Micro-droplet ice-gas interface forming and detecting device and method thereof

Abstract

The invention provides a micro-droplet ice-gas interface forming and detecting device which comprises a sample feeding pipe, the tail end of the sample feeding pipe is communicated with a first circulating pipe, and the first circulating pipe is provided with a first gas passage perpendicular to the first circulating pipe; a second runner pipe is arranged at the tail end of the first runner pipe, the second runner pipe is arranged in a double-layer mode and comprises an inner layer and an outer layer, the inner layer is communicated with the first runner pipe, a cooling medium circulates in the outer layer in a circulating mode, and a second gas channel is further formed in the second runner pipe and communicated with the inner layer; the tail end of the inner layer is communicated with a detection instrument. The invention further provides a micro-droplet ice-gas interface forming and detecting method, and the micro-droplet ice-gas interface forming and detecting device is used in the micro-droplet ice-gas interface forming and detecting method. Formation, reaction and detection of the micro-droplet ice-gas interface are combined, online reaction, real-time detection and in-situ analysis of the micro-droplet ice-gas interface are achieved, operation is simple, and the accuracy of an analysis result is improved; belongs to the technical field of ice-gas interface reaction.

Description

Technical Field

[0001] The present invention belongs to the technical field of ice-air interface reaction, and in particular relates to a micro-droplet ice-air interface formation and detection device and method. Background Art

[0002] Most of the water on Mars and its polar regions exists in the form of ice. With the increasing number of deep space exploration missions both domestically and internationally, the water-ice environment and habitability of Mars are attracting increasing attention. Research on the Martian ice-air interface can provide insights into Mars' climate evolution history, habitability, and other aspects, as well as support future Mars exploration missions. Research on the polar ice-air interface can also provide a deeper understanding of the characteristics of the polar regions and contribute to their protection. Furthermore, some reactions that are difficult to occur in a homogeneous phase can occur heterogeneously at the ice-air interface. Therefore, studying ice-air interface reactions is of great significance.

[0003] The unique properties and high specific surface area of ​​microdroplets make certain chemical reactions or physical processes more efficient. By combining microdroplets with ice-air interface reactions, freezing micron-sized droplets and allowing reactions to occur at the ice-air interface, the high specific surface area of ​​the microdroplets significantly increases the contact area with the ice-air interface, thereby increasing the exchange rate of reactants. This makes chemical reactions or physical processes at the ice-air interface more efficient. Therefore, studying reactions at the microdroplet ice-air interface has far-reaching significance.

[0004] Currently, when studying reactions at microdroplet ice-air interfaces, a microdroplet generation device is typically used to generate microdroplets from a sample solution. These microdroplets are then frozen and reacted, and the reacted microdroplets are then transferred to a detection instrument for analysis. However, this method is cumbersome, and careless operation can lead to loss or changes in the microdroplets, resulting in low accuracy in the analysis results. Given this, there is an urgent need to develop a microdroplet ice-air interface reaction and detection device that can combine the formation, reaction, and detection of microdroplet ice-air interfaces. Summary of the Invention

[0005] The purpose of the present invention is to provide a micro-droplet ice-air interface formation and detection device and method thereof, aiming to solve the technical problems of the prior art such as complicated steps and low accuracy of analysis results.

[0006] To achieve the above-mentioned purpose, the technical solution adopted by the present invention is: to provide a micro-droplet ice-gas interface formation and detection device, including an inlet tube, the end of the inlet tube is connected to a first flow tube, and the first flow tube is provided with a first gas passage arranged perpendicular to it; the end of the first flow tube is provided with a second flow tube, and the second flow tube is a double-layer arrangement, including an inner layer and an outer layer, the inner layer is connected to the first flow tube, and a cooling medium circulates in the outer layer, and the second flow tube is also provided with a second gas passage, and the second gas passage is connected to the inner layer; the end of the inner layer is connected to a detection instrument.

[0007] In one embodiment, a heating material is coated on the inner wall of the inner layer, a wire is connected to the heating material, a heater is provided on the outside of the second flow tube, and the wire is connected to the heater.

[0008] In one embodiment, a temperature sensor is provided inside the inner layer, and the temperature sensor is electrically connected to the heater via a PID controller.

[0009] In one embodiment, a cooling medium inlet and a cooling medium outlet are provided on the outer wall of the second circulation tube, and both the cooling medium inlet and the cooling medium outlet are communicated with the outer layer.

[0010] In one embodiment, the temperature inside the inner layer is -210-0°C.

[0011] In one embodiment, a filter is provided at the connection between the second gas passage and the inner layer, and the filter is a micron-grade filter.

[0012] In one embodiment, the sample injection tube is a capillary tube; the detection instrument is provided with a detection instrument inlet, and the end of the inner layer is connected to the detection instrument inlet.

[0013] The present invention also provides a method for forming and detecting a micro-droplet ice-air interface, using any of the above-described micro-droplet ice-air interface forming and detecting devices, the method comprising the following steps:

[0014] S1: The sample solution is introduced into the sample inlet tube, and the first gas is introduced into the first gas passage. Under the high-pressure shearing action of the first gas, the sample solution forms a micro-droplet spray and is sent into the second flow tube;

[0015] S2: At the same time, a cooling medium is introduced into the outer layer. Under the action of the cooling medium, the micro-droplet spray is frozen into ice microspheres, and an ice-air interface is formed on the surface of the micro-droplet spray. The sample molecules in the micro-droplet spray react at the ice-air interface.

[0016] S3: At the same time, the second gas is introduced into the inner layer through the second gas passage. Under the action of the second gas, the ice microspheres are sent into the detection instrument for detection.

[0017] In one embodiment, in S1, the pressure of the first gas is 0.1-1.0 MPa.

[0018] In one embodiment, in S2, the cooling medium includes liquid nitrogen.

[0019] The present invention provides a micro-droplet ice-air interface formation and detection device and method. Compared with the prior art, the present invention has the following beneficial effects:

[0020] (1) The present invention combines the formation, reaction, and detection of the micro-droplet ice-air interface, thereby realizing online reaction, real-time detection, and in-situ analysis of the micro-droplet ice-air interface. The operation is simple and the accuracy of the analysis results is improved. In addition, during the detection process, the time for the micro-droplet spray to pass through the second flow tube can be controlled by adjusting the flow rate of the second gas, thereby controlling the reaction time. The dynamic changes in the reaction process can be captured, and online real-time detection and dynamic detection of the reaction can be realized, so as to conduct in-depth research on the reaction process and reaction mechanism.

[0021] (2) The present invention adjusts the cooling temperature in the second flow tube by setting a heating material, a heater, a temperature sensor and a PID controller for use in combination, so that the microdroplets can be smoothly frozen to form an ice-air interface, thereby allowing the reaction on the ice-air interface to proceed smoothly, thereby improving the sensitivity and response speed of the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments or descriptions of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0023] Figure 1 A schematic structural diagram of a micro-droplet ice-air interface formation and detection device provided in one embodiment of the present application;

[0024] Figure 2 for Figure 1 The schematic diagram of the structure of the micro-droplet ice-air interface formation and detection device in use is shown.

[0025] Explanation of symbols in the figure:

[0026] 1. Injection tube; 2. First circulation tube; 3. First gas passage; 4. Second circulation tube; 401. Inner layer; 402. Outer layer; 5. Second gas passage; 6. Detection instrument; 601. Detection instrument inlet; 7. Heating material; 8. Wire; 9. Heater; 10. Temperature sensor; 11. PID controller; 12. Cooling medium inlet; 13. Cooling medium outlet; 14. Filter; 15. Sample solution; 16. First gas; 17. Cooling medium; 18. Second gas; 19. Micro-droplet spray. DETAILED DESCRIPTION

[0027] In order to make the technical problems, technical solutions and beneficial effects to be solved by this application more clearly understood, this application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain this application and are not intended to limit this application.

[0028] It should be noted that when an element is referred to as being “fixed” or “disposed” on another element, it may be directly on the other element or indirectly on the other element. When an element is referred to as being “connected” to another element, it may be directly connected to the other element or indirectly connected to the other element.

[0029] It should be understood that the terms "length," "width," "up," "down," "front," "back," "left," "right," "vertical," "horizontal," "top," "bottom," "inside," "outside," and the like, indicating positions or relationships, are based on the positions or relationships shown in the accompanying drawings and are used solely for the purpose of facilitating and simplifying the description of this application. They should not be construed as indicating or implying that the devices or elements referred to must have a specific orientation, be constructed, or operate in a specific orientation. Therefore, they should not be construed as limiting this application. Furthermore, the terms "first," "second," "third," and the like are used solely for distinguishing descriptions and should not be construed as indicating or implying relative importance.

[0030] (1) Micro-droplet ice-air interface formation and detection device

[0031] A first aspect of the embodiments of the present application provides a micro-droplet ice-air interface formation and detection device.

[0032] See also Figure 1 , is a schematic diagram of the structure of a micro-droplet ice-air interface formation and detection device provided in one embodiment of the present application. For ease of explanation, only the parts related to this embodiment are shown, which are detailed as follows:

[0033] In one embodiment, please combine Figure 2A micro-droplet ice-gas interface formation and detection device includes an injection tube 1, the end of the injection tube 1 is connected to a first flow tube 2, and the first flow tube 2 is provided with a first gas passage 3 arranged perpendicularly thereto; the end of the first flow tube 2 is provided with a second flow tube 4, and the second flow tube 4 is a double-layer arrangement, including an inner layer 401 and an outer layer 402, the inner layer 401 is connected to the first flow tube 2, and a cooling medium 17 circulates in the outer layer 402, and a second gas passage 5 is also provided on the second flow tube 4, and the second gas passage 5 is connected to the inner layer 401; the end of the inner layer 401 is connected to a detection instrument 6.

[0034] The inlet end of the sample injection tube 1 is connected to a sample injection pump, which introduces a sample solution 15 into the sample injection tube 1. A first gas 16 is introduced into the first gas passage 3. The sample solution 15 is sheared by the high pressure of the first gas 16 to form a micro-droplet spray 19, which is then fed into the second flow tube 4. The first gas 16 can be high-pressure nitrogen or other high-pressure gases, such as compressed air or argon.

[0035] Cooling medium 17 in second flow tube 4 freezes microdroplet spray 19 into ice microspheres, forming an ice-air interface on their surface. Sample molecules in microdroplet spray 19 react at this interface. Second gas 18 flows into second gas passage 5 to control the movement of microdroplet spray 19 and the ice microspheres, delivering the reacted ice microspheres to detection instrument 6 for testing. Second gas 18 can be nitrogen or other gases, such as argon.

[0036] By setting up a second circulation tube 4, a second gas passage 5, and a detection instrument 6 for use in conjunction, the formation, reaction, and detection of the micro-droplet ice-gas interface are combined, thereby realizing online reaction, real-time detection, and in-situ analysis of the micro-droplet ice-gas interface. The operation is simple and the accuracy of the analysis results is improved. In addition, during the detection process, the time for the micro-droplet spray 19 to pass through the second circulation tube 4 can be controlled by adjusting the flow rate of the second gas 18, thereby controlling the reaction time, capturing dynamic changes in the reaction process, realizing online real-time detection and dynamic detection of the reaction, and conducting in-depth research on the reaction process and reaction mechanism.

[0037] For details, please refer to Figure 1-Figure 2 The sample injection tube 1 is a capillary tube. The high surface tension of the capillary tube facilitates the stable flow of the sample solution 15 within the sample injection tube 1. The small inner diameter of the capillary tube forms a high-speed stream of the sample solution 15 at its outlet. When the sample solution 15 comes into contact with the high-pressure first gas 16, the shearing effect of the first gas 16 is stronger, making it easier to form uniform micro-droplets.

[0038] The outer wall of the second circulation tube 4 is provided with a cooling medium inlet 12 and a cooling medium outlet 13, both of which are in communication with the outer layer 402. The cooling medium inlet 12 and the cooling medium outlet 13 enable the circulation of the cooling medium 17 within the outer layer 402, thereby cooling the inner layer 401 and creating a low-temperature cooling environment. This facilitates the rapid freezing of the micro-droplet spray 19 into ice microspheres, forming an ice-air interface on the surface of the micro-droplet spray 19, and facilitating the smooth reaction at the ice-air interface. The cooling medium 17 can be liquid nitrogen or other types of cooling media, such as dry ice.

[0039] The inner wall of inner layer 401 is coated with a heating material 7, to which a wire 8 is connected. A heater 9 is provided on the exterior of second flow tube 4, to which wire 8 is connected. A temperature sensor 10 is located within inner layer 401 and electrically connected to heater 9 via a PID controller 11. By combining heating material 7, heater 9, temperature sensor 10, and PID controller 11, the cooling temperature within inner layer 401 is regulated to a range of -210°C to 0°C, enabling the microdroplets to be successfully frozen to form an ice-air interface. This allows reactions at the ice-air interface to proceed smoothly, improving reaction sensitivity and response speed.

[0040] A filter 14 is provided at the connection between the second gas passage 5 and the inner layer 401. The filter 14 is a micron-grade filter and is used to prevent the micro-droplet spray 19 and ice microspheres from being discharged from the second gas passage 5 to the outside of the second flow pipe 4.

[0041] Detection instrument 6 is provided with a detection instrument inlet 601, to which the distal end of inner layer 401 is connected. The reacted ice microspheres are transported by second gas 18 into detection instrument inlet 601 and then into detection instrument 6 for detection. Detection instrument 6 can be a mass spectrometer, chromatograph, spectrometer, or other type of detector, and should be adjusted according to actual circumstances during operation.

[0042] During use, the sample solution 15 forms a micro-droplet spray 19 under the high-pressure shearing action of the first gas 16 and is sent into the second circulation tube 4; the micro-droplet spray 19 is frozen into ice microspheres under the action of the cooling medium 17, and an ice-air interface is formed on its surface. The sample molecules in the micro-droplet spray 19 react at the ice-air interface; the second gas 18 sends the reacted ice microspheres into the detection instrument 6 for detection.

[0043] The first gas 16 and the second gas 18 can be the same type of gas or different types of gas. By adjusting the type of the second gas 18, the gas phase composition during the reaction process can be flexibly changed to simulate different gas phase environments.

[0044] (2) Formation and detection methods of micro-droplet ice-air interface

[0045] A second aspect of the embodiments of the present application provides a method for forming and detecting a micro-droplet ice-air interface.

[0046] See also Figure 1-Figure 2 A method for forming and detecting a micro-droplet ice-air interface, using the above-mentioned micro-droplet ice-air interface formation and detection device, the method comprises the following steps:

[0047] S1: The sample solution 15 is introduced into the sample injection tube 1, and the first gas 16 is introduced into the first gas passage 3. Under the high-pressure shearing action of the first gas 16, the sample solution 15 forms a micro-droplet spray 19 and is sent into the second circulation tube 4.

[0048] Specifically, the inlet end of the sampling tube 1 is connected to an external sampling pump, and the sampling pump introduces the sample solution 15 into the sampling tube 1; at the same time, the high-pressure first gas 16 is introduced into the first gas passage 3; the sample solution 15 and the high-pressure first gas 16 meet in the first circulation tube 2, and the sample solution 15 forms a micro-droplet spray 19 under the high-pressure shearing action of the first gas 16 and is sent into the second circulation tube 4.

[0049] The injection tube 1 is a capillary tube. The first gas 16 can be high-pressure nitrogen or other types of high-pressure gases, such as compressed air, argon, etc. The pressure of the first gas 16 is 0.1-1.0 MPa.

[0050] S2: At the same time, the cooling medium 17 is introduced into the outer layer 402. Under the action of the cooling medium 17, the micro-droplet spray 19 is frozen into ice microspheres, an ice-air interface is formed on the surface of the micro-droplet spray 19, and the sample molecules in the micro-droplet spray 19 react at the ice-air interface.

[0051] Specifically, at the same time, the cooling medium 17 is introduced into the outer layer 402, and the cooling medium 17 circulates in the outer layer 402 to cool the inner layer 401, controlling its temperature at -210-0°C to create a low-temperature cooling environment; the micro-droplet spray 19 is frozen into ice microspheres under the action of the cooling medium 17, and an ice-air interface is formed on its surface, and the sample molecules in the micro-droplet spray 19 react at the ice-air interface.

[0052] The cooling medium 17 may be liquid nitrogen or other types of cooling media, such as dry ice.

[0053] S3: At the same time, the second gas 18 is introduced into the inner layer 401 through the second gas passage 5. Under the action of the second gas 18, the ice microspheres are sent to the detection instrument 6 for detection.

[0054] Specifically, at the same time, the second gas 18 is introduced into the second gas passage 5, and the second gas 18 enters the inner layer 401. Under the action of the second gas 18, the reacted ice microballs are sent into the detection instrument inlet 601 by the second gas 18, and then enter the detection instrument 6 for detection.

[0055] During the detection process, the time for the micro-droplet spray 19 to pass through the second circulation tube 4 can be controlled by adjusting the flow rate of the second gas 18, thereby controlling the reaction time. This can capture the dynamic changes in the reaction process, realize online real-time detection and dynamic detection of the reaction, and conduct in-depth research on the reaction process and reaction mechanism.

[0056] Second gas 18 can be nitrogen or other types of gases, such as argon. First gas 16 and second gas 18 can be the same type of gas or different types of gases. By adjusting the type of second gas 18, the gas phase composition during the reaction process can be flexibly changed to simulate different gas phase environments. Detection instrument 6 can be a mass spectrometer, a chromatograph, a spectrometer, or other types of detectors, and adaptive adjustments are made during actual operation based on actual conditions.

