Liquid temperature control cyclic irradiation test device and method

Abstract

The invention discloses a liquid temperature control cyclic irradiation test device and method, belongs to the technical field of nuclear power spent fuel post-treatment, and aims to solve the problems of how to improve irradiation uniformity and effectively control the temperature of a sample in the irradiation process. The liquid temperature control circulating irradiation test device comprises an irradiation container, a thermostat, a buffer bottle and liquid conveying equipment, the buffer bottle is arranged in a temperature control groove of the thermostat; and the irradiation container is circularly connected with the buffer bottle through a pipeline to form a liquid circulation system. Liquid can be driven to circularly flow in the liquid circulating system through the liquid conveying equipment, and the liquid circulating system is used in the irradiation test process of an exogenous method research on a sample, the circularly flowing sample can be fully and mechanically mixed uniformly, the irradiation uniformity is improved, and the temperature difference of each part of the sample can be ensured to be relatively small. By arranging the thermostat and the buffer bottle, heat exchange can be carried out between the thermostat and liquid in the buffer bottle, so that the temperature of a sample in the liquid circulation system is effectively controlled.

Description

Technical Field

[0001] The invention belongs to the technical field of nuclear power spent fuel post-processing, and in particular relates to a liquid temperature-controlled cyclic irradiation test device and method. Background Art

[0002] Solvent extraction is a primary process in the reprocessing of spent nuclear power fuel. However, because spent fuel contains a variety of highly radioactive fission products and actinides, the extraction system is subject to intense irradiation from various radiation sources. Compared to β and γ radiation, α radiation can lead to more complex radiolytic behavior when interacting with the extraction system. Therefore, the α radiation stability of the extraction system is a key issue that needs to be addressed in spent fuel reprocessing.

[0003] The α-irradiation stability of the extraction system is usually studied by the endogenous method and the exogenous method. Among them, the endogenous method is to add α-radioactive nuclides into the extraction system, such as 238 Pu, 241 Am, 244 Cm, etc., thereby irradiating the extraction system internally. The external source method, on the other hand, uses an accelerator to accelerate alpha particles, allowing them to perform external irradiation tests on the extraction system. The external source method has the advantages of alpha particle energy, controllable beam current, and no interference from alpha nuclides, which can obtain more accurate test results.

[0004] However, the current experimental device used for exogenous method research is a static liquid irradiation device, which includes an irradiation container for holding the sample (extraction system), and the irradiation container has an irradiation surface for the external α irradiation beam to be injected to irradiate the sample. The existing irradiation device has the following problems: (1) Since the penetration depth of α particles is very shallow, generally only about 0.23mm can be injected. Therefore, when the existing irradiation device is used to perform α irradiation tests on samples, the interior of the sample is not effectively irradiated, the irradiation is uneven, and the temperature difference between the irradiated part and the non-irradiated part is large; (2) The temperature of the sample cannot be effectively controlled during the irradiation process; (3) The irradiated sample cannot be collected online; (4) The gaseous radiolysis products cannot be discharged and collected; (5) The sample cannot be changed without stopping the machine. Summary of the Invention

[0005] The present invention provides a liquid temperature-controlled cyclic irradiation test device and method, aiming to solve the problem of how to improve the uniformity of irradiation and effectively control the temperature of the sample during the irradiation process.

[0006] The technical solution adopted by the present invention to solve the technical problem is: a liquid temperature-controlled cycle irradiation test device includes an irradiation container with an irradiation surface, a thermostat, a buffer bottle and a liquid conveying device;

[0007] The buffer bottle is arranged in a temperature control tank of a thermostat;

[0008] The liquid outlet of the irradiation container is connected to the liquid inlet of the buffer bottle through a first pipeline, and the liquid outlet of the buffer bottle is connected to the liquid inlet of the irradiation container through a second pipeline to form a liquid circulation system;

[0009] The liquid delivery device is arranged in the liquid circulation system and is used to drive the liquid to circulate in the liquid circulation system.

[0010] Furthermore, the irradiation container includes an irradiation bottle and a piston driver;

[0011] The irradiation bottle is arranged horizontally, and a film window is provided at one end of the irradiation bottle as an irradiation surface. A piston is provided in the irradiation bottle, and an irradiation cavity is formed between the piston and the irradiation surface.

[0012] The piston driver is in driving connection with the piston and can drive the piston to move axially to adjust the volume of the irradiation chamber.

[0013] Furthermore, the film window is made of polyimide material, and a polytetrafluoroethylene O-ring for sealing and an annular end cap for fixing are provided at the connection between the film window and the end of the irradiation bottle;

[0014] And / or, the top of the irradiation bottle is provided with an exhaust hole connected to the irradiation chamber, and the exhaust hole is provided with an exhaust valve.

[0015] Furthermore, the thermostat is a constant temperature metal bath, a temperature control panel is provided on the front of the constant temperature metal bath, a thermocouple is provided in the temperature control tank of the constant temperature metal bath, and the thermocouple is communicatively connected to the temperature control panel.

[0016] Furthermore, the test device also includes a container stand and a device box with rollers;

[0017] The container rack includes a horizontal adjustment rod provided on the side of the device box, a vertical adjustment rod connected to the horizontal adjustment rod via an adjustable fixing clamp, and a support platform provided on the top end of the vertical adjustment rod;

[0018] The irradiation container is arranged on the table of the support table;

[0019] The thermostat is arranged on the top surface of the device box.

[0020] Furthermore, the test device also includes a solvent bottle, a gas bottle, a multi-channel solenoid valve, and a multi-channel switching valve with a switching motor;

[0021] There are at least six solvent bottles, at least two of which are used to store two or more liquids to be irradiated, at least two of which are used to collect irradiated liquids, at least one of which is used to store cleaning liquid, and at least one of which is used to store waste cleaning liquid;

[0022] The multi-channel solenoid valve has at least eight valve ports;

[0023] The multi-channel switching valve has at least five valve ports;

[0024] The first pipeline includes a first hose connecting the liquid outlet of the irradiation container to one of the valve ports of the multi-channel solenoid valve, and a second hose connecting one of the valve ports of the multi-channel solenoid valve to the liquid inlet of the buffer bottle;

[0025] The second pipeline includes a third hose connecting the liquid outlet of the buffer bottle to one of the valve ports of the multi-channel switching valve, a fourth hose connecting one of the valve ports of the multi-channel switching valve to one of the valve ports of the multi-channel solenoid valve, and a fifth hose connecting one of the valve ports of the multi-channel solenoid valve to the liquid inlet of the irradiation container;

[0026] The solvent bottle for collecting the irradiated liquid and the solvent bottle for storing the waste cleaning liquid are respectively connected to the valve ports of the multi-channel solenoid valve, and the remaining solvent bottles are respectively connected to the valve ports of the multi-channel switching valve;

[0027] The gas cylinder is connected to one of the valve ports of the multi-channel solenoid valve.

