Impurity analysis radioactive sample pretreatment device and method
By designing an impurity analysis system with automatic weighing, digestion and nuclide separation modules, the problems of complex and low degree of automation in the prior art are solved, and efficient automated pretreatment and impurity separation of radioactive samples are achieved, and analysis efficiency and data stability are improved.
Patent Information
- Application Number
- CN202411949039.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-03-18
AI Technical Summary
The existing impurity analysis system has problems such as complex manual pre-processing operations, long time consumption, low efficiency, poor data traceability, high equipment failure rate, and inability to achieve complete automation, resulting in low analysis efficiency and difficult to guarantee product quality.
An impurity analysis radioactive sample pretreatment system including an automatic weighing module, an automatic digestion module and an automatic nuclide separation module is designed. Through the two-way transmission of the robot and the middle turntable, the automated pretreatment and impurity separation of radioactive samples are realized.
It realizes automated pre-processing of radioactive samples and impurity separation, reduces manual participation, improves analysis efficiency and data stability, reduces equipment failure rate and operation error, and ensures data traceability.
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Figure CN119643269A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the field of radioactive material processing, and in particular, relates to a radioactive sample pre-processing device and method for impurity analysis. Background Art
[0002] Nuclear materials play a wide range of irreplaceable roles in the military and national defense fields, civilian reactors, nuclear power fuels, and core fuels. Impurity content is an analytical item that must be monitored during the production of nuclear materials and is the key to detecting whether nuclear material production is qualified.
[0003] At present, the existing impurity analysis system has problems such as complex manual pre-processing operation process, long time consumption, low efficiency, high requirements on the operating quality of analysts, poor traceability of pre-processing process and analysis data, requiring a lot of manpower, frequent human errors, limited operating space, large radiation measurement, etc., resulting in low analysis efficiency, failure to provide analysis data for the process in time, delaying the judgment of the process, and seriously slowing down the progress of the project. At present, there are relatively few types of relevant automated processing equipment suitable for analysis of radioactive nuclear materials at home and abroad. The pre-processing analysis methods that have been put into use have few single functions and cannot be used for multiple purposes. The equipment has a high failure rate and cannot fully realize automated pre-processing. It still requires manual participation, inspection and maintenance are difficult, internal system information cannot be fully obtained, and coefficient calculation cannot be performed on the processed samples. Summary of the invention
[0004] In order to solve the problems existing in the above-mentioned technologies, reduce the labor intensity of personnel, improve the analysis efficiency, reduce manual errors and manual mistakes, ensure the stability of data and the traceability of the process, provide data reference for the process in a timely manner, ensure the quality of unit products and improve efficiency at the same time, the patent of the present invention provides a sample automatic pretreatment system, which covers automatic weighing, automatic digestion and volume determination, automatic nuclide separation and other multifunctional impurity analysis radioactive sample pretreatment systems. In addition to being used for the sample pretreatment part of the determination of impurity element content in nuclear materials, the system can also perform automated pretreatment operations for multiple analysis projects and multiple radioactive samples simultaneously.
[0005] The technical solution of the present invention is as follows:
[0006] The present invention provides a radioactive sample pretreatment device for impurity analysis, which is characterized by comprising an automatic weighing module, an automatic digestion module and an automatic nuclide separation module, wherein radioactive samples are bidirectionally transferred between the automatic weighing module and the automatic digestion module, and radioactive samples are bidirectionally transferred between the automatic digestion module and the automatic nuclide separation module.
[0007] The automatic weighing module weighs the radioactive sample and puts it into the digestion tube; the automatic digestion module adds acid to digest, heats and fixes the radioactive sample; the automatic nuclide separation module activates the radioactive sample to separate impurities.
[0008] The automatic weighing module includes an automatic cover opening device, a bracket, a manipulator a, a turntable a, a code scanning area, a sample tray a, a balance, and a balance display screen;
[0009] The bracket is located below the support plate and is used to support the upper equipment; the support plate runs through the impurity analysis radioactive sample pretreatment device; the manipulator a is suspended and fixed at the center of the support plate by a mechanical arm; the automatic cover opening device, code scanning area, sample tray a, balance, and balance display are located above the bottom plate and placed around the manipulator a; the turntable a is located at the edge of the support plate, and a movable rack is installed underneath it, which can move left and right to transport radioactive samples.
