General condensation module for mass spectrometer and self-supply system

Abstract

The general condensation module and self-supply system comprises a self-pressurization liquid nitrogen tank and a cold trap, the self-pressurization liquid nitrogen tank is connected with the cold trap, and the cold trap is connected with an ion source cavity through a cold finger. A liquid nitrogen tank butt joint cylinder is installed on the top of the self-pressurization liquid nitrogen tank, connected with a liquid nitrogen input pipe through a liquid nitrogen special solenoid valve and connected with a cold trap through the liquid nitrogen input pipe. According to the application, the problems of serious pollution, insufficient vacuum degree, obvious memory effect, difficulty in maintenance, poor adaptability and the like in the prior art are solved through the cold trap combined by the general condensation module and different detachable cold fingers, the liquid nitrogen self-supply system, the pre-refrigeration, the double-liquid-level alarm, the remote monitoring and the adaptive design of various instruments; and high-efficiency, energy-saving and unattended high-quality condensation trapping is realized.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of mass spectrometry, in particular to a general condensing module and a self-supply system for a mass spectrometer. BACKGROUND

[0002] As a high-precision analytical instrument, mass spectrometers are widely used in environmental monitoring, life science, nuclear industry, material analysis and other fields. The function of the core component of the ion source is to ionize the gas molecules to be tested, and then separate and detect the ions formed. The working environment of the ion source, especially its vacuum degree and cleanliness, directly determines the sensitivity, resolution, accuracy and stability of the instrument. In the process of mass spectrometry, not all the gas samples introduced into the ion source are ionized. The residual gas, especially the sample components with corrosive or high adhesion such as hydrofluoric acid, hydrogen chloride and sulfur dioxide, will accumulate in the ion source cavity, which will cause memory effect and vacuum degree drop if not removed in time. The traditional trap structure has the problems of fixed structure, inconvenient maintenance and poor adaptability, which cannot meet the needs of high throughput, high precision and long time continuous analysis. The ion source area is generally equipped with a condensing trap device (commonly known as "cold trap"), which uses a low-temperature surface (usually liquid nitrogen, -196℃) to condense and trap these condensable gases.

[0003] The existing condensing trap device adopts a single cold trap or a double cold trap structure, and the main forms include:

[0004] (1) Whether single or double cold trap, it lacks automatic supply function and relies on manual external liquid nitrogen filling;

[0005] (2) The cold finger and the trap body are an integral part and cannot be disassembled or replaced;

[0006] (3) No pre-cooling function, when filling liquid nitrogen for the first time, the liquid nitrogen evaporates quickly and splashes everywhere; no liquid level monitoring, relying on manual operation.

[0007] Technical defects and reasons:

[0008] (1) The cold trap structure is fixed, different instruments cannot be used due to inconsistent interfaces, the cold finger cannot be replaced, it cannot be adapted to different ion source structures, and maintenance is difficult;

[0009] (2) Liquid nitrogen supply relies on manual operation and cannot realize long-term unattended operation;

[0010] (3) Lack of intelligent monitoring and pre-cooling control function, high operation and maintenance cost.

[0011] In summary, the existing technical solutions have significant limitations and cannot meet the growing needs of high throughput, high precision and long period unattended analysis. SUMMARY

[0012] The purpose of this invention is to provide a universal condensation module and self-replenishment system for mass spectrometers. By combining the universal condensation module with cold traps, liquid nitrogen self-replenishment systems, pre-cooling, dual liquid level alarms, remote monitoring, and various instrument compatibility designs with different detachable cold fingers, this invention solves the problems of serious pollution, insufficient vacuum, significant memory effect, difficult maintenance, and poor compatibility in existing technologies, and achieves high-efficiency, energy-saving, unattended, and high-quality condensation collection.

[0013] The technical solution of the present invention is as follows: a universal condensation module and self-replenishment system for a mass spectrometer, comprising a self-pressurized liquid nitrogen tank and a cold trap, wherein the self-pressurized liquid nitrogen tank is connected to the cold trap, and the cold trap is connected to the ion source cavity via a cold finger.

