A fully automatic split type radioactive element-containing sample pretreatment device

Abstract

The application provides a full-automatic split type radioactive element sample pretreatment device, characterized in that: a split type structure is adopted to include a master control box assembly, a device host assembly, a syringe pump assembly and a reagent bottle assembly, wherein the device host assembly and the syringe pump assembly are arranged in the glove box, and the master control box assembly and the reagent bottle assembly are arranged outside the glove box. The master control box assembly containing more electronic components is arranged outside the glove box, so that the service life and reliability are greatly improved; and the reagent bottle assembly is arranged outside the glove box, so that the replacement is convenient.

Description

TECHNICAL FIELD

[0001] The present application relates to a sample pretreatment device, in particular to a full-automatic split type radioactive element-containing sample pretreatment device. BACKGROUND

[0002] Solid phase extraction is a commonly used sample pretreatment technology, which is to pass the sample solution through an ion exchange column or an extraction column, and to purify and separate the sample by using the partitioning of the separated substances between the liquid-solid two phases, so as to separate and purify the elements to be measured from other elements in the sample. This technology is widely used in the fields of biology, food, medicine, environment, and nuclide.

[0003] At present, most of the sample pretreatment devices process samples that do not contain radioactivity, and the application occasions are mainly laboratories, fume hoods, etc.

[0004] If the processed sample is a low radioactivity sample, the use environment is generally a glove box with a relatively small space. The glove box has strong sealing and relatively poor ventilation, and acid reagents are often used in the sample pretreatment process, which can easily cause equipment corrosion and damage to electronic components, thereby causing equipment failure and affecting experimental results.

[0005] The method currently used for analyzing low-low radioactivity samples needs to adjust the sample, extract (back extract), wash, and prepare a source, which is complicated and time-consuming, and the whole process needs to be manually operated by a post staff. In the extraction process, there are problems such as entrainment, loss, and contamination of the container wall. In multiple extractions, the removal of impurity nuclides is not sufficient, and other nuclides are introduced into the operating environment during the source preparation stage, which causes a large error in the measurement results. SUMMARY

[0006] To solve the above problems, the present application provides a full-automatic split type radioactive element-containing sample pretreatment device, which solves the problems of radioactive sample pretreatment in a small glove box and personnel exposure time, adopts a split design on the basis of meeting the device functions, improves the reliability of the device, and reduces the device failure rate.

[0007] To achieve the above purpose, the technical scheme adopted by the present application is:

[0008] A full-automatic split type radioactive element-containing sample pretreatment device, characterized in that: a split structure is adopted and includes a master control box assembly, a device main machine assembly, a syringe pump assembly, and a reagent bottle assembly, wherein the device main machine assembly and the syringe pump assembly are placed inside the glove box, and the master control box assembly and the reagent bottle assembly are placed outside the glove box.

[0009] The full-automatic split type radioactive element sample pre-treatment device, wherein: the equipment host assembly has a mechanical arm capable of horizontal and vertical movement, an injection needle and a reagent needle are arranged at the terminal end of the mechanical arm along the vertical direction, and the injection needle and the reagent needle are connected with the peristaltic pump; a sample collection module, a cleaning and waste liquid tank module, a stock solution module and a dilution and shaking module are arranged below the injection needle and the reagent needle.

[0010] The full-automatic split type radioactive element sample pre-treatment device, wherein: the horizontal and vertical movement of the mechanical arm is respectively controlled by a step motor, and each step motor is provided with a driver.

[0011] The full-automatic split type radioactive element sample pre-treatment device, wherein: the stock solution module is composed of a detachable support and a sample bottle.

[0012] The full-automatic split type radioactive element sample pre-treatment device, wherein: the dilution and shaking module can perform dilution and mixing and standard solution mixing, the shaking form adopts a circumferential oscillation shaking or a swing oscillation shaking form, and the mixing mode is a bubble mixing, a vortex mixing or a magnetic stirring mixing mode.

[0013] The full-automatic split type radioactive element sample pre-treatment device, wherein: a tablet computer is integrated in the main control box, or a notebook computer or a desktop computer is arranged in the main control box.