[0010] The automatic digestion module includes a manipulator b, a support lifter, a constant volume device, a flow path component, a graphite component, an exhaust component, and a reagent cabinet;
[0011] The support lifter is connected to a robot b via a support arm; a hole groove is provided on the support lifter, a graphite component is inserted into the hole groove of the support lifter, and a surface of the graphite component is sprayed with Teflon; the flow path component is located between the constant volume device and the reagent cabinet, and liquid is extracted from the reagent cabinet located below it.
[0012] The automatic nuclide separation module includes a liquid transfer device, a sampler, a middle turntable b, a sample tray b, and an ion exchange column;
[0013] The liquid transfer device includes a water tank, from which a liquid adding arm extends, and moves on the top track of the automatic nuclide separation module; the turntable b is located on the second track of the automatic nuclide separation module, and can move left and right along the track to transport radioactive samples; the sample tray b is located on the support plate, and the ion exchange column is inserted into the bracket above the sample tray b; the sampler is connected across the first track and the second track, and the clamping claws below the sampler can be retracted and opened and closed after being separated from the track.
[0014] The present invention provides a method for pre-treatment of radioactive samples for impurity analysis, comprising the following steps:
[0015] Step 1, the automatic weighing module weighs the radioactive sample, puts the radioactive sample into a digestion tube and transmits it to the automatic digestion module;
[0016] Step 2, the automatic digestion module adds acid to the digestion tube for digestion and heats the graphite, and accurately determines the volume and adds liquid through the constant volume device;
[0017] Step 3: The radioactive sample is transferred to the ion exchange column of the automatic nuclide separation module and activated to achieve nuclide separation.
[0018] The step 1, sample weighing and tube loading, comprises the following steps:
[0019] Step 1.1 Robot a grabs the digestion tube on the turntable a and moves it to the balance for weighing;
[0020] Step 1.2: Robot a grabs the sample bottle on sample tray a, scans the barcode in the barcode scanning area and enters it into the computer software system to record the radioactive sample information;
[0021] Step 1.3: Move to the bottom of the automatic opening device and open the cover of the sample bottle;
[0022] Step 1.4: Robot a grabs the opened sample bottle, pours the radioactive sample into the digestion tube on the balance, and weighs it;
[0023] Step 1.5 Robot a removes the tube, places it on the turntable a, and pushes it to the automatic digestion module.
[0024] The step 2, heating and digestion to constant volume, comprises the following steps:
[0025] Step 2.1 The robot b grabs the digestion tube transferred from the turntable a to the automatic digestion module, and the support lift drives the robot b to descend, placing the digestion tube in the corresponding hole of the graphite component;
[0026] Step 2.2 The flow path assembly draws acid solution from the reagent cabinet and adds liquid to the digestion tube;
[0027] Step 2.3: The digestion tube is heated and digested in the graphite assembly;
[0028] Step 2.4 After the heating and digestion is completed, the support lifter drives the manipulator b to rise, so that the digestion tube is separated from the heating and sent to the exhaust assembly to exhaust the acid mist;
[0029] Step 2.5: Robot B clamps the tube and moves to the bottom of the constant volume device, automatically identifies the volume of the solution in the digestion tube and then adds liquid.
[0030] The step 3, isotope separation, comprises the following steps:
[0031] Step 3.1: Robot b transfers the digestion tube to the middle turntable b of the automatic nuclide separation module, moves the sampler, takes out the radioactive sample from the digestion tube, and transfers it to the ion exchange column;
[0032] Step 3.2: Move and start the pipetting device, add activation solution to the ion exchange column, and perform activation, elution and washing;
[0033] The radioactive sample processed in step 3.3 is picked up by the sampler and moved to the sample tray b for receiving.
[0034] The above-mentioned radioactive sample pretreatment method for impurity analysis can process multiple radioactive samples at the same time;
[0035] The graphite components are arranged in 8×6, with a total of 48 holes that can accommodate 20 ml digestion tubes, and can process 48 radioactive samples at the same time. In the step 2.2, acid is added to each digestion tube independently and simultaneously;
[0036] The ion exchange columns are arranged in a 6×6 pattern, with a total of 36 columns, and can process 36 radioactive samples at the same time. In the step 3.2, activation liquid is independently injected into each ion exchange column.
[0037] In step 1.1, the balance display screen displays the mass m1 of the digestion tube, and in step 1.4, the balance display screen displays the mass m2 of the digestion tube and the radioactive sample. It can be seen that the initial mass of the radioactive sample is m2-m1.