[0028] Furthermore, the test device also includes a porous hose connector, a storage box and a gas cylinder rack;

[0029] At least two solvent bottles are used to store cleaning liquid, and the solvent bottles for storing cleaning liquid are connected to the valve ports of the multi-channel switching valve through porous hose connectors;

[0030] The storage box is arranged on the top surface of the device box, and each solvent bottle is placed in the storage box;

[0031] The gas cylinder rack is arranged on the side of the device box, and the gas cylinder is arranged on the gas cylinder rack.

[0032] Furthermore, the test device also includes a support plate arranged on the top surface of the device box;

[0033] The liquid delivery device includes a first peristaltic pump provided on the fourth hose and a second peristaltic pump provided on the second hose;

[0034] The multi-channel solenoid valve, the multi-channel switching valve, the first peristaltic pump and the second peristaltic pump are all arranged on the support plate.

[0035] The present invention also provides a liquid temperature-controlled cyclic irradiation test method, which uses the above-mentioned liquid temperature-controlled cyclic irradiation test device to perform irradiation testing, including a liquid filling process, a temperature-controlled irradiation process, and a pipeline cleaning process;

[0036] The liquid filling process comprises: filling the liquid to be irradiated into at least one solvent bottle, and filling the cleaning liquid into at least one solvent bottle;

[0037] The temperature-controlled irradiation process comprises the following steps:

[0038] A1. Control the multi-channel switching valve and the multi-channel solenoid valve to connect one of the solvent bottles containing the liquid to be irradiated to the liquid circulation system. Then, use the liquid delivery device to pump the liquid to be irradiated in the solvent bottle into the liquid circulation system. After all the liquid to be irradiated in the solvent bottle has entered the liquid circulation system, cut off the connection between the solvent bottle and the liquid circulation system.

[0039] A2. Allow the irradiation beam to pass through the irradiation surface to irradiate the liquid in the irradiation chamber of the irradiation container. Simultaneously, the liquid is driven to circulate in the liquid circulation system through the liquid delivery device, and heat is exchanged with the liquid in the buffer bottle through the thermostat to maintain the liquid temperature in the liquid circulation system at the set temperature ±5°C, -100°C ≤ set temperature ≤ 100°C;

[0040] A3. After irradiation is completed, control the multi-channel switching valve and the multi-channel solenoid valve to connect one of the empty solvent bottles to the liquid circulation system. Then, use the liquid delivery device to pump the irradiated liquid in the liquid circulation system into the solvent bottle for storage. After all the irradiated liquid in the liquid circulation system has entered the solvent bottle, the connection between the solvent bottle and the liquid circulation system is cut off.

[0041] The pipeline cleaning process includes the following steps:

[0042] B1. After the temperature-controlled irradiation process is completed, the multi-channel switching valve and the multi-channel solenoid valve are controlled to connect the solvent bottle containing the cleaning liquid to the liquid circulation system. The cleaning liquid in the solvent bottle is then pumped into the irradiation container through the liquid delivery device, and the connection between the solvent bottle and the liquid circulation system is then cut off.

[0043] B2. Pump the cleaning liquid in the irradiation container into the buffer bottle through the liquid conveying equipment;

[0044] B3. Control the multi-channel switching valve and the multi-channel solenoid valve to connect one of the empty solvent bottles to the liquid circulation system, and then pump the cleaning liquid in the buffer bottle into the solvent bottle through the liquid delivery device to complete the storage of the waste cleaning liquid;

[0045] B4. Repeat steps B1 to B3 to clean the liquid circulation system three or more times;

[0046] B5. Control the multi-channel switching valve and the multi-channel solenoid valve to connect the gas cylinder with the liquid circulation system. Use the gas in the gas cylinder to blow the residual liquid in the liquid circulation system into the solvent bottle storing the waste cleaning liquid, and then cut off the passage between the solvent bottle and the liquid circulation system.

[0047] Furthermore, the method also includes an online sample exchange irradiation process;

[0048] The liquid filling process comprises: filling two or more liquids to be irradiated into different solvent bottles, and filling at least one solvent bottle with a cleaning liquid;

[0049] The online sample-changing irradiation process is as follows: after one liquid to be irradiated is irradiated according to the temperature-controlled irradiation process and the liquid circulation system is cleaned through the pipeline cleaning process, the temperature-controlled irradiation process is repeated to irradiate another liquid to be irradiated and the liquid circulation system is cleaned through the pipeline cleaning process.

[0050] The beneficial effects of the present invention are:

[0051] 1) The test device has a liquid circulation system, and the liquid can be driven to circulate in the liquid circulation system through the liquid delivery equipment. When the sample is irradiated in the exogenous method, the circulating sample can be fully mechanically mixed, which improves the uniformity of irradiation and ensures that the temperature difference between different parts of the sample is small, solving the problem of uneven exogenous irradiation, especially the problem of uneven exogenous α irradiation, and the problem of local overheating of the sample during irradiation.

[0052] 2) The test device is equipped with a thermostat and a buffer bottle. The thermostat can be used to exchange heat with the liquid in the buffer bottle to effectively control the temperature of the sample in the liquid circulation system, ensuring that the temperature difference between the sample temperature and the set temperature does not exceed 5°C.

[0053] 3) An exhaust hole connected to the irradiation chamber is provided at the top of the irradiation bottle, and an exhaust valve is provided at the exhaust hole to facilitate the discharge and collection of gaseous radiolysis products.

[0054] 4) The test device also includes multiple solvent bottles, gas cylinders, multi-channel solenoid valves and multi-channel switching valves. During the irradiation test using the test device and the liquid temperature-controlled cyclic irradiation test method provided by the present invention, online collection of irradiated samples and non-stop sample replacement can be achieved, greatly improving the irradiation efficiency.