[0014] The full-automatic split type radioactive element sample pre-treatment device, wherein: the injection pump assembly is composed of two half-boxes, one of the half-boxes is arranged with an eight-way valve, an extraction column, a first three-way valve and a large-range injection pump, the front end of the large-range injection pump is connected with the lower end of the first three-way valve, one end of the first three-way valve is connected with the eight-way valve through a flange interface, the other end is connected with a buffer reagent through a flange joint, one channel of each eight-way valve is connected with one extraction column, and different reagents and solutions in standard solution bottles can be sucked through switching of the eight-way valve.

[0015] The other half-box is arranged with a five-way valve, a second three-way valve and a small-range injection pump, the front end of the small-range injection pump is connected with the lower end of the second three-way valve, one end of the second three-way valve is connected with the five-way valve through a flange interface, the other end is connected with a buffer reagent through a flange joint, and different reagents can be sucked through switching of the five-way valve.

[0016] The main control box assembly containing many electronic components is arranged outside the glove box, so that the service life and reliability are greatly improved; and the reagent bottle assembly is arranged outside the glove box, so that the replacement is convenient.

[0017] This invention uses a high-precision syringe pump as the power pump and combines it with a solenoid valve. It has the advantages of high pressure resistance, high flow accuracy, unidirectional flow path design, buffer ring to prevent solvent from flowing into the syringe, simple structure, controllable flow rate, and good corrosion resistance. Attached Figure Description

[0018] Figure 1 This is a schematic diagram illustrating the working principle of the solid-phase extraction device of the present invention.

[0019] Figure 2 This is a three-dimensional view of the overall structure of the present invention.

[0020] Figure 3 This is a three-dimensional view of the overall structure of the main unit of the device.

[0021] Figure 4 This is a schematic diagram showing the relative unfolding of the planar components of the injection pump assembly.

[0022] Figure labeling: 1-Tablet PC; 2-Control box assembly; 3-Main unit assembly; 4-Injection pump assembly; 5-Reagent bottle assembly; 6-Robotic arm; 7-Injection needle; 8-Peristaltic pump; 9-Sample collection module; 10-Cleaning and waste liquid tank module; 11-Stock solution module; 12-Dilution and mixing module; 13-Reagent needle holder; 14-Eight-way valve; 15-Extraction column; 16-No. 1 three-way valve; 17-Large range injection pump; 18-Five-way valve; 19-No. 2 three-way valve; 20-Small range injection pump; 21, 21'-Buffer reagent; 22-No. 1 buffer tube; 23-V gas interface; 24-V column interface; 25-Sample loading interface; 26-First reagent interface; 27-Collection tube; 29-Dilution interface; 30-Second reagent interface; 31-No. 2 buffer tube; 32-Fine needle; 40-Glove box. Detailed Implementation

[0023] like Figure 1 As shown, the general structure of a solid-phase extraction device is as follows:

[0024] The large-range syringe pump 17 is selectively connected to the buffer reagent 21 and the buffer tube 22 via the first three-way valve 16. The first buffer tube 22 is also connected to the eight-way valve 14. The eight-way valve 14 has a V-gas interface 23, a V-column interface 24, a sample loading interface 25, and five first reagent interfaces 26. The V-column interface 24 is connected to the collection tube 27 (the collection tube 27 is connected to the extraction column). The sample loading interface 25 is connected to the injection needle 7.

[0025] The small-range syringe pump 20 is selectively connected to the buffer reagent 21' and the five-way valve 18 via the second three-way valve 19. The five-way valve 18 has a dilution port 29 and four second reagent ports 30. The dilution port 29 is connected to one end of the second buffer tube 31, and the other end of the second buffer tube 31 is connected to the fine needle 32.