[0038] In step 2, heating digestion and constant volume, the temperature control range is room temperature to 230°C, and the temperature control accuracy is ±0.1°C;
[0039] In the step 2.3, the digestion tube is heated in the graphite assembly for a digestion process with a multi-stage programmed temperature increase.
[0040] In the step 2.5, the constant volume device uses an ultrasonic sensor to detect the liquid level and identify the liquid volume. The liquid adding process is controlled by two pumps, firstly pre-adding by a peristaltic pump and then accurately adding by a syringe pump.
[0041] In step 3.3, the mass of the processed radioactive sample received in the sample tray b is m3, and the reduced portion of the radioactive sample is the impurity.
[0042] The remarkable effect of the present invention is that the device and method for pre-treatment of radioactive samples for impurity analysis provided by the present invention can automatically complete the pre-treatment of radioactive samples and the impurity separation process, reduce manual participation, and save labor costs; and the equipment is easy to operate and maintain. The automatic weighing module, the automatic digestion module, and the automatic nuclide separation module respectively have mechanical devices with precise positioning such as manipulator a, manipulator b, and a liquid transfer device, which reduces manual operation errors, weighs with high precision, and ensures the reliability of impurity analysis results. The flow path component automatically adds acid for digestion, and the constant volume device uses an ultrasonic sensor to accurately determine the volume, and accurately adds liquid through a peristaltic pump and a syringe pump, which can save raw materials and reduce the impact on component reliability in an acid gas corrosion environment. By setting 48 graphite components and 36 ion exchange columns, multi-channel parallel processing is achieved, and different types of radioactive samples can be processed simultaneously, thereby improving the work efficiency of the assembly line. BRIEF DESCRIPTION OF THE DRAWINGS
[0043] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.
[0044] Figure 1 Schematic diagram of a radioactive sample pretreatment device for impurity analysis;
[0045] Figure 2 This is the main view of the automatic weighing module;
[0046] Figure 3 It is the top view of the automatic weighing module;
[0047] Figure 4 This is the main view of the automatic digestion module;
[0048] Figure 5 It is the top view of the automatic digestion module;
[0049] Figure 6 It is a structural schematic diagram of the automatic nuclide separation module;
[0050] Reference numerals: 1-automatic weighing module; 2-automatic digestion module; 3-automatic nuclide separation module; 4-support plate;
[0051] 11-automatic cover opening device; 12-bracket; 13-manipulator a; 14-turntable a; 15-code scanning area; 16-sample tray a; 17-balance; 18-balance display screen;
[0052] 21-manipulator b; 22-support lifter; 23-volume constant device; 24-flow path assembly; 25-graphite assembly; 26-exhaust assembly; 27-reagent cabinet;
[0053] 31-liquid transfer device; 32-sampler; 33-middle turntable b; 34-sample tray b; 35-ion exchange column. DETAILED DESCRIPTION
[0054] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Generally, the components of the embodiments of the present invention described and shown in the drawings here can be arranged and designed in various different configurations.
[0055] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0056] In the description of the embodiments of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0057] The present application provides a radioactive sample pretreatment device for impurity analysis, such as Figure 1 As shown, it includes an automatic weighing module, an automatic digestion module, and an automatic nuclide separation module, and radioactive samples are bidirectionally transmitted between the modules through a transfer device or a manipulator;
[0058] Radioactive samples are transferred between the automatic weighing module and the automatic digestion module via the middle turntable a14, and the robot b clamps the samples; samples are clamped between the automatic digestion module and the automatic nuclide separation module via the robot b, and the middle turntable b33 transfers the samples.
[0059] Automatic weighing module 1 Figure 2 , Figure 3 As shown, it is used to weigh radioactive samples and load them into digestion tubes, including an automatic cover opening device 11, a bracket 12, a manipulator a13, a turntable a14, a code scanning area 15, a sample tray a16, a balance 17, and a balance display screen 18;
[0060] The support 12 is located below the support plate 4 and is used to support the upper device; the support plate 4 runs through the three modules of the impurity analysis radioactive sample pretreatment device, so as to facilitate the transmission of radioactive samples between the three modules;
[0061] The manipulator a13 is suspended and fixed at the center of the support plate 4 by a manipulator arm. The support can move left and right, forward and backward in the middle area, and the manipulator can rotate 360°; optionally, the manipulator arm is a four-axis manipulator arm;
[0062] The automatic cover opening device 11, the code scanning area 15, the sample tray a16, the balance 17, and the balance display screen 18 are located above the bottom plate 11 and are placed around the manipulator a13 in a counterclockwise direction;
[0063] The middle turntable a14 is located at the edge of the support plate 4, and optionally, movable wheels or electronic slide rails are installed underneath it to move left and right in the horizontal direction to transport radioactive samples.
[0064] Automatic digestion module 2 Figure 4 , Figure 5 As shown, it is used for acid digestion, heating and volume determination of radioactive samples, including a manipulator b21, a support lifter 22, a volume determination device 23, a flow path component 24, a graphite component 25, an exhaust component 26, and a reagent cabinet 27;
[0065] The support lifter 22 is connected to the manipulator b21 through a support arm. The support lifter 22 can move left and right and up and down, thereby driving the manipulator b21 to move. The support lifter 22 is provided with a hole slot;
[0066] In this embodiment, the support lifter 22 has 48 holes arranged in 8×6, and the graphite assembly 25 is inserted into the hole of the support lifter 22. Each graphite assembly can accommodate a 20mL digestion tube;
[0067] The surface of the graphite component 25 is sprayed with Teflon;
[0068] The flow path assembly 24 is located between the constant volume device 23 and the reagent cabinet 27, and extracts liquid from the reagent cabinet 27 located below it from bottom to top;
[0069] The constant volume device 23 controls the liquid addition through two pumps, the peristaltic pump performs pre-addition, and the syringe pump performs accurate volume addition.
[0070] Automatic nuclide separation module 3 Figure 6 As shown, it includes a liquid transfer device 31, a sampler 32, a middle turntable b33, a sample tray b34, and an ion exchange column 35;
[0071] The liquid transfer device 31 includes a water tank, from which a liquid adding arm extends, and moves on the uppermost track of the automatic nuclide separation module 3;
[0072] The middle turntable b33 is located on the second track of the automatic nuclide separation module 3 and can move left and right along the track to transport radioactive samples;
[0073] The sample tray b34 is located on the support plate 4 and is used to receive the processed radioactive samples; the sample tray b34 has a bracket with a plurality of holes and slots;
[0074] In this embodiment, the bracket above the sample tray b34 is provided with 36 holes arranged in a 6×6 pattern, and the ion exchange column 35 is inserted into the holes to separate the sample from the liquid;
[0075] The sampler 32 is connected between the first track and the second track. The clamping jaws below the sampler 32 can be retracted and opened after being separated from the second track, and moved to the corresponding position to clamp the radioactive sample.
[0076] The operation methods of each module in the impurity analysis radioactive sample pretreatment device are as follows:
[0077] The automatic weighing module 1 uses a manipulator a13 simulating a human hand to perform vibration inversion, and the balance 17 is a high-precision balance, and its reading can be read through the balance display 18;
[0078] The automatic digestion module 2 adopts a graphite heating method to achieve high-precision temperature control and multi-stage programmed temperature rise; the flow path component 24 is used to achieve accurate acid addition; an ultrasonic sensor is used for accurate volume determination, and a peristaltic pump and a syringe pump are used for accurate liquid addition;
[0079] The automatic nuclide separation module 3 uses a pipetting device 31 to accurately add activation liquid to realize automatic operation of the entire process of activation, elution and washing.
[0080] Specifically, the present invention provides a method for pre-treatment of radioactive samples for impurity analysis, comprising the following steps:
[0081] Step 1, weighing and loading the sample into a tube;
[0082] Step 1.1 The robot a13 grabs the digestion tube pre-placed on the middle turntable a14, moves it to the balance 17 for weighing, and reads the indication m1 on the balance display 18;
[0083] Step 1.2 The robot a13 grabs the sample bottle pre-placed on the sample tray a16, scans the barcode in the barcode scanning area (15) and enters it into the computer software system to record the radioactive sample information. The corresponding ICP analysis results will also be synchronously entered into the computer after completion, realizing data traceability and audit tracking of the entire process;
[0084] Step 1.3: the robot a13 moves the sample bottle to the bottom of the automatic opening device 11 and opens the cover of the sample bottle;
[0085] Step 1.4: The robot a13 grabs the opened sample bottle, pours the radioactive sample into the digestion tube on the balance 17, weighs it, and reads the indication m2 on the balance display 18; the robot a13 puts the empty sample bottle back on the sample tray a16;
[0086] Step 1.5 Robot a13 removes the tube, places it on the turntable a14, and pushes it to the automatic digestion module 2.
[0087] Step 2, heating, digestion and volume determination;
[0088] Step 2.1 The robot b21 grabs the digestion tube transferred from the middle turntable a14 to the automatic digestion module 2, and the support lifter 22 drives the robot b21 to descend, and places the digestion tube in the corresponding hole of the graphite component 25;
[0089] Step 2.2: The flow path component 24 extracts the acid solution from the reagent cabinet 27;
[0090] It should be noted that the solution delivery pipeline is a PTFE tube, and multiple pipelines are independent of each other. The acid solution is injected into the digestion tube from bottom to top, and the acid solution can be added to multiple digestion tubes at the same time, which can avoid cross contamination of reagents;
[0091] In addition, the digestion tube cover adopts a buffer design, which can condense and reflux the acid solution during the digestion process and digest the radioactive samples multiple times;
[0092] Step 2.3: the digestion tube is heated and digested in the graphite assembly 25;
[0093] In the specific implementation, the heating process is a multi-stage programmed temperature increase, and the heating rate can be set; the temperature is increased from room temperature to 230°, and the temperature error range is ±0.1°C;
[0094] Step 2.4 After the heating digestion is completed, the support lifter 22 drives the manipulator b21 to rise, so that the digestion tube is separated from the heating, and the manipulator b21 removes the digestion tube cover and sends the digestion tube to the exhaust assembly 26 to exhaust the acid mist and accelerate cooling to room temperature;
[0095] Optionally, the exhaust component working time can be set;
[0096] Step 2.5 The robot b (21) clamps the digestion tube and moves to the bottom of the volume setting device (23), uses an ultrasonic sensor to detect the liquid level for volume setting, and automatically identifies the volume of the solution in the digestion tube;
[0097] After the volume is set, two pumps are used to control the addition of liquid. The peristaltic pump is used for pre-addition, and the syringe pump is used for accurate addition.
[0098] During specific implementation, the last 2 mL of the remaining volume is accurately added using a syringe pump.
[0099] Step 3, nuclide separation;
[0100] Step 3.1 The robot b21 transfers the digestion tube to the middle turntable b33 of the automatic nuclide separation module 3, moves the sampler 32, takes out the radioactive sample from the digestion tube, and transfers it to the ion exchange column 35;
[0101] Step 3.2: Move and start the liquid transfer device 31, and accurately add the activation solution to the ion exchange column 35 through the liquid adding arm thereon to perform activation, washing and elution;
[0102] Step 3.3: The treated radioactive sample is clamped by the sampler 32 and moved to the sample tray b34 for receiving; in specific implementation, a waste liquid tray is provided below the ion exchange column 35, and the waste liquid after elution is discharged into the waste liquid tray and enters the post-processing process;
[0103] The received sample can be transferred back to the automatic weighing module 1 for weighing or other high-precision weighing devices can be used to read the indication m3 on the balance display screen 18 .
[0104] The impurity analysis results show that the impurity content is m2-m1-m3.
[0105] In one example, there are 8 radioactive samples to be processed:
[0106] First, execute step 1.1 to step 2.1, and repeat 8 times, that is, the balance display screen 18 displays 16 data in sequence, and the order is sample 1: m1, sample 1: m2...sample 8: m1, sample 8: m2;
[0107] After the eight digestion tubes containing radioactive samples are placed in the graphite assembly 25, the eight radioactive samples are digested and heated simultaneously, and the flow path assembly independently and simultaneously injects acid solution into the eight holes;
[0108] After digestion and heating, since there is only one manipulator b21 and one sampler 32, and the constant volume device 23 has only one liquid adding function, it is necessary to perform steps 2.4 to 3.1 on each digestion tube in sequence;
[0109] After the eight samples have been transferred to the ion exchange column 35, the liquid transfer device 31 is turned on, and the liquid transfer device 31 automatically moves to the top of the corresponding ion exchange column 35 in sequence along the shortest route, and adds the activation solution;
[0110] The processed radioactive samples are picked up by the sampler 32 in sequence and placed in different positions of the sample tray b in sequence. The balance display screen 18 or other high-precision weighing device displays 8 data in sequence: sample 1: m3, sample 2: m3...sample 3: m3;
[0111] According to the data sequence, the impurity content of 8 radioactive samples was analyzed.