[0057] In summary, the present invention provides a micro-droplet ice-air interface formation and detection device and method thereof. Compared with the prior art, (1) the present invention combines the formation, reaction, and detection of the micro-droplet ice-air interface, realizing online reaction, real-time detection, and in-situ analysis of the micro-droplet ice-air interface, which is simple to operate and improves the accuracy of the analysis results. In addition, during the detection process, the time for the micro-droplet spray to pass through the second circulation tube can be controlled by adjusting the flow rate of the second gas, thereby controlling the reaction time, capturing the dynamic changes in the reaction process, realizing online real-time detection and dynamic detection of the reaction, and deeply studying the reaction process and reaction mechanism. (2) The present invention realizes the regulation of the cooling temperature in the second circulation tube by setting a heating material, a heater, a temperature sensor, and a PID controller for use in combination, so that the micro-droplets can be smoothly frozen to form an ice-air interface, thereby allowing the reaction on the ice-air interface to proceed smoothly, and improving the sensitivity and response speed of the reaction. The present invention can be widely used in the field of ice-air interface reaction technology.

[0058] The above-described embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. These modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the present application, and should all be included in the scope of protection of the present application.

Claims

1. A micro-droplet ice-air interface formation and detection device, characterized in that: The invention comprises an injection tube (1), wherein the end of the injection tube (1) is connected to a first flow tube (2), and the first flow tube (2) is provided with a first gas passage (3) arranged perpendicularly thereto; a second flow tube (4) is provided at the end of the first flow tube (2), and the second flow tube (4) is a double-layered arrangement, comprising an inner layer (401) and an outer layer (402), wherein the inner layer (401) is connected to the first flow tube (2), and a cooling medium circulates in the outer layer (402); a second gas passage (5) is further provided on the second flow tube (4), and the second gas passage (5) is connected to the inner layer (401); and a detection instrument (6) is connected to the end of the inner layer (401).

2. The micro-droplet ice-air interface formation and detection device according to claim 1, characterized in that: The inner wall of the inner layer (401) is coated with a heating material (7), and a wire (8) is connected to the heating material (7). A heater (9) is provided on the outside of the second flow tube (4), and the wire (8) is connected to the heater (9).

3. The micro-droplet ice-air interface formation and detection device according to claim 2, characterized in that: A temperature sensor (10) is provided inside the inner layer (401), and the temperature sensor (10) is electrically connected to the heater (9) via a PID controller (11).

4. The micro-droplet ice-air interface formation and detection device according to claim 1, characterized in that: A cooling medium inlet (12) and a cooling medium outlet (13) are provided on the outer wall of the second circulation tube (4), and both the cooling medium inlet (12) and the cooling medium outlet (13) are in communication with the outer layer (402).

5. The micro-droplet ice-air interface formation and detection device according to claim 4, characterized in that: The temperature inside the inner layer (401) is -210-0°C.

6. The micro-droplet ice-air interface formation and detection device according to claim 1, characterized in that: A filter (14) is provided at the connection between the second gas passage (5) and the inner layer (401), and the filter (14) is a micron-grade filter.

7. The micro-droplet ice-air interface formation and detection device according to claim 1, characterized in that: The sample injection tube (1) is a capillary tube; the detection instrument (6) is provided with a detection instrument inlet (601), and the end of the inner layer (401) is connected to the detection instrument inlet (601).

8. A method for forming and detecting a micro-droplet ice-air interface, characterized in that: Using the micro-droplet ice-air interface formation and detection device according to any one of claims 2 to 7, the method includes the following steps: S1: A sample solution (15) is introduced into a sample inlet tube (1), and a first gas (16) is introduced into a first gas passage (3). Under the high-pressure shearing action of the first gas (16), the sample solution (15) forms a micro-droplet spray (19) and is sent into a second flow tube (4); S2: Simultaneously, a cooling medium (17) is introduced into the outer layer (402). Under the action of the cooling medium (17), the micro-droplet spray (19) is frozen into ice microspheres, an ice-air interface is formed on the surface of the micro-droplet spray (19), and sample molecules in the micro-droplet spray (19) react at the ice-air interface. S3: At the same time, the second gas (18) is introduced into the inner layer (401) through the second gas passage (5). Under the action of the second gas (18), the ice microspheres are sent to the detection instrument (6) for detection.

9. The micro-droplet ice-air interface formation and detection method according to claim 8, characterized in that: In S1, the pressure of the first gas (16) is 0.1-1.0 MPa.

10. The method for forming and detecting a micro-droplet ice-air interface according to claim 8, wherein: In S2, the cooling medium (17) includes liquid nitrogen.

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