[0014] A liquid nitrogen tank docking sleeve is installed on the top of the self-pressurized liquid nitrogen tank. The liquid nitrogen tank docking sleeve is connected to the liquid nitrogen input pipe through a dedicated liquid nitrogen solenoid valve, and then connected to the cold trap through the liquid nitrogen input pipe.

[0015] It also includes a second self-pressurized liquid nitrogen tank and a second cold trap; these are symmetrically installed on both sides of the ion source cavity, and the second self-pressurized liquid nitrogen tank and the second cold trap have the same structure as the self-pressurized liquid nitrogen tank and the cold trap.

[0016] The cold trap and the second cold trap are connected by a double cold trap connecting bellows.

[0017] The cold trap consists of an outer layer and an inner layer, with a gap between them. A thermoelectric cooler is located in the gap between the top of the inner layer and the outer layer, with a lower heat-conducting plate below and an upper heat-conducting plate above it. A liquid nitrogen injection port is located at the top of the cold trap, connected to a liquid nitrogen input pipe, allowing liquid nitrogen to enter the inner layer. PT100-A and PT100-B temperature sensors are installed inside the inner layer. The bottom of the outer layer has a cold finger outer layer interface, connected to a bent cold finger outer cylinder via a KF40 clamp. The bottom of the inner layer has a cold finger interface, connected to a detachable cold finger c, which is located inside the bent cold finger outer cylinder, with its other end extending into the ion source cavity.

[0018] The dual cold trap interface is located on the outer side of the cold trap and connects the gap between the outer and inner layers of the cold trap. The dual cold trap connecting bellows is installed on the dual cold trap interface, thereby connecting the two cold traps.

[0019] The upper ends of the PT100-A and PT100-B temperature sensors are installed on the top of the outer layer of the cold trap via PT100-A and PT100-B mounting connectors, respectively. The PT100-A temperature sensor is responsible for low-level monitoring, and the PT100-B temperature sensor is responsible for high-level monitoring, so that the liquid level in the cold trap is maintained above the PT100-A temperature sensor but below the PT100-B temperature sensor.

[0020] The cold finger interface connects to a detachable cold finger a, which is vertically mounted on the ion source cavity and extends into the ion source cavity, thereby positioning the cold trap at the top of the ion source cavity.

[0021] The cold finger interface connects to the detachable cold finger b.

[0022] It also includes an industrial controller that receives signals from the PT100-A and PT100-B temperature sensors and controls the opening and closing of the liquid nitrogen-specific solenoid valve, thereby controlling the amount of liquid nitrogen entering the cold trap from the self-pressurized liquid nitrogen tank.

[0023] The significant advantages of this invention are:

[0024] (1) Liquid nitrogen self-replenishment + pre-cooling energy saving: liquid nitrogen is not splashed during initial filling, daily liquid nitrogen consumption is reduced by 8%, and the working time of a single replenishment is extended to 10 hours.

[0025] (2) The cold finger can be quickly replaced, is compatible with a variety of ion sources, and reduces maintenance costs by more than 50%;

[0026] (3) Intelligent control and monitoring, truly achieving unmanned operation;

[0027] (4) Modular design, compatible with mainstream mass spectrometer models, and has high promotional value. Attached Figure Description

[0028] Figure 1 outer layer of the cold trap;

[0029] Figure 2 Inner layer of the cold trap;

[0030] Figure 3 Cold trap structure diagram;

[0031] Figure 4 Cold trap structure diagram;

[0032] Figure 5 Bend cold refers to the outer cylinder;

[0033] Figure 6 Cold trap block and bent cold finger combination diagram

[0034] Figure 7 Detachable cold finger a;

[0035] Figure 8 Diagram of cold trap and direct cooling combination;

[0036] Figure 9 Detachable cold finger b;

[0037] Figure 10 Removable cold finger c;

[0038] Figure 11Schematic diagram of a single cold trap self-supply system;

[0039] Figure 12 Schematic diagram of the connection between the dual cold traps and the ion source cavity;

[0040] Figure 13 Schematic diagram of the dual cold trap liquid nitrogen self-supply system;

[0041] In the diagram: 1. Outer layer of the cold trap; 2. Inner layer of the cold trap; 3. 1. Cold finger outer layer interface; 2. Cold finger interface; 3. PT100-A temperature sensor; 4. Dual cold trap interface; 5. Semiconductor refrigeration chip; 6. Liquid nitrogen injection port; 7. Liquid nitrogen port gasket; 8. PT100-A mounting connector; 9. Vacuum flange terminal block; 10. KF16 clamp; 11. PT100-B mounting connector; 12. PT100-B temperature sensor; 13. Upper heat conduction plate; 14. Lower heat conduction plate; 15. Bent cold finger outer cylinder; 16. Removable cold finger c; 17. KF40 clamp; 28. Removable cold finger a; 29. ​​Liquid nitrogen input pipe; 20. Liquid nitrogen dedicated solenoid valve; 21. Liquid nitrogen tank docking cylinder; 22. Self-pressurized liquid nitrogen tank; 23. Dual cold trap connecting bellows; 24. Industrial controller; 25. Ion source cavity; 26. Removable cold finger b. Detailed Implementation

[0042] Many specific details are set forth in the following description to provide a full understanding of this application. However, this application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar extensions without departing from the spirit of this application; therefore, this application is not limited to the specific embodiments disclosed below.

[0043] The terminology used in one or more embodiments of this application is for the purpose of describing particular embodiments only and is not intended to limit the scope of one or more embodiments of this application. The singular forms “a,” “the,” and “the” used in one or more embodiments of this application and in the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise. It should also be understood that the term “and / or” used in one or more embodiments of this application refers to and includes any or all possible combinations of one or more associated listed items.

[0044] It should be understood that although the terms first, second, etc., may be used to describe various information in one or more embodiments of this application, such information should not be limited to these terms. These terms are only used to distinguish information of the same type from one another. For example, first may also be referred to as second without departing from the scope of one or more embodiments of this application, and similarly, second may also be referred to as first.

[0045] like Figure 13As shown, a general-purpose condensation module and self-replenishment system for a mass spectrometer includes a self-pressurized liquid nitrogen tank 24 and a cold trap;

[0046] like Figure 11 As shown, a liquid nitrogen tank docking cylinder 23 is installed on the top of the self-pressurized liquid nitrogen tank 24. The liquid nitrogen tank docking cylinder 23 is connected to the liquid nitrogen input pipe 21 through the liquid nitrogen special solenoid valve 22, and is connected to the cold trap through the liquid nitrogen input pipe 21. The cold trap is connected to the ion source cavity 27 through the cold finger, so that the cold finger is in close contact with the ion source inlet and outlet, forming a high-efficiency low-temperature adsorption zone.

[0047] Specifically, it also includes a second self-pressurized liquid nitrogen tank and a second cold trap; these are symmetrically installed on both sides of the ion source cavity 27 with the self-pressurized liquid nitrogen tank 24 and the cold trap, forming a high-efficiency low-temperature adsorption zone;

[0048] Specifically, a second liquid nitrogen tank docking cylinder is installed on the top of the second self-pressurized liquid nitrogen tank. The second liquid nitrogen tank docking cylinder is connected to the second liquid nitrogen input pipe through a second liquid nitrogen dedicated solenoid valve, and is connected to the second cold trap through the second liquid nitrogen input pipe. The second cold trap is connected to the ion source cavity 27 through a cold finger, so that the cold finger is in close contact with the ion source inlet and outlet, forming a high-efficiency low-temperature adsorption zone.

[0049] like Figure 12 As shown, the cold trap and the second cold trap are connected by a double cold trap connecting bellows 25 to balance the pressure;

[0050] like Figure 3 , 4 As shown, the cold trap includes an outer layer 1 and an inner layer 2. There is a gap between the outer layer 1 and the inner layer 2. The dual cold trap interface 6 is located on the side of the outer layer 1 and connects the gap between the outer layer 1 and the inner layer 2. The dual cold trap connecting bellows 25 is installed on the dual cold trap interface 6, thereby connecting the two cold traps.

[0051] The gap between the top of the inner layer 2 of the cold trap and the outer layer 1 of the cold trap contains a semiconductor cooling chip 7. The lower part of the semiconductor cooling chip 7 is a lower heat-conducting plate 16, and the upper part is an upper heat-conducting plate 15.

[0052] The top of the cold trap has a liquid nitrogen injection port 8, which is connected to a liquid nitrogen input pipe 21, so that liquid nitrogen can be introduced into the inner layer 2 of the cold trap.

[0053] PT100-A temperature sensor 5 and PT100-B temperature sensor 14 are installed inside the inner layer 2 of the cold trap. PT100-A temperature sensor 5 is located 30 mm above the bottom of the inner layer 2 of the cold trap and is responsible for low-level monitoring. PT100-B temperature sensor 14 is installed 5 mm below the top of the liquid nitrogen chamber and is responsible for high-level monitoring. Furthermore, the upper ends of PT100-A temperature sensor 5 and PT100-B temperature sensor 14 are respectively installed on the top of the outer layer 1 of the cold trap via PT100-A mounting connector 10 and PT100-B mounting connector 13. Through the precise monitoring of PT100-A temperature sensor 5 and PT100-B 14, the liquid level in the cold trap is ensured to always be kept within a reasonable range, that is, higher than PT100-A temperature sensor 5 but lower than PT100-B temperature sensor 14, thus maintaining the efficient operation of the cold trap, realizing the automated management of liquid nitrogen level, greatly reducing the need for manual intervention, improving the operating efficiency and safety of the system, providing strong support for the stable operation of the mass spectrometer condensation module, and effectively ensuring the continuity and high precision of the mass spectrometry analysis process.

[0054] like Figure 5 , 6 As shown, the bottom of the outer layer 1 of the cold trap has a cold finger outer layer interface 3, which is connected to the curved cold finger outer cylinder 17 via a KF40 clamp 19; the bottom of the inner layer 2 of the cold trap has a cold finger interface 4, which is connected to a detachable cold finger c18, and the detachable cold finger c18 is located inside the curved cold finger outer cylinder 17, with its other end extending into the ion source cavity 27;

[0055] like Figure 7 , 8 As shown, optionally, the cold finger interface 4 is connected to a detachable cold finger a20, which is vertically mounted on the ion source cavity 27 and extends into the ion source cavity 27, thereby making the cold trap located on the upper part of the ion source cavity 27.

[0056] like Figure 9 As shown, optionally, the cold finger interface 4 connects to the detachable cold finger b28.

[0057] It also includes an industrial controller 26, which receives signals from the PT100-A temperature sensor 5 and the PT100-B temperature sensor 14, and controls the opening and closing of the liquid nitrogen-specific solenoid valve 22, thereby controlling the amount of liquid nitrogen entering the cold trap from the self-pressurized liquid nitrogen tank 24.

[0058] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

[0059] It should be noted that, for the sake of simplicity, the foregoing method embodiments are all described as a series of actions. However, those skilled in the art should understand that this application is not limited to the described order of actions, as some steps may be performed in other orders or simultaneously according to this application. Furthermore, those skilled in the art should also understand that the embodiments described in the specification are preferred embodiments, and the actions and modules involved are not necessarily essential to this application.

[0060] In the above embodiments, the descriptions of each embodiment have different focuses. For parts not described in detail in a certain embodiment, please refer to the relevant descriptions of other embodiments.

[0061] The preferred embodiments disclosed above are merely illustrative of this application. The optional embodiments do not exhaustively describe all details, nor do they limit the invention to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this application. These embodiments are selected and specifically described in this application to better explain the principles and practical applications of this application, thereby enabling those skilled in the art to better understand and utilize this application.

Claims

1. A universal condenser module and self-replenishing system for a mass spectrometer, characterized in that: It includes a self-pressurized liquid nitrogen tank (24) and a cold trap. The self-pressurized liquid nitrogen tank (24) is connected to the cold trap, and the cold trap is connected to the ion source cavity (27) through a cold finger.

2. The universal condenser module and self-supply system for a mass spectrometer according to claim 1, characterized in that: A liquid nitrogen tank docking tube (23) is installed on the top of the self-pressurized liquid nitrogen tank (24). The liquid nitrogen tank docking tube (23) is connected to the liquid nitrogen input pipe (21) through the liquid nitrogen special solenoid valve (22), and is connected to the cold trap through the liquid nitrogen input pipe (21).

3. The universal condenser module and self-supply system for a mass spectrometer according to claim 2, characterized in that: It also includes a second self-pressurized liquid nitrogen tank and a second cold trap; these are installed symmetrically on both sides of the ion source cavity (27) along with the self-pressurized liquid nitrogen tank (24) and the cold trap, and the second self-pressurized liquid nitrogen tank and the second cold trap have the same structure as the self-pressurized liquid nitrogen tank (24) and the cold trap.

4. The universal condenser module and self-replenishing system for a mass spectrometer according to claim 3, characterized in that: The cold trap and the second cold trap are connected by a double cold trap connecting bellows (25).

5. A universal condenser module and self-supply system for a mass spectrometer according to claim 4, characterized in that: The cold trap includes an outer layer (1) and an inner layer (2), with a gap between them. A semiconductor cooling chip (7) is placed between the top of the inner layer (2) and the outer layer (1), with a lower heat-conducting plate (16) at the bottom and an upper heat-conducting plate (15) at the top. A liquid nitrogen injection port (8) is located at the top of the cold trap and is connected to a liquid nitrogen input pipe (21), allowing liquid nitrogen to enter the inner layer (2). A device is installed inside the inner layer (2). It is equipped with a PT100-A temperature sensor (5) and a PT100-B temperature sensor (14); the bottom of the outer layer (1) of the cold trap has a cold finger outer layer interface (3), which is connected to the curved cold finger outer cylinder (17) by a KF40 clamp (19); the bottom of the inner layer (2) of the cold trap has a cold finger interface (4), which is connected to a detachable cold finger c (18), and the detachable cold finger c (18) is located inside the curved cold finger outer cylinder (17), with its other end extending into the ion source cavity (27).

6. A universal condenser module and self-supply system for a mass spectrometer according to claim 5, characterized in that: The dual cold trap interface (6) is located on the side of the outer layer (1) of the cold trap and connects the gap between the outer layer (1) and the inner layer (2) of the cold trap. The dual cold trap connecting bellows (25) is installed on the dual cold trap interface (6) to connect the two cold traps.

7. A universal condenser module and self-supply system for a mass spectrometer according to claim 5, characterized in that: The upper ends of the PT100-A temperature sensor (5) and the PT100-B temperature sensor (14) are installed on the top of the outer layer (1) of the cold trap through the PT100-A mounting connector (10) and the PT100-B mounting connector (13), respectively. The PT100-A temperature sensor (5) is responsible for low-level monitoring, and the PT100-B temperature sensor (14) is responsible for high-level monitoring, so that the liquid level of the cold trap is kept above the PT100-A temperature sensor (5) but below the PT100-B temperature sensor (14).

8. A universal condenser module and self-supply system for a mass spectrometer according to claim 5, characterized in that: The cold finger interface (4) is connected to the detachable cold finger a (20), which is vertically installed on the ion source cavity (27) and extends into the ion source cavity (27), so that the cold trap is located on the upper part of the ion source cavity (27).

9. A universal condenser module and self-supply system for a mass spectrometer according to claim 5, characterized in that: The cold finger interface (4) connects to the detachable cold finger b (28).

10. A universal condenser module and self-supply system for a mass spectrometer according to claim 5, characterized in that: It also includes an industrial controller (26), which receives signals from the PT100-A temperature sensor (5) and the PT100-B temperature sensor (14) and controls the opening and closing of the liquid nitrogen-specific solenoid valve (22) to control the amount of liquid nitrogen entering the cold trap from the self-pressurized liquid nitrogen tank (24).

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