[0112] It is understandable that when the number of radioactive samples is less than or equal to 36, the radioactive sample pre-treatment for impurity analysis is performed with reference to the above steps, except that the number of executions of the above steps is changed.
[0113] In another example, there are 48 radioactive samples to be processed:
[0114] The difference from the above embodiment is that after completing step 2.5, step 3 is first performed on 36 samples; the remaining 12 samples are placed in the middle turntable b33;
[0115] After all 36 samples are processed and moved to the sample tray b34, the 12 samples are transferred from the middle turntable b33 to the ion exchange column 35 in sequence to execute the subsequent process.
[0116] It can be understood that when the number of radioactive samples is 37 to 48, the execution steps of the radioactive sample pretreatment method for impurity analysis are consistent.
[0117] The above description is only a preferred embodiment of this patent and is not intended to limit this patent. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of this patent should be included in the scope of protection of this patent.
[0118] The preferred embodiments of the present application disclosed above are only used to help explain the present application. The optional embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of the present application. The present application selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present application, so that those skilled in the art can understand and use the present application well.
Claims
1. A radioactive sample pretreatment device for impurity analysis, characterized in that: The invention comprises an automatic weighing module (1), an automatic digestion module (2) and an automatic nuclide separation module (3), wherein the automatic weighing module (1) and the automatic digestion module (2) transfer radioactive samples in both directions, and the automatic digestion module (2) and the automatic nuclide separation module (3) transfer radioactive samples in both directions; The automatic weighing module (1) weighs the radioactive sample and puts it into a digestion tube; the automatic digestion module (2) adds acid to digest, heats and fixes the volume of the radioactive sample; and the automatic nuclide separation module (3) activates the radioactive sample to separate impurities.
2. The radioactive sample pretreatment device for impurity analysis according to claim 1, characterized in that: The automatic weighing module (1) comprises an automatic cover opening device (11), a bracket (12), a manipulator a (13), a central turntable a (14), a code scanning area (15), a sample tray a (16), a balance (17), and a balance display screen (18); The support (12) is located below the support plate (4) and is used to support the upper device; The support plate (4) passes through the impurity analysis radioactive sample pre-treatment device; The robot a (13) is suspended in the air and fixed at the center of the support plate (4) by a robot arm; The automatic cover opening device (11), the code scanning area (15), the sample tray a (16), the balance (17), and the balance display screen (18) are located above the bottom plate (11) and are placed around the manipulator a (13); The middle turntable a (14) is located at the edge of the support plate (4), and a movable rack is installed below it, which can be moved left and right to transport radioactive samples.
3. The radioactive sample pretreatment device for impurity analysis according to claim 1, characterized in that: The automatic digestion module (2) comprises a manipulator b (21), a support lifter (22), a constant volume device (23), a flow path component (24), a graphite component (25), an exhaust component (26), and a reagent cabinet (27); The support lifter (22) is connected to the manipulator b (21) via a support arm; a hole groove is provided in the support lifter (22), and the graphite component (25) is inserted into the hole groove of the support lifter (22), and the surface of the graphite component (25) is sprayed with Teflon; The flow path component (24) is located between the constant volume device (23) and the reagent cabinet (27), and extracts liquid from the reagent cabinet (27) located below it.
4. The radioactive sample pretreatment device for impurity analysis according to claim 1, characterized in that: The automatic nuclide separation module (3) comprises a liquid transfer device (31), a sampler (32), a middle turntable b (33), a sample tray b (34), and an ion exchange column (35); The liquid transfer device (31) comprises a water tank, from which a liquid adding arm extends, and moves on the uppermost track of the automatic nuclide separation module (3); The middle turntable b (33) is located on the second track of the automatic nuclide separation module (3) and can move left and right along the track to transport radioactive samples; The sample tray b (34) is located on the support plate (4), and the ion exchange column (35) is inserted into the bracket above the sample tray b (34); The sampler (32) is connected between the first track and the second track, and the clamping claw below the sampler (32) can be extended and opened after being separated from the track.
5. A method for pre-treatment of radioactive samples for impurity analysis, characterized in that: The following steps are involved: Step 1, the automatic weighing module (1) weighs the radioactive sample, puts the radioactive sample into a digestion tube and transmits it to the automatic digestion module (2); Step 2, the automatic digestion module (2) adds acid to the digestion tube for digestion and graphite heating, and accurately determines the volume and adds liquid through the constant volume device (23); Step 3, the radioactive sample is transferred to the ion exchange column (35) of the automatic nuclide separation module (3), and the nuclide separation is achieved after activation.
