Device for detecting glove leakage rate of glove box by using vacuum deoxidization and detection method

By designing a vacuum deoxygenation detection device, using a vacuum pump and a nitrogen source to reduce the oxygen content, combined with a differential pressure gauge and an oxygen analyzer to detect changes in the oxygen content, the problem of the inability to accurately detect the permeability leakage rate of glove boxes in the prior art is solved, and accurate detection and efficient testing of glove leakage rate are achieved.

CN119714720AActive Publication Date: 2025-03-28CHINA INST FOR RADIATION PROTECTION
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Patent Information

Application Number
CN202411633629.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-15
Publication Date
2025-03-28
Estimated Expiration
2044-11-15

AI Technical Summary

Technical Problem

The prior art lacks special detection devices and methods to accurately and quantitatively reflect the permeability leakage rate of glove materials, and cannot effectively measure the leakage rate of glove box gloves.

Method used

A device for detecting the leakage rate of glove boxes using vacuum deoxygenation is designed, including a detection chamber, a deoxygenation system and a data acquisition system. The oxygen content in the space to be detected is reduced by a vacuum pump and a nitrogen source, and the oxygen content changes are detected by a differential pressure gauge and an oxygen analyzer to calculate the leakage rate of the gloves.

Benefits of technology

It realizes accurate detection of the leakage rate of glove boxes and can be suitable for gloves of different materials and sizes, providing a rigorous leakage rate testing solution, reducing the interference of internal volume changes on the test results and improving detection accuracy.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a device and method for detecting the glove leakage rate of a glove box through vacuum deoxygenation, and the device comprises a detection cabin which is provided with a cavity and a glove installation part, the outer surface of the cavity is provided with a connection hole assembly, and the connection hole assembly comprises a plurality of connection holes; the glove mounting piece is positioned at one end of the cavity and is fixedly connected with the cavity; the glove mounting piece is provided with a hollow circular opening protruding part, and the glove to be detected, the protruding part and the cavity jointly form a space to be detected; the deoxidizing system comprises a vacuum pump and a nitrogen source, and the vacuum pump and the nitrogen source are both arranged outside the cavity and connected with the outer surface of the cavity through connecting hole assemblies; the vacuum pump and the nitrogen source work cooperatively, the oxygen content of the to-be-detected space is reduced by means of vacuumizing and nitