oscillation, avoids human errors, reduces the sample rework rate, and improves detection accuracy.

[0049] Furthermore, by using centrifugation instead of the static step in manual operation, the sample does not need to be static, and the lower aqueous phase can be directly removed after centrifugation. The detection time of each sample is shortened from the original static 5 minutes to only centrifugation (100-120) seconds. The extraction effect is better than static stratification, the stratification is more obvious, the uranium matrix is ​​separated more thoroughly, and the detection efficiency and detection repeatability are improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] In order to more clearly illustrate the technical solution of the present application, the following is a brief introduction to the drawings required for the technical description.

[0051] Figure 1 A flow chart of the method for automatically extracting and separating uranium matrix from uranium-containing solution provided in the present application;

[0052] Figure 2 This is a schematic structural diagram of a fully automatic extraction and separation system for automatically extracting and separating a uranium matrix from a uranium-containing solution provided in the present application.

[0053] Description of reference numerals:

[0054] 1. Sample input rack 1; 2. Sample input rack 2; 3. Sample input rack 3; 4. Sample output rack 1; 5. Sample output rack 2; 6. Sample output rack 3; 7. Cap opener 1; 8. Cap opener 2; 9. Vortex oscillator; 10. Sample addition rack; 11. Waste liquid tube rack; 12. Pipette rack; 13. Pipette waste port; 14. Centrifuge. DETAILED DESCRIPTION

[0055] The following is further explained in detail through specific implementation methods.

[0056] like Figure 1 As shown, the present application discloses a method for automatically extracting and separating a uranium matrix from a uranium-containing solution, comprising:

[0057] Pipette the sample solution into a centrifuge tube;

[0058] Placing the centrifuge tube rack containing the sample solution on the input rack, which includes input rack 1, input rack 2, and input rack 3;

[0059] Select a method for automatically extracting and separating the uranium matrix from the uranium-containing solution and start the extraction and separation procedure;

[0060] Step 1: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the first position of the decapping machine, and the mechanical arm of the decapping machine unscrews the tube cap;

[0061] Step 2: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the position 10 of the sample loading rack;

[0062] Step 3: Add the extractant with a high-precision syringe pump;

[0063] Step 4: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the position of the decapping machine 7, and the mechanical arm of the decapping machine 7 tightens the tube cap;

[0064] Step 5: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the vortex oscillator 9 position and wait for vortexing;

[0065] Step 6: Repeat steps 1 to 5 until there are six centrifuge tubes containing sample solutions on the vortex oscillator, and vortex;

[0066] Step 7: Move the mechanical arm to pick up the centrifuge tubes containing the sample solution from the vortex oscillator in turn and place them in the centrifuge position for centrifugation;

[0067] Step 8: After centrifugation is completed, the mobile robot arm sequentially picks up the centrifuge tubes containing the sample solution from the centrifuge position and places them on the centrifuge tube input rack;

[0068] Step 9: Repeat steps 1 to 8 until all centrifuge tubes in the centrifuge tube input racks 1, 2, and 3 are extracted;

[0069] Step 10: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the position 7 of the decapping machine, and the mechanical arm of the decapping machine unscrews the tube cap;

[0070] Step 11: Move the mechanical arm to clamp the empty centrifuge tube 2 on the output rack to the position of the second decapping machine 8, and the mechanical arm of the second decapping machine 8 unscrews the tube cap;

[0071] Step 12: The robotic arm pipette draws the lower aqueous phase solution from the centrifuge tube into the empty centrifuge tube of the second decapping machine;

[0072] Step 13: The mechanical arm pipette moves to the top of the pipette waste port 13 and pushes out the pipette;

[0073] Step 14: The mechanical arm of the decapping machine 1 tightens the tube cap; the mechanical arm of the decapping machine 2 tightens the tube cap;

[0074] Step 15: Move the mechanical arm to clamp the centrifuge tube containing the sample solution from the first position of the decapping machine to the input rack;

[0075] Step 16: The robotic arm clamps the centrifuge tube containing the solution to be tested from the second position of the capping machine to the output rack;

[0076] Step 17: Repeat steps 10 to 16 until the separation of the uranium matrix of all sample solutions in the centrifuge tubes containing the solution to be tested in racks 1, 2, and 3 is completed.

[0077] Then, the centrifuge tube containing the solution to be tested can be taken out from the output rack for testing.

[0078] Example

[0079] The method for automatically extracting and separating uranium matrix from uranium-containing solution is carried out in the following steps during a certain implementation:

[0080] (1) Remove the sample solution

[0081] Use a pipette to transfer 5 mL of sample solution into a 15 mL centrifuge tube, tighten the tube caps and place them on the centrifuge tube rack in sequence. Tighten the tube caps of a corresponding number of empty centrifuge tubes to the positions corresponding to the centrifuge tubes containing the sample solution and place them on the centrifuge tube rack in sequence.

[0082] The 6 centrifuge tube racks are made of stainless steel, 3 of which are used to hold centrifuge tubes containing sample solutions, and the remaining 3 are used to hold empty centrifuge tubes. Each centrifuge tube rack has 48 holes arranged in a 12*4 pattern, and can process 144 samples at a time.

[0083] (2) Place the sample tube rack

[0084] When the number of samples is ≤48, place the centrifuge tube rack containing the sample solution on the sample input rack-1, and place the empty centrifuge tube rack on the sample output rack-4;

[0085] When the number of samples is ≤96, place the centrifuge tube rack containing the sample solution on the sample input rack 1 and the sample input rack 2, and place the empty centrifuge tube rack on the sample output rack 1 and the sample output rack 2;

[0086] When the number of samples is ≤144, place the centrifuge tube rack containing the sample solution on sample input rack 1 1, sample input rack 2 2 and sample output rack 3 3, and place the empty centrifuge tube rack on sample output rack 1 4, sample output rack 2 5 and sample output rack 3 6.

[0087] (3) Initialization confirmation

[0088] Turn on the fully automatic extraction and separation system, turn on the air compressor, the pressure gauge of the fully automatic extraction and separation system is ≥6bar, turn on the computer, and start the software. Before initialization, determine the corresponding content according to Table 2. After confirmation, press the reset button to initialize and return to the original position.

[0089] Table 2 Confirmation content before initialization

[0090] Serial number Confirm the content Confirmation criteria 1 Capping station or robotic bottle gripper Clampless Centrifuge Tubes 2 Pipette No pipette 3 Sample processing tube Empty centrifuge tube 4 The waste bottle is empty No waste liquid accumulation 5 The centrifuge is empty Empty centrifuge tube 6 The filling station is empty Empty centrifuge tube 7 Vortex mixer is empty Empty centrifuge tube

[0091] Match the corresponding consumables and reagents according to the number of samples to be processed. Add additional extractant to ensure that the amount of extractant is sufficient. The pipette rack icon on the main screen automatically displays the number and position distribution of pipettes on the pipette rack 12. The operator needs to confirm whether there are enough pipettes to transfer the sample solution. If the number of pipettes on the pipette rack 12 is insufficient, the operator needs to replenish and refresh the counter.

[0092] (4) Cleaning reagent pipelines

[0093] The mobile robotic arm clamps the waste liquid tube from the waste liquid tube rack 11 to the decapping machine 7, the robotic arm of the decapping machine unscrews the tube cap, and the mobile robotic arm clamps the waste liquid tube to the position of the sample treatment tube 10. After the extraction agent is added through the high-precision injection pump, the mobile robotic arm clamps the waste liquid tube back to the decapping machine 7, the robotic arm of the decapping machine tightens the tube cap, and the mobile robotic arm puts the waste liquid tube back to the waste liquid tube rack 11.

[0094] (5) Sample extraction, vortexing and centrifugation

[0095] The mobile robotic arm clamps the centrifuge tube containing the sample solution from the sample input rack to the decapping machine 7, the robotic arm of the decapping machine unscrews the tube cap, the mobile robotic arm clamps the centrifuge tube containing the sample solution to the sample addition processing rack 10 position, after adding 4.5mL of extraction agent through the high-precision injection pump, the mobile robotic arm clamps the centrifuge tube containing the sample back to the decapping machine, the robotic arm of the decapping machine tightens the tube cap, and the mobile robotic arm places the centrifuge tube containing the sample solution on the vortex oscillator.

[0096] The vortex rotation speed is (2200-2400) r / min, the vortex time is (40-60) s, the vortex oscillator has 6 holes in total, and 6 samples can be processed at one time. After vortex oscillation, the centrifuge 14 automatically opens the cover, and the mobile mechanical arm moves 45° vector motion to put the centrifuge tubes containing samples into the centrifuge holes in turn without damage. The centrifuge 14 automatically closes the cover, the centrifugal speed is (6000-8000) r / min, and the centrifugal time is (100-120) s. After centrifugation, the mobile mechanical arm moves 45° vector motion to take out the centrifuge tubes containing samples in turn without damage and put them back on the sample input rack.

[0097] (6) Sample collection

[0098] The mobile robot arm clamps the centrifuge tube containing the sample from the sample input rack and places it at the decapping machine 1 7. The robot arm of the decapping machine 1 unscrews the tube cover. The mobile robot arm clamps the empty centrifuge tube at the decapping machine 2 8. The robot arm of the decapping machine 2 8 unscrews the tube cover. The robot arm pipette obtains the pipette from the pipette rack 12. The robot arm pipette moves to the decapping machine 1 7 and slowly inserts it into the centrifuge tube containing the sample solution. The tip of the pipette is 5 mm away from the bottom of the centrifuge tube. 3 mL of the lower aqueous phase solution is absorbed. The robot arm pipette moves above the empty centrifuge tube. The tip of the pipette is located below the mouth of the empty centrifuge tube. All the absorbed lower aqueous phase solution is released. The robot arm pipette moves to the pipette waste port 13 next to the pipette box and pushes out the pipette. The robot arms of the decapping machine 1 7 and the decapping machine 2 8 tighten the tube cover. The mobile robot arm puts the centrifuge tube back on the input rack and the output rack.

[0099] (7) Stop operation

[0100] Stop the current run, the robot will continue to operate until the current operation is completed. When the current operation is completed, the light turns green and the run completed message is displayed.

[0101] (8) Operation termination

[0102] At the end of the run, the user interface notifies the user that the run is complete. When the run is successfully completed, the system indicator turns green, if an error occurs at any stage of the process, the indicator turns red and the door can be opened to remove the sample.

[0103] (9) Shutdown

[0104] Exit the software, press the emergency stop button, turn off the knob switch, and turn off the air compressor.

[0105] In summary, in this method, the fully automatic extraction and separation system can work 24 hours a day, with a high degree of automation and high extraction efficiency. The fully automatic extraction and separation system uses a vortex module instead of manual operation or vertical oscillation of the oscillator. The vortex rotation speed is (2200-2400) r / min, and the vortex time is (40-60) s, ensuring that the extractant and the sample solution are fully contacted and mixed, achieving effective mixing and better extraction repeatability. Centrifugation is used instead of the static step. The centrifugal speed is (6000-8000) r / min, and the centrifugal time is (100-120) s, which shortens the processing time, has a good extraction effect, obvious stratification, and improved efficiency and detection repeatability.

[0106] This application realizes full process automation. After starting the extraction and separation procedure, the mobile mechanical arm replaces manpower to clamp the sample tube, and the automation module automatically opens the cover, automatically adds the extraction agent, automatically closes the cover, automatically vortexes and mixes, automatically centrifuges, automatically opens the cover, and automatically draws the lower layer of clear liquid into the clean sample tube.

[0107] This application uses vortex oscillation instead of vertical oscillation. The vortex oscillation module is used for oscillation, and the vortex rotation speed can reach up to 2500r / min. The recommended vortex rotation speed is (2200-2400)r / min, and the vortex time is (40-60)s, which ensures that the extractant and the sample solution are fully contacted and mixed, avoiding human error, achieving effective mixing and better extraction repeatability.

[0108] This application uses centrifugation instead of static stratification. The centrifuge is adapted to robot arm operation, and there is no human intervention during the entire operation process, including automatic opening and closing of the lid after the centrifuge is started, 45° vector movement to complete the non-destructive insertion and removal of centrifuge tubes, and accurate identification of each centrifuge tube sequence. The centrifuge speed is (6000~8000) r / min, and the centrifugation time is (100~120) s, which shortens the processing time, has a good extraction effect, obvious stratification, and improves detection efficiency and detection repeatability.

[0109] The above description is only a specific implementation manner of the present application, but the protection scope of the present application is not limited thereto. Any changes or substitutions that can be easily conceived by any technician familiar with the technical field within the technical scope disclosed in the present application should be covered within the protection scope of the present application.

Claims

1. A method for automatically extracting and separating uranium matrix from uranium-containing solution, characterized in that: include: Step 1: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the first position of the decapping machine, and the mechanical arm of the decapping machine unscrews the tube cap; Step 2: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the sample loading rack; Step 3: Add the extractant with a high-precision syringe pump; Step 4: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the first position of the decapping machine, and the mechanical arm of the decapping machine tightens the tube cap; Step 5: Move the robotic arm to pick up the centrifuge tube containing the sample solution and place it on the vortex oscillator, and wait for vortexing; Step 6: Repeat the above steps until there are six centrifuge tubes containing sample solutions on the vortex oscillator, and vortex; Step 7: Move the mechanical arm to pick up the centrifuge tubes containing the sample solution from the vortex oscillator in turn and place them in the centrifuge position for centrifugation; Step 8: After centrifugation is completed, the mobile robot arm sequentially picks up the centrifuge tubes containing the sample solution from the centrifuge position and puts them on the centrifuge tube input rack; Step 9: Repeat the above steps until all the centrifuge tubes in the centrifuge tube input rack 1, the centrifuge tube input rack 2, and the centrifuge tube input rack 3 are extracted; Step 10: Move the mechanical arm to clamp the centrifuge tube containing the sample solution to the first position of the decapping machine, and the mechanical arm of the decapping machine unscrews the tube cap; Step 11: Move the mechanical arm to pick up the empty centrifuge tube on the output rack to the second position of the decapping machine, and the mechanical arm of the second decapping machine unscrews the tube cap; Step 12: The mechanical arm pipette obtains a pipette from the pipette box, and draws the lower aqueous phase solution from the centrifuge tube containing the sample solution into the empty centrifuge tube of the second decapping machine; Step 13: The mechanical arm pipette moves to the top of the pipette waste port and pushes out the pipette; Step 14: The mechanical arm of the decapping machine 1 tightens the tube cap; the mechanical arm of the decapping machine 2 tightens the tube cap; Step 15: Move the mechanical arm to clamp the centrifuge tube containing the sample solution from the first position of the decapping machine to the input rack; Step 16: The robotic arm clamps the centrifuge tube containing the solution to be tested from the second position of the capping machine to the output rack; Step 17: Repeat Step 10 to Step 16 until the uranium matrix of all sample solutions in the centrifuge tube input rack 1, the centrifuge tube input rack 2, and the centrifuge tube input rack 3 containing the solution to be tested is separated.

2. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 1, characterized in that: Six centrifuge tube racks are used, three of which contain centrifuge tubes containing sample solutions, and the other three contain empty centrifuge tubes.

3. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 2, characterized in that: Each centrifuge tube rack has 48 holes, arranged in a 12*4 pattern.

4. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 3, characterized in that: This method can process 144 samples at one time.

5. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 1 or 4, characterized in that: When the number of samples is ≤48, place the centrifuge tube rack containing the sample solution in the sample input rack 1, and place the empty centrifuge tube rack in the sample output rack 1; When the number of samples is ≤96, place the centrifuge tube racks containing sample solutions in sample input rack 1 and sample input rack 2, and place the empty centrifuge tube racks in sample output rack 1 and sample output rack 2; When the number of samples is ≤144, place the centrifuge tube racks containing sample solutions on sample input rack one, sample input rack two, and sample input rack three, and place the empty centrifuge tube racks on sample output rack one, sample output rack two, and sample output rack three.

6. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 1, characterized in that: Turn on the fully automatic extraction and separation system, turn on the air compressor, and set the pressure gauge pressure of the fully automatic extraction and separation system to ≥6 bar.

7. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 1, characterized in that: Add 4.5 mL of extractant to the syringe pump.

8. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 1, characterized in that: The robot arm is moved to place the centrifuge tube containing the sample solution on the vortex oscillator, the vortex rotation speed is 2200-2400 r / min, and the vortex time is 40-60 s.

9. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 8, characterized in that: After vortex oscillation, the centrifuge automatically opens the lid, and the mobile mechanical arm moves 45° vectorially to place the centrifuge tubes containing the sample solution into the centrifuge holes in sequence. The centrifuge automatically closes the lid, the centrifugal speed is 6000-8000r / min, and the centrifugal time is 100-120s.

10. The method for automatically extracting and separating uranium matrix from uranium-containing solution according to claim 1, characterized in that: The robotic arm pipette obtains the pipette from the pipette rack, moves to the decapping machine, inserts it into the centrifuge tube containing the sample solution, absorbs the lower aqueous phase solution, moves the robotic arm pipette to the top of the empty centrifuge tube, and the tip of the pipette is located below the tube mouth of the empty centrifuge tube, releases all the absorbed lower aqueous phase solution, moves the robotic arm pipette to the pipette waste port next to the pipette box, pushes out the pipette, the robotic arms of decapping machine 1 and decapping machine 2 tighten the tube cap, and move the robotic arm to put the centrifuge tube back to the input rack and output rack.

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