6. A method for pre-treatment of radioactive samples for impurity analysis according to claim 5, characterized in that: The step 1 comprises the following steps: Step 1.1 The robot a (13) grabs the digestion tube on the turntable a (14) and moves it to the balance (17) for weighing; Step 1.2: Robot a (13) grabs the sample bottle on the sample tray a (16), scans the barcode in the barcode scanning area (15), enters it into the computer software system, and records the radioactive sample information; Step 1.3: the robot a (13) moves the sample bottle to the bottom of the automatic opening device (11) and opens the cover of the sample bottle; Step 1.4: Robot a (13) grasps the opened sample bottle, pours the radioactive sample into the digestion tube on the balance (17), and weighs it; Step 1.5: Robot a (13) removes the tube, places it on the middle turntable a (14), and pushes it to the automatic digestion module (2).
7. The method for pre-treatment of radioactive samples for impurity analysis according to claim 5, characterized in that: The step 2 comprises the following steps: Step 2.1 The robot b (21) grabs the digestion tube transmitted from the middle turntable a (14) to the automatic digestion module (2), and the support lifter (22) drives the robot b (21) to descend, and places the digestion tube in the corresponding hole of the graphite component (25); Step 2.2: The flow path component (24) draws acid solution from the reagent cabinet (27) and adds liquid to the digestion tube; Step 2.3: the digestion tube is heated and digested in the graphite assembly (25); Step 2.4 After the heating and digestion is completed, the support lifter (22) drives the manipulator b (21) to rise, so that the digestion tube is separated from the heating and sent to the exhaust assembly (26) to exhaust the acid mist; Step 2.5: Robot b (21) clamps the digestion tube and moves to the bottom of the volume-fixing device (23), automatically identifies the volume of the solution in the digestion tube and then adds liquid.
8. The method for pre-treatment of radioactive samples for impurity analysis according to claim 5, characterized in that: The step 3 comprises the following steps: Step 3.1 The robot b (21) transfers the digestion tube to the middle turntable b (33) of the automatic nuclide separation module (3), moves the sampler (32), takes out the radioactive sample from the digestion tube, and transfers it to the ion exchange column (35); Step 3.2: Move and start the liquid transfer device (31), add activation solution into the ion exchange column (35), and perform activation, washing and elution; The radioactive sample after the treatment in step 3.3 is clamped by the sampler (32) and moved to the sample tray b (34) for receiving.
9. A method for pre-treatment of radioactive samples for impurity analysis according to any one of claims 5 to 8, characterized in that: Capable of processing multiple radioactive samples simultaneously; The graphite assembly (25) is arranged in 8×6, with a total of 48 holes that can accommodate 20 ml digestion tubes, and can process 48 radioactive samples at the same time. In the step 2.2, acid is added to each digestion tube independently and simultaneously; The ion exchange columns (35) are arranged in a 6×6 pattern, with a total of 36 columns, and can process 36 radioactive samples simultaneously. In the step 3.2, activation liquid is independently injected into each ion exchange column (35).
10. The method for pre-treatment of radioactive samples for impurity analysis according to claim 6, characterized in that: In step 1.1, the balance display screen (18) displays the mass m1 of the digestion tube, and in step 1.4, the balance display screen (18) displays the mass m2 of the digestion tube and the radioactive sample. It can be seen that the initial mass of the radioactive sample is m2-m1.
11. A method for pre-treatment of radioactive samples for impurity analysis according to claim 7, characterized in that: In the heating digestion and volume setting step, the temperature control range is room temperature to 230°C, and the temperature control accuracy is ±0.1°C; In the step 2.3, the digestion tube is heated in the graphite assembly (25) by a multi-stage programmed temperature increase process. In the step 2.5, the volume-fixing device (23) uses an ultrasonic sensor to detect the liquid level and identify the liquid volume. The liquid adding process is controlled by two pumps, firstly by a peristaltic pump for pre-addition and then by a syringe pump for accurate liquid addition.
12. The method for pre-treatment of radioactive samples for impurity analysis according to claim 8, characterized in that: In step 3.3, the mass of the processed radioactive sample received in the sample tray b (34) is m3, and the reduced portion of the radioactive sample is the impurity.