[0026] When working, the large-range syringe pump 17 sucks the buffer reagent 21 to fill the small-range syringe pump 20, and then switches the No. 1 three-way valve 16 to punch the buffer reagent 21 into the No. 1 buffer tube 22; when the small-range syringe pump 20 is sucking the reagent, the buffer reagent 21 returns to the small-range syringe pump 20, and the reagent enters the No. 1 buffer tube 22, so that the small-range syringe pump 20 does not contact the reagent, the small-range syringe pump 20 is protected, and the service life is prolonged; after the sample is sucked into the No. 1 buffer tube 22, the sample is punched into a dilution bottle; the small-range syringe pump 20 sucks the reagent to be diluted into the No. 2 buffer tube 31, and then punches into the corresponding sample bottle through different electromagnetic valves to dilute the sample, so as to avoid cross infection; then the diluted sample is sucked by the large-range syringe pump 17 for sample loading; the electromagnetic valve of the V column is switched to punch the sample into the extraction column, so that the small column is completely loaded, and the sample is separated and recovered.

[0027] The full-automatic split type radioactive element-containing sample pretreatment device provided by the application is a newly designed nuclide sample pretreatment system, which refers to a general process method of solid-phase extraction column separation, that is, a syringe pump is used as a power element to realize sample transfer, dilution, shaking, loading, cleaning of a sample bottle, elution and other processes of a nuclide solid-phase extraction column. The application can realize a double-sample-needle separation process and a multi-separation-column separation process, adopts a modular design, one module corresponds to one channel, and the combination of any channel can be realized. The application is one-key type operation with a built-in program, a control system can display the running condition of the device in real time, and can display an error and stop running in a timely manner when a fault occurs. The application has a small structure and is placed in a glove box 40 for convenient disassembly and maintenance.

[0028] As shown in Figure 2 , the application adopts a split type design, mainly includes a main control box assembly 2 (containing a tablet computer 1), a device host assembly 3, a syringe pump assembly 4 and a reagent bottle assembly 5. The device host assembly 3 and the syringe pump assembly 4 are placed inside a glove box 40, and the main control box assembly 2 and the reagent bottle assembly 5 are placed outside the glove box 40.

[0029] The device host assembly 3 and the syringe pump assembly 4 mainly adopt stainless steel, modified polytetrafluoroethylene or modified PP plate and other materials, which are resistant to radiation and corrosion, and the internal motor adopts a radiation-resistant motor, which guarantees the reliability of the device running.

[0030] The main control box assembly 2 contains many electronic components and is placed outside the glove box 40, which greatly improves the service life and reliability.

[0031] The reagent bottle assembly 5 is placed outside the glove box 40, which is convenient to replace.

[0032] The application is a multi-channel multi-reagent device, a customized automatic separation device has the following functions: automatic sampling function, automatic dilution function, automatic elution function, automatic elution function and automatic solution receiving function, the application requires to be convenient to take down and replace the extraction separation column. The operation object of the automatic separation device has nitric acid volatilization and corrosion, and the mechanical moving part, reagent conveying part and control system of the separation device need to have corrosion protection measures.

[0033] All fluid pipelines of the application are made of full corrosion-resistant material PTFE, and the injection pump box body is provided with a stepping motor, a control circuit board, a high-precision syringe, a multi-channel valve block and a corrosion-resistant electromagnetic valve, which can accurately control the volume and flow rate of the reagent.

[0034] As shown in Figure 3 The device host assembly 3 has a mechanical arm 6 capable of horizontal and vertical movement, and a sampling needle 7 and a reagent needle are arranged at the terminal end of the mechanical arm 6 along the vertical direction. The sampling needle 7 and the reagent needle are connected with a peristaltic pump 8, and can perform cleaning (pipette needle, sample bottle) operation and sample loading, extraction steps. The horizontal and vertical movements are respectively controlled by a stepping motor, and each stepping motor is provided with a driver. The parameters on the driver can be adjusted by a knob, and the moving speed can be adjusted by adjusting the parameters on the driver.