[0055] The technical effects brought about or directly produced by other technical features of the present invention will be described in detail in the subsequent specific implementation methods. BRIEF DESCRIPTION OF THE DRAWINGS

[0056] Figure 1 It is a schematic diagram of the three-dimensional structure of the liquid temperature-controlled cyclic irradiation test device provided by the present invention;

[0057] Figure 2 This is a simplified schematic diagram of the liquid temperature-controlled cyclic irradiation test device in Example 1 of the present invention;

[0058] The markings in the figure are: 1-irradiation bottle; 2-fifth hose; 3-piston driver; 4-support table; 5-vertical adjustment rod; 6-adjustable fixing clamp; 7-horizontal adjustment rod; 8-temperature control panel; 9-thermostat; 10-buffer bottle; 11-multi-channel solenoid valve; 12-first peristaltic pump; 13-second peristaltic pump; 14-support plate; 15-multi-channel switching valve; 16-switching motor; 17-multi-porous hose connector; 18-storage box; 19-solvent bottle; 20-gas cylinder rack; 21-gas cylinder; 22-device box; 23-roller; 24-irradiation surface. DETAILED DESCRIPTION

[0059] The present invention will be further described below with reference to the accompanying drawings and embodiments. The same reference numerals in the accompanying drawings represent components with the same or similar functions. Although various aspects of the embodiments are shown in the accompanying drawings, the drawings are not necessarily drawn to scale unless otherwise indicated.

[0060] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positions, and dimensional relationships are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of description, and do not indicate or imply that the device or component referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0061] The term "transmission connection" refers to a connection used to transmit power or motion in a mechanical system, such as a direct connection or a connection achieved through a transmission mechanism such as a coupling, reducer, gear assembly, or worm gear assembly. When the term "plurality" refers to a quantity, it generally refers to three or more. For example, "a plurality" generally refers to three or more. The expression "primarily composed of" should be interpreted as including structural components not mentioned in the sentence. The term "and / or" simply describes an association between associated objects, indicating that three possible relationships exist. For example, "A and / or B" can mean: A exists alone, A and B exist simultaneously, or B exists alone. The term "communication connection" refers to communication between connected devices through the transmission of signals. It can be divided into wired and wireless connections. Wired connections typically include cables, optical fibers, and other connections; wireless connections typically include radio, Bluetooth, infrared, NFC, and other connections. Furthermore, the terms "first," "second," "third," "fourth," and "fifth" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0062] like Figure 1 As shown, the liquid temperature-controlled cycle irradiation test device includes an irradiation container with an irradiation surface 24, a thermostat 9, a buffer bottle 10 and a liquid delivery device;

[0063] The irradiation container is a container used to provide a space for the liquid to be irradiated. The irradiation surface 24 of the container is a window for the liquid to be irradiated, allowing the irradiation beam to penetrate.

[0064] Thermostat 9 is a device that directly or indirectly controls one or more heat sources and / or cold sources to maintain the required temperature;

[0065] The buffer bottle 10 is arranged in the temperature control tank of the thermostat 9, and the buffer bottle 10 is used to provide a cavity for the liquid to exchange heat with the thermostat 9;

[0066] The liquid outlet of the irradiation container is connected to the liquid inlet of the buffer bottle 10 through a first pipeline, and the liquid outlet of the buffer bottle 10 is connected to the liquid inlet of the irradiation container through a second pipeline to form a liquid circulation system;

[0067] The liquid conveying equipment is arranged in the liquid circulation system to drive the liquid to circulate in the liquid circulation system; the liquid conveying equipment can be of various types, for example: a conveying equipment composed of one or more peristaltic pumps, or a conveying equipment composed of one or more pneumatic conveying pumps.

[0068] This test device is used for exogenous method research. During the irradiation test of the sample, the sample is driven to circulate in the liquid circulation system through the liquid delivery equipment, and can be fully mechanically mixed to improve the uniformity of irradiation and ensure that the temperature difference between different parts of the sample is small; at the same time, the thermostat 9 can be used to exchange heat with the sample in the buffer bottle 10 to effectively control the temperature of the sample in the liquid circulation system.

[0069] For example Figure 1 As shown, in some embodiments, the irradiation container includes an irradiation bottle 1 and a piston driver 3. The irradiation bottle 1 is arranged horizontally, with a thin film window at one end serving as an irradiation surface 24. A piston is disposed within the irradiation bottle 1, forming an irradiation chamber between the piston and the irradiation surface 24. The piston driver 3 is in driving connection with the piston and is capable of driving the piston axially to adjust the volume of the irradiation chamber. The piston driver 3 can be of various types, such as a pneumatic cylinder, an electric push rod, a ball screw pair, a crank slider mechanism, and the like. The irradiation container of the above structure can adjust the volume of the irradiation chamber according to test requirements to accommodate different irradiation conditions and / or sample doses. This not only improves the irradiation effect, but also, by precisely controlling the volume, enables better data analysis, thereby increasing the reliability of the test results.

[0070] Based on the previous embodiment, the film window is preferably made of a polyimide material, more preferably a film called Kapton. A polytetrafluoroethylene (PTFE) O-ring for sealing and an annular end cap for securing the film window to the end of the irradiation bottle 1 are provided at the connection between the film window and the end of the irradiation bottle 1. The annular end cap is generally detachably connected to the end of the irradiation bottle 1, such as by a threaded connection, a snap connection, or a clamp connection. This not only seals the irradiation chamber while allowing the irradiation beam, such as alpha particles, to penetrate into the irradiation chamber, but also facilitates replacement of the film window and the polytetrafluoroethylene (PTFE) O-ring by securing the film window to the end of the irradiation bottle 1.

[0071] To facilitate the discharge and collection of gaseous radiolysis products, based on the previous embodiment, the top of the irradiation bottle 1 is provided with a vent connected to the irradiation chamber, and a vent valve is installed at the vent. When the gaseous radiolysis products need to be discharged, the vent valve is opened. Typically, a gas collection container is connected to the vent to collect the gaseous radiolysis products generated during the irradiation process.

[0072] Based on the previous embodiment, the piston driver 3 is preferably a linear motor with smooth operation, precise control and fast response; the piston is connected to a piston rod extending from the other end of the irradiation bottle 1 and is connected to the linear motor through the piston rod.

[0073] In order to facilitate the operator to read the volume of the irradiation chamber, preferably, a scale line representing the volume of the irradiation chamber is provided on the linear motor, and the scale line is generally arranged along the axial direction of the linear motor.

[0074] For example Figure 1 As shown, in some embodiments, thermostat 9 is preferably a constant-temperature metal bath with stable and rapid temperature control. A temperature control panel 8 is provided on the front of the constant-temperature metal bath, and a thermocouple is provided in the temperature control tank of the constant-temperature metal bath. The thermocouple is communicatively connected to the temperature control panel 8. The advantages of using a constant-temperature metal bath include: small size and rapid temperature control; the thermocouple can monitor the temperature of the liquid in real time during the irradiation process for precise temperature control.

[0075] For example Figure 1 As shown, in some embodiments, the test apparatus further includes a container stand and an apparatus box 22 with rollers 23. The container stand includes a horizontal adjustment rod 7 mounted on the side of the apparatus box 22, a vertical adjustment rod 5 connected to the horizontal adjustment rod 7 via an adjustable fixing clamp 6, and a support platform 4 mounted on top of the vertical adjustment rod 5. The irradiation container is mounted on the surface of the support platform 4, and a thermostat 9 is mounted on the top surface of the apparatus box 22. The container stand, primarily composed of the horizontal adjustment rod 7, the adjustable fixing clamp 6, and the vertical adjustment rod 5, facilitates adjustment of the height and horizontal position of the support platform 4 and the irradiation container mounted thereon, thereby facilitating effective penetration of the irradiation beam into the irradiation chamber to irradiate the liquid. The apparatus box 22 with rollers 23 not only enables the flexible movement of the test apparatus and allows docking with irradiation output equipment such as an accelerator, but also facilitates storage of test instruments and / or placement of control components of the test apparatus.

[0076] To improve the stability and load-bearing capacity of the test device, based on the previous embodiment, the number of rollers 23 is preferably four, and the four rollers 23 are distributed in a rectangular array at the bottom of the device box 22. The rollers 23 can be of various types. To facilitate flexible steering during movement of the test device and stable fixation during operation, the rollers 23 are preferably universal wheels with brakes.

[0077] For example Figure 1As shown, in some embodiments, the test device further includes a solvent bottle 19, a gas cylinder 21, a multi-channel solenoid valve 11 and a multi-channel switching valve 15 with a switching motor 16; there are at least six solvent bottles 19, of which at least two solvent bottles 19 are used to store two or more liquids to be irradiated, at least two solvent bottles 19 are used to collect irradiated liquids, at least one solvent bottle 19 is used to store cleaning liquid, and at least one solvent bottle 19 is used to store waste cleaning liquid; the multi-channel solenoid valve 11 has at least eight valve ports; the multi-channel switching valve 15 has at least five valve ports; the first pipeline includes a first hose connecting the liquid outlet of the irradiation container to one of the valve ports of the multi-channel solenoid valve 11, and a hose connecting the multi-channel solenoid valve 15 to the liquid outlet of the irradiation container. 11 is connected to the liquid inlet of the buffer bottle 10; the second pipeline includes a third hose connecting the liquid outlet of the buffer bottle 10 to one of the valve ports of the multi-channel switching valve 15, a fourth hose connecting one of the valve ports of the multi-channel switching valve 15 to one of the valve ports of the multi-channel solenoid valve 11, and a fifth hose 2 connecting one of the valve ports of the multi-channel solenoid valve 11 to the liquid inlet of the irradiation container; a solvent bottle 19 for collecting irradiated liquid and a solvent bottle 19 for storing waste cleaning liquid are respectively connected to the valve ports of the multi-channel solenoid valve 11, and the remaining solvent bottles 19 are respectively connected to the valve ports of the multi-channel switching valve 15; a gas cylinder 21 is connected to one of the valve ports of the multi-channel solenoid valve 11.

[0078] Gas cylinder 21 contains a gas used to blow liquid out of the liquid circulation system. This gas is typically an inert gas, preferably argon (Ar). The first, second, third, fourth, and fifth hoses are typically made of a chemically inert material, preferably soft and corrosion-resistant Teflon. They are typically removable during installation for easy replacement. By controlling the multi-channel solenoid valve 11 and the multi-channel switching valve 15, different flow paths can be arranged and combined, such as a liquid circulation system addition path, a liquid circulation path, a liquid circulation path, a liquid circulation system discharge path, and so on. This allows the test device, driven by the liquid delivery device, to perform functions such as sample addition, sample circulation, online collection, and non-stop sample replacement.

[0079] For example Figure 1 As shown, in some embodiments, the test device also includes a porous hose connector 17, a storage box 18 and a gas cylinder rack 20; at least two solvent bottles 19 are used to store cleaning fluid, and the solvent bottles 19 for storing cleaning fluid are connected to the valve port of the multi-channel switching valve 15 through the porous hose connector 17; the storage box 18 is arranged on the top surface of the device box 22, and each solvent bottle 19 is placed in the storage box 18; the gas cylinder rack 20 is arranged on the side of the device box 22, and the gas cylinder 21 is arranged on the gas cylinder rack 20.

[0080] For example Figure 1As shown, in some embodiments, the test apparatus further includes a support plate 14 disposed on the top surface of the apparatus box 22; the liquid delivery equipment includes a first peristaltic pump 12 disposed on the fourth hose and a second peristaltic pump 13 disposed on the second hose; the multi-channel solenoid valve 11, the multi-channel switching valve 15, the first peristaltic pump 12, and the second peristaltic pump 13 are all disposed on the support plate 14. The first peristaltic pump 12 is primarily used to pump liquid into the irradiation container, while the second peristaltic pump 13 is primarily used to pump liquid from the irradiation container into the buffer bottle 10. By adjusting the rotational speed of the two peristaltic pumps, the amount of liquid pumped in and out can be substantially equal, achieving dynamic balance in liquid circulation during the irradiation process. The adjustable speed range of both the first and second peristaltic pumps 12, 13 is 0 to 3000 rpm. The liquid delivery equipment, primarily composed of the first and second peristaltic pumps 12, 13, achieves contamination-free liquid delivery and is easy to install and maintain.

[0081] In some embodiments, the test apparatus further includes an accelerator for emitting an irradiation beam; the irradiation surface 24 corresponds to the beam exit portion of the accelerator.

[0082] In some embodiments, the test apparatus further includes a remote control panel; a local control panel with an emergency stop button is provided on the apparatus box 22; and the remote control panel is communicatively connected to the local control panel. Through the remote control panel, an operator can remotely control the test apparatus and edit one-button shortcut programs, such as automatic liquid extraction, automatic sampling, automatic circulation, and automatic cleaning. The computer program involved in implementing these one-button operations can be edited and controlled according to the following liquid temperature-controlled cyclic irradiation test method or the method provided in Example 1 of the present invention. The selection of a specific programming language and the writing of the code are conventional techniques and are not elaborated here.

[0083] A liquid temperature-controlled cyclic irradiation test method, which uses the liquid temperature-controlled cyclic irradiation test device provided by the present invention to perform irradiation testing, including a liquid filling process, a temperature-controlled irradiation process, and a pipeline cleaning process;

[0084] The liquid filling process is as follows: the liquid to be irradiated is filled into at least one solvent bottle 19, and the cleaning liquid is filled into at least one solvent bottle 19; the liquid to be irradiated is usually an extraction system sample;

[0085] The temperature-controlled irradiation process includes the following steps:

[0086] A1. Control the multi-channel switching valve 15 and the multi-channel solenoid valve 11 to connect one of the solvent bottles 19 containing the liquid to be irradiated to the liquid circulation system. Then, the liquid to be irradiated in the solvent bottle 19 is pumped into the liquid circulation system through the liquid delivery device. After all the liquid to be irradiated in the solvent bottle 19 has entered the liquid circulation system, the passage between the solvent bottle 19 and the liquid circulation system is cut off.

[0087] A2. The irradiation beam is directed through the irradiation surface 24 to irradiate the liquid in the irradiation chamber of the irradiation container. Simultaneously, the liquid is driven to circulate in the liquid circulation system by the liquid delivery device, and heat is exchanged with the liquid in the buffer bottle 10 through the thermostat 9 to maintain the temperature of the liquid in the liquid circulation system at a set temperature of ±5°C, with a range of -100°C ≤ set temperature ≤ 100°C. Commonly used set temperatures are 25°C and 50°C.

[0088] A3. After irradiation is completed, the multi-channel switching valve 15 and the multi-channel solenoid valve 11 are controlled to connect one of the empty solvent bottles 19 to the liquid circulation system. The irradiated liquid in the liquid circulation system is then pumped into the solvent bottle 19 for storage through the liquid delivery device. After all the irradiated liquid in the liquid circulation system has entered the solvent bottle 19, the passage between the solvent bottle 19 and the liquid circulation system is cut off.

[0089] The pipeline cleaning process includes the following steps:

[0090] B1. After the temperature-controlled irradiation process is completed, the multi-channel switching valve 15 and the multi-channel solenoid valve 11 are controlled to connect the solvent bottle 19 containing the cleaning liquid to the liquid circulation system. The cleaning liquid in the solvent bottle 19 is then pumped into the irradiation container through the liquid delivery device, and then the connection between the solvent bottle 19 and the liquid circulation system is cut off.

[0091] B2. Pumping the cleaning liquid in the irradiation container into the buffer bottle 10 through the liquid conveying equipment;

[0092] B3. Control the multi-channel switching valve 15 and the multi-channel solenoid valve 11 to connect one of the empty solvent bottles 19 to the liquid circulation system, and then pump the cleaning liquid in the buffer bottle 10 into the solvent bottle 19 through the liquid delivery device to complete the storage of the waste cleaning liquid;

[0093] B4. Repeat steps B1 to B3 to clean the liquid circulation system three or more times;

[0094] B5. Control the multi-channel switching valve 15 and the multi-channel solenoid valve 11 to connect the gas cylinder 21 with the liquid circulation system, and use the gas in the gas cylinder 21 to blow the residual liquid in the liquid circulation system into the solvent bottle 19 storing the waste cleaning liquid, and then cut off the passage between the solvent bottle 19 and the liquid circulation system.

[0095] In some embodiments, the method further comprises an online sample exchange irradiation step;

[0096] The liquid filling process is as follows: two or more liquids to be irradiated are filled into different solvent bottles 19, and a cleaning liquid is filled into at least one solvent bottle 19;

[0097] The online sample-changing irradiation process is as follows: one of the liquids to be irradiated is irradiated according to the temperature-controlled irradiation process and the liquid circulation system is cleaned through the pipeline cleaning process, and then the temperature-controlled irradiation process is repeated to irradiate another liquid to be irradiated and the liquid circulation system is cleaned through the pipeline cleaning process.

[0098] Conducting experiments according to the above method can realize online collection of irradiated samples and sample replacement without stopping the machine, which greatly improves the irradiation efficiency.

[0099] Example 1

[0100] Combine Figure 1 and Figure 2 As shown, the liquid temperature-controlled cyclic irradiation test device includes an irradiation container with an irradiation surface 24, a thermostat 9, a buffer bottle 10, a liquid conveying device, a container rack, a device box 22 with rollers 23, a support plate 14, a solvent bottle 19, a gas cylinder 21, a multi-channel solenoid valve 11, and a multi-channel switching valve 15 with a switching motor 16;

[0101] The container rack includes a horizontal adjustment rod 7 provided on the side of the device box 22, a vertical adjustment rod 5 connected to the horizontal adjustment rod 7 via an adjustable fixing clamp 6, and a support platform 4 provided on the top of the vertical adjustment rod 5;

[0102] The irradiation container is arranged on the table of the support table 4; the irradiation container includes an irradiation bottle 1 and a piston driver 3; the irradiation bottle 1 is arranged horizontally, and a film window is provided at one end of the irradiation bottle 1 as an irradiation surface 24. A piston is provided in the irradiation bottle 1, and an irradiation chamber is formed between the piston and the irradiation surface 24; the piston driver 3 is in transmission connection with the piston, and can drive the piston to move axially to adjust the volume of the irradiation chamber; the top of the irradiation bottle 1 is provided with an exhaust hole connected to the irradiation chamber, and an exhaust valve is provided at the exhaust hole;

[0103] The thermostat 9 is provided on the top surface of the device box 22; the thermostat 9 is a constant temperature metal bath, a temperature control panel 8 is provided on the front of the constant temperature metal bath, a thermocouple is provided in the temperature control tank of the constant temperature metal bath, and the thermocouple is communicated with the temperature control panel 8;

[0104] The buffer bottle 10 is arranged in the temperature control tank of the thermostat 9;

[0105] There are at least seven solvent bottles 19, three of which are used to store three liquids to be irradiated and are marked as #1, #2, and #3, respectively; at least two of which are used to collect irradiated liquids and one of which is marked as #6; two of which are used to store cleaning liquids and are marked as #4 and #5, respectively; and one of which is used to store waste cleaning liquid and is marked as #7;

[0106] The multi-channel solenoid valve 11 is composed of a two-position three-way solenoid valve and a two-position five-way two-way solenoid valve, wherein the valve ports of the two-position three-way solenoid valve are marked as #1, #2, and #3 respectively, and the valve ports of the two-position five-way two-way solenoid valve are marked as #4, #5, #6, #7, and #8 respectively;

[0107] The multi-channel switching valve 15 has eleven valve ports, one of which is an output port and the others are input ports and are sequentially labeled #1 to #10.

[0108] The liquid outlet of the irradiation container is connected to the liquid inlet of the buffer bottle 10 through a first pipeline, and the liquid outlet of the buffer bottle 10 is connected to the liquid inlet of the irradiation container through a second pipeline, forming a liquid circulation system; the first pipeline includes a first hose connecting the liquid outlet of the irradiation container to the #5 valve port of the multi-channel solenoid valve 11, and a second hose connecting the #4 valve port of the multi-channel solenoid valve 11 to the liquid inlet of the buffer bottle 10; the second pipeline includes a third hose connecting the liquid outlet of the buffer bottle 10 to the #1 valve port of the multi-channel switching valve 15, a fourth hose connecting the valve port of the multi-channel switching valve 15 as an output port to the #2 valve port of the multi-channel solenoid valve 11, and a fifth hose 2 connecting the #1 valve port of the multi-channel solenoid valve 11 to the liquid inlet of the irradiation container;

[0109] The #1 solvent bottle 19 is connected to the #6 valve port of the multi-channel switching valve 15, the #2 solvent bottle 19 is connected to the #7 valve port of the multi-channel switching valve 15, the #3 solvent bottle 19 is connected to the #8 valve port of the multi-channel switching valve 15, the #4 solvent bottle 19 and the #5 solvent bottle 19 are connected to the #9 valve port of the multi-channel switching valve 15 via the porous hose connector 17, the #6 solvent bottle 19 is connected to the #7 valve port of the multi-channel solenoid valve 11, the #7 solvent bottle 19 is connected to the #6 valve port of the multi-channel solenoid valve 11, and the gas cylinder 21 is connected to the #8 valve port of the multi-channel solenoid valve 11; the #3 valve port of the multi-channel solenoid valve 11 is reserved;

[0110] The liquid delivery device is arranged in the liquid circulation system, and is used to drive the liquid to circulate in the liquid circulation system; the liquid delivery device includes a first peristaltic pump 12 arranged on the fourth hose and a second peristaltic pump 13 arranged on the second hose;

[0111] The support plate 14 is disposed on the top surface of the device box 22 , and the multi-channel solenoid valve 11 , the multi-channel switching valve 15 , the first peristaltic pump 12 and the second peristaltic pump 13 are all disposed on the support plate 14 .

[0112] Liquid temperature-controlled cyclic irradiation test method, wherein the liquid temperature-controlled cyclic irradiation test device is used to perform irradiation test, including liquid filling process, temperature-controlled irradiation process, pipeline cleaning process and online sample replacement irradiation process;

[0113] The liquid filling process is as follows: two different samples to be irradiated are placed in the #1 and #2 solvent bottles 19 respectively, and the cleaning liquid is placed in the #4 and #5 solvent bottles 19, all bottle stoppers are capped and the pipelines are connected to prepare for the test;

[0114] The temperature-controlled irradiation process includes the following steps:

[0115] A1. Control the multi-channel switching valve 15 and the multi-channel solenoid valve 11 to connect the #1 solvent bottle 19, the fourth hose, the fifth hose, the irradiation bottle 1, the first hose, and the buffer bottle 10 in sequence. Then, turn on the first peristaltic pump 12 and rotate it counterclockwise to pump the sample to be irradiated in the #1 solvent bottle 19 into the irradiation bottle 1. Turn on the second peristaltic pump 13 and rotate it clockwise to pump the sample in the irradiation bottle 1 into the buffer bottle 10. When all the sample in the #1 solvent bottle 19 enters the liquid circulation system, close the #6 valve port of the multi-channel switching valve 15 and open the #1 valve port. At this time, the sample in the buffer bottle 10 can be pumped back into the irradiation bottle 1 by the first peristaltic pump 12 to realize liquid circulation.

[0116] A2. Allow the α irradiation beam to pass through the irradiation surface 24 to irradiate the sample in the irradiation cavity of the irradiation container. Simultaneously, the sample is driven to circulate in the liquid circulation system by the liquid delivery device, and heat is exchanged with the sample in the buffer bottle 10 through the thermostat 9 to maintain the liquid temperature in the liquid circulation system at 50±5°C.

[0117] A3. After the irradiation is completed, the #5 and #4 valve ports of the multi-channel solenoid valve 11 are connected, and the second peristaltic pump 13 is turned on and rotated clockwise to pump all the samples in the irradiation bottle 1 into the buffer bottle 10 for temporary storage. After the irradiation is completed, the #5 and #4 valve ports of the multi-channel solenoid valve 11 are closed first, and the second peristaltic pump 13 is closed after a delay of 10 seconds; then, the #4 and #7 valve ports of the multi-channel solenoid valve 11 are connected, and the second peristaltic pump 13 is turned on and rotated counterclockwise to pump the sample in the buffer bottle 10 into the #6 solvent bottle 19 for collection; after the collection is completed, the #4 and #7 valve ports of the multi-channel solenoid valve 11 are closed, and the second peristaltic pump 13 is closed; gas collection: before the irradiation test begins, the gas collection container is connected to the exhaust port of the irradiation bottle 1, and the exhaust valve is opened. The gas radiolysis products generated during the irradiation test can be collected in the gas collection container. After the test is completed, the exhaust valve is closed to complete the gas collection;

[0118] The pipeline cleaning process includes the following steps:

[0119] B1. After the temperature-controlled irradiation process is completed, the multi-channel switching valve 15 and the multi-channel solenoid valve 11 are controlled to connect the #4 and #5 solvent bottles 19, the fourth hose, the fifth hose, and the irradiation bottle 1 in sequence, and then the first peristaltic pump 12 is started to rotate counterclockwise to pump the cleaning solution into the irradiation bottle 1. After completion, the #9 valve port of the multi-channel switching valve 15 is first closed, and after a delay of 10 seconds, the first peristaltic pump 12 is turned off, and then the #2 and #1 valve ports of the multi-channel solenoid valve 11 are closed.

[0120] B2. Control the multi-channel switching valve 15 and the multi-channel solenoid valve 11 to connect the irradiation bottle 1, the first hose, and the buffer bottle 10 in sequence. Then start the second peristaltic pump 13 and rotate it clockwise to pump all the cleaning liquid in the irradiation bottle 1 into the buffer bottle 10. After the cleaning liquid is completely pumped out, close the #5 and #4 valve ports of the multi-channel solenoid valve 11 first, and then turn off the second peristaltic pump 13 after a delay of 10 seconds.

[0121] B3. Control the multi-channel switching valve 15 and the multi-channel solenoid valve 11, connect the #4 and #6 valve ports of the multi-channel solenoid valve 11, start the second peristaltic pump 13 to rotate counterclockwise, and drain all the cleaning liquid from the buffer bottle 10 and collect it in the #7 solvent bottle 19. After completion, close the #4 and #6 ports of the multi-channel solenoid valve 11 and the second peristaltic pump 13;

[0122] B4. Repeat steps B1 to B3 to clean the liquid circulation system three times;

[0123] B5. Control multi-channel switching valve 15 and multi-channel solenoid valve 11, connect valve ports #8 and #6 of multi-channel solenoid valve 11, connect gas cylinder 21 to the liquid circulation system, and use the gas in gas cylinder 21 to blow the remaining liquid in the liquid circulation system into solvent bottle #7 19. Then, cut off the passage between solvent bottle #7 19 and the liquid circulation system.

[0124] The online sample change irradiation process is as follows: the sample in the #1 solvent bottle 19 is irradiated according to the temperature control irradiation process and the liquid circulation system is cleaned through the pipeline cleaning process, and then the temperature control irradiation process is repeated to irradiate the sample in the #2 solvent bottle 19 and the liquid circulation system is cleaned through the pipeline cleaning process to achieve online sample change irradiation.

[0125] The description of various embodiments of the present invention is presented herein for illustrative purposes only and is not intended to be exhaustive or limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments. The terms used herein are selected to best explain the principles of the embodiments, practical applications, or technological advancements, or to enable others skilled in the art to understand the embodiments disclosed herein, as compared to commercially available technology.

[0126] In this article, various embodiments of the present invention may be presented in the form of ranges. It should be understood that the description in range form is merely for convenience and brevity and should not be construed as a hard limit to the scope of the invention. Therefore, the description of a range should be considered to specifically disclose all possible sub-ranges and individual values within the range. For example, a description of a range such as from 1 to 6 should be considered to specifically disclose sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as individual values within the range, such as 1, 2, 3, 4, 5, 6, which has nothing to do with the width of the range.

[0127] It should be understood that certain features of the invention described in the context of separate embodiments for the sake of clarity may also be provided in combination in a single embodiment. Conversely, various features of the invention described in the context of a single embodiment for the sake of brevity may also be provided individually or in any suitable subcombination, or in any other described embodiment of the invention, where appropriate. Certain features described in the context of various embodiments are not considered essential features of those embodiments unless the embodiment would not function without those features.

Claims

1. A liquid temperature-controlled cyclic irradiation test device comprising an irradiation container having an irradiation surface (24), characterized in that: It also includes a thermostat (9), a buffer bottle (10) and a liquid delivery device; The buffer bottle (10) is arranged in the temperature control tank of the thermostat (9); The liquid outlet of the irradiation container is connected to the liquid inlet of the buffer bottle (10) through a first pipeline, and the liquid outlet of the buffer bottle (10) is connected to the liquid inlet of the irradiation container through a second pipeline, forming a liquid circulation system; The liquid delivery device is arranged in the liquid circulation system and is used to drive the liquid to circulate in the liquid circulation system.

2. The liquid temperature-controlled cyclic irradiation test device according to claim 1, characterized in that: The irradiation container comprises an irradiation bottle (1) and a piston driver (3); The irradiation bottle (1) is arranged horizontally, and a film window is provided at one end of the irradiation bottle (1) as an irradiation surface (24). A piston is provided in the irradiation bottle (1), and an irradiation chamber is formed between the piston and the irradiation surface (24); The piston driver (3) is in driving connection with the piston and can drive the piston to move axially to adjust the volume of the irradiation chamber.

3. The liquid temperature-controlled cyclic irradiation test device according to claim 2, characterized in that: The film window is made of polyimide material, and a polytetrafluoroethylene O-ring for sealing and an annular end cap for fixing are provided at the connection between the film window and the end of the irradiation bottle (1); And / or, the top of the irradiation bottle (1) is provided with an exhaust hole connected to the irradiation chamber, and an exhaust valve is provided at the exhaust hole.

4. The liquid temperature-controlled cyclic irradiation test device according to claim 1, characterized in that: The thermostat (9) is a constant temperature metal bath, a temperature control panel (8) is provided on the front of the constant temperature metal bath, a thermocouple is provided in the temperature control tank of the constant temperature metal bath, and the thermocouple is communicatively connected to the temperature control panel (8).

5. The liquid temperature-controlled cyclic irradiation test device according to any one of claims 1 to 4, characterized in that: Also included is a container rack and a device box (22) with rollers (23); The container rack includes a horizontal adjustment rod (7) arranged on the side of the device box (22), a vertical adjustment rod (5) connected to the horizontal adjustment rod (7) through an adjustable fixing clamp (6), and a support platform (4) arranged on the top of the vertical adjustment rod (5); The irradiation container is arranged on the table of the support table (4); The thermostat (9) is arranged on the top surface of the device box (22).

6. The liquid temperature-controlled cyclic irradiation test device according to claim 5, characterized in that: It also includes a solvent bottle (19), a gas bottle (21), a multi-channel electromagnetic valve (11), and a multi-channel switching valve (15) with a switching motor (16); There are at least six solvent bottles (19), at least two of which are used to store two or more liquids to be irradiated, at least two of which are used to collect irradiated liquids, at least one of which is used to store cleaning liquid, and at least one of which is used to store waste cleaning liquid; The multi-channel solenoid valve (11) has at least eight valve ports; The multi-channel switching valve (15) has at least five valve ports; The first pipeline comprises a first hose connecting the liquid outlet of the irradiation container with one of the valve ports of the multi-channel solenoid valve (11), and a second hose connecting one of the valve ports of the multi-channel solenoid valve (11) with the liquid inlet of the buffer bottle (10); The second pipeline comprises a third hose connecting the liquid outlet of the buffer bottle (10) to one of the valve ports of the multi-channel switching valve (15), a fourth hose connecting one of the valve ports of the multi-channel switching valve (15) to one of the valve ports of the multi-channel solenoid valve (11), and a fifth hose (2) connecting one of the valve ports of the multi-channel solenoid valve (11) to the liquid inlet of the irradiation container; A solvent bottle (19) for collecting irradiated liquid and a solvent bottle (19) for storing waste cleaning liquid are respectively connected to the valve ports of the multi-channel electromagnetic valve (11), and the remaining solvent bottles (19) are respectively connected to the valve ports of the multi-channel switching valve (15); The gas cylinder (21) is connected to one of the valve ports of the multi-channel electromagnetic valve (11).

7. The liquid temperature-controlled cyclic irradiation test device according to claim 6, characterized in that: It also includes a porous hose connector (17), a storage box (18) and a gas cylinder stand (20); At least two solvent bottles (19) are used to store cleaning liquid, and the solvent bottles (19) for storing cleaning liquid are connected to the valve ports of the multi-channel switching valve (15) through a porous hose connector (17); The storage box (18) is arranged on the top surface of the device box (22), and each solvent bottle (19) is placed in the storage box (18); The gas cylinder rack (20) is arranged on the side of the device box (22), and the gas cylinder (21) is arranged on the gas cylinder rack (20).

8. The liquid temperature-controlled cyclic irradiation test device according to claim 6, characterized in that: It also includes a support plate (14) arranged on the top surface of the device box (22); The liquid delivery device comprises a first peristaltic pump (12) arranged on a fourth hose and a second peristaltic pump (13) arranged on a second hose; The multi-channel solenoid valve (11), the multi-channel switching valve (15), the first peristaltic pump (12) and the second peristaltic pump (13) are all arranged on a support plate (14).

9. Liquid temperature controlled cyclic irradiation test method, characterized by: The method uses the liquid temperature-controlled cycle irradiation test device according to any one of claims 6 to 8 to perform irradiation testing, including a liquid filling process, a temperature-controlled irradiation process, and a pipeline cleaning process; The liquid filling process comprises: filling the liquid to be irradiated into at least one solvent bottle (19), and filling the cleaning liquid into at least one solvent bottle (19); The temperature-controlled irradiation process comprises the following steps: A1, controlling the multi-channel switching valve (15) and the multi-channel solenoid valve (11) so that one of the solvent bottles (19) containing the liquid to be irradiated is connected to the liquid circulation system, then pumping the liquid to be irradiated in the solvent bottle (19) into the liquid circulation system through the liquid delivery device, and after all the liquid to be irradiated in the solvent bottle (19) enters the liquid circulation system, cutting off the passage between the solvent bottle (19) and the liquid circulation system; A2. The irradiation beam is passed through the irradiation surface (24) to irradiate the liquid in the irradiation chamber of the irradiation container, and at the same time, the liquid is driven to circulate in the liquid circulation system through the liquid delivery device, and heat is exchanged with the liquid in the buffer bottle (10) through the thermostat (9) so that the temperature of the liquid in the liquid circulation system is maintained at a set temperature ±5°C, and -100°C ≤ set temperature ≤ 100°C; A3. After the irradiation is completed, the multi-channel switching valve (15) and the multi-channel solenoid valve (11) are controlled to connect one of the empty solvent bottles (19) to the liquid circulation system, and then the irradiated liquid in the liquid circulation system is pumped into the solvent bottle (19) for storage through the liquid conveying device. After all the irradiated liquid in the liquid circulation system has entered the solvent bottle (19), the passage between the solvent bottle and the liquid circulation system is cut off; The pipeline cleaning process includes the following steps: B1. After the temperature-controlled irradiation process is completed, the multi-channel switching valve (15) and the multi-channel solenoid valve (11) are controlled to connect the solvent bottle (19) containing the cleaning liquid to the liquid circulation system, and then the cleaning liquid in the solvent bottle (19) is first pumped into the irradiation container through the liquid delivery device, and then the passage between the solvent bottle (19) and the liquid circulation system is cut off; B2. Pumping the cleaning liquid in the irradiation container into the buffer bottle (10) through the liquid conveying equipment; B3, controlling the multi-channel switching valve (15) and the multi-channel solenoid valve (11) to connect one of the empty solvent bottles (19) to the liquid circulation system, and then pumping the cleaning liquid in the buffer bottle (10) into the solvent bottle (19) through the liquid delivery device to complete the storage of the waste cleaning liquid; B4. Repeat steps B1 to B3 to clean the liquid circulation system three or more times; B5, controlling the multi-channel switching valve (15) and the multi-channel solenoid valve (11) to connect the gas cylinder (21) to the liquid circulation system, blowing the liquid remaining in the liquid circulation system into the solvent bottle (19) storing the waste cleaning liquid through the gas in the gas cylinder (21), and then cutting off the passage between the solvent bottle (19) and the liquid circulation system.

10. The liquid temperature-controlled cyclic irradiation test method according to claim 9, characterized in that: The method also includes an online sample changing irradiation process; The liquid filling process comprises: filling two or more liquids to be irradiated into different solvent bottles (19), and filling at least one solvent bottle (19) with a cleaning liquid; The online sample-changing irradiation process is as follows: after one liquid to be irradiated is irradiated according to the temperature-controlled irradiation process and the liquid circulation system is cleaned through the pipeline cleaning process, the temperature-controlled irradiation process is repeated to irradiate another liquid to be irradiated and the liquid circulation system is cleaned through the pipeline cleaning process.

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