[0035] A sample collection module 9, a cleaning and waste tank module 10, an original liquid module 11 and a dilution and shaking module 12 are arranged on the base below the sampling needle and the reagent needle. The original liquid module 11, the cleaning and waste tank module 10, the dilution and shaking module 12 and the sample collection module 9 are on the same horizontal plane. Among them:

[0036] The base is made of stainless steel, has good corrosion resistance, small size, light weight and simple and convenient operation;

[0037] The original liquid module 11 is composed of a detachable support and a sample bottle, which is convenient to replace;

[0038] The cleaning and waste tank module 10 integrates the functions of cleaning needle and collecting waste liquid, and is provided with three-stage cleaning tanks to ensure the cleaning effect of the inner and outer walls of the pipette needle. The liquid in the waste tank is introduced into the waste tank by the peristaltic pump 8;

[0039] During operation, the mechanical arm 6 drives the sampling needle to absorb a specified volume of solution from the original liquid bottle of the original liquid module 11 into the dilution bottle of the dilution and shaking module 12, and adds reagent according to a specified proportion to dilute the original liquid. After the reagent is completely added, the mixing motor in the dilution and shaking module 12 is started to quickly mix the sample. After the dilution is completed, the mechanical arm 6 drives the sampling needle to move to the cleaning and waste tank module 10 for cleaning of the sampling needle. After cleaning is completed, the mechanical arm 6 drives the sampling needle to take sample from the dilution bottle of the dilution and shaking module 12 to the dilution and shaking module 12.

[0040] The dilution shaking module 12 adopts a rotary amplitude oscillation technology, is convenient for maintenance and overall replacement, the rotary oscillation time is controllable, and the oscillation and shaking effect is remarkable.

[0041] Further looking at Figure 4 The injection pump assembly 4 is composed of two half housings, one of the half housings is arranged with eight-way valves 14, extraction columns 15, a first three-way valve 16 and a large-range injection pump 17, the front end of the large-range injection pump 17 is connected with the lower end of the first three-way valve 16, one end of the first three-way valve 16 is connected with the eight-way valves 14 through a flange interface, and the other end is connected with a buffer reagent (not shown in the figure) through a flange joint, one of the channels of each eight-way valve 14 is connected with one of the extraction columns 15, and different reagents and solutions in the standard solution bottles can be sucked through switching of the eight-way valves 14;

[0042] The other half housing is arranged with five-way valves 18, a second three-way valve 19 and a small-range injection pump 20, the front end of the small-range injection pump 20 is connected with the lower end of the second three-way valve 19, one end of the second three-way valve 19 is connected with the five-way valves 18 through a flange interface, and the other end is connected with a buffer reagent (not shown in the figure) through a flange joint, and different reagents can be sucked through switching of the five-way valves 18;

[0043] In this way, the sample can be added into the extraction column 15 from the sample bottle and the solution in the standard solution bottle according to the set flow rate and volume through high-precision injection pumps and electromagnetic valve switching, the activation of the extraction column 15, the sample loading, elution and elution operations are completed; and the target solution enters the collection bottle through the collection pipeline.

[0044] In summary, the high-precision injection pump is used as a power pump in the present application, and the electromagnetic valve is used in combination, which has the advantages of high pressure resistance, high flow precision, one-way design of the flow path, avoidance of the flow of solvent into the syringe through the buffer ring, simple structure, controllable flow rate, good corrosion resistance and the like. The nuclide automatic extraction and separation experiment requires accurate control of the flow rate at a low flow rate, and the sample cannot enter the pipeline to avoid cross contamination. The injection pump is driven by a stepping motor, which can ensure the flow rate and volume accuracy at a low flow rate. The flow rate accuracy and volume accuracy can meet the experimental requirements at a low flow rate, and the use of a pipette needle makes it easier to correct the volume, which fully meets the experimental requirements.

[0045] In addition, the present application has the following alternative solutions:

[0046] 1. In the case of large sample processing amount and low control precision, the large-range injection pump 17 and the small-range injection pump 20 can be replaced by peristaltic pumps 8 respectively;

[0047] 2. The dilution and mixing module 12 in the foregoing embodiments integrates the functions of dilution and mixing, and adopts a circumferential oscillation mixing mode. The circumferential oscillation mixing mode can be replaced by a swing oscillation mixing mode, and the mixing mode can be replaced by a bubble mixing mode, a vortex mixing mode, or a magnetic stirring mixing mode. Moreover, the integrated dilution and mixing module 12 can be replaced by a split structure, i.e., composed of a separate dilution and mixing module and a separate standard and mixing module (wherein the dilution mixing refers to adding water, and the standard mixing refers to adding reagents to prevent mutual contamination during mixing, and the oscillation mixing of the present application adopts a mode of two rows of collection tubes with a middle space to avoid mutual contamination during mixing).

[0048] 3. The large-range injection pump 17 and the small-range injection pump 20 in the foregoing embodiments are respectively integrated as two separate modules, and can also be integrated as one module to replace them.

[0049] 4. The main control box and the tablet computer 1 are integrated as one module, and can be replaced by a combination of the main control box and a notebook computer or a desktop computer.

[0050] The above description is only illustrative and not restrictive, and those skilled in the art understand that many modifications, changes or equivalents can be made without departing from the spirit and scope of the claims, and all of them fall within the protection scope of the present application.

Claims

1. A fully automated split-type radioactive element-containing sample pre-treatment device, characterized by: The device adopts a split structure and comprises a master control box assembly, a device host assembly, an injection pump assembly and a reagent bottle assembly, wherein the device host assembly and the injection pump assembly are arranged inside a glove box, and the master control box assembly and the reagent bottle assembly are arranged outside the glove box; The device host assembly is provided with a mechanical arm capable of moving horizontally and vertically, and a sample injection needle and a reagent needle are arranged at the terminal end of the mechanical arm in the vertical direction, and the sample injection needle and the reagent needle are connected to a peristaltic pump; a sample collection module, a cleaning and waste liquid tank module, a stock solution module and a dilution and mixing module are arranged below the sample injection needle and the reagent needle, the dilution and mixing module is capable of dilution and mixing and standard solution mixing, the oscillation form is circumferential oscillation or swing oscillation, and the mixing mode is bubble mixing, vortex mixing or magnetic stirring mixing; The injection pump assembly is composed of two half-boxes, one of which is arranged with an eight-way valve, an extraction column, a first three-way valve and a large-range injection pump, the front end of the large-range injection pump is connected to the lower end of the first three-way valve, one end of the first three-way valve is connected to the eight-way valve through a flange interface, and the other end is connected to a buffer reagent through a flange joint, one channel of each eight-way valve is connected to one extraction column, and different reagents and solutions in the standard solution bottles can be sucked through switching of the eight-way valve; the large-range injection pump is connected to a buffer reagent one and a first buffer pipe through the first three-way valve, the first buffer pipe is also connected to the eight-way valve, the eight-way valve is provided with a V gas interface, a V column interface, a sample loading interface and five first reagent interfaces, the V column interface is connected to a collection pipe, the collection pipe is connected to the extraction column, and the sample loading interface is connected to the sample injection needle; The other half-box is arranged with a five-way valve, a second three-way valve and a small-range injection pump, the front end of the small-range injection pump is connected to the lower end of the second three-way valve, one end of the second three-way valve is connected to the five-way valve through a flange interface, and the other end is connected to a buffer reagent through a flange joint, different reagents can be sucked through switching of the five-way valve; the small-range injection pump is connected to a buffer reagent two and the five-way valve through the second three-way valve, the five-way valve is provided with a dilution interface and four second reagent interfaces, one end of a second buffer pipe is connected to the dilution interface, and the other end of the second buffer pipe is connected to a fine needle.

2. The fully automated split-type radioactive element containing sample pre-treatment device according to claim 1, characterized in that: The horizontal and vertical movements of the mechanical arm are respectively controlled by a step motor, and each step motor is provided with a driver.

3. The fully automated split-type radioactive element containing sample pre-treatment device according to claim 1, characterized in that: The stock solution module is composed of a detachable support and a sample bottle.

4. The fully automated split-type radioactive element containing sample pre-treatment device according to claim 1, characterized in that: A tablet computer is integrated in the master control box, or a notebook computer or a desktop computer is arranged in the master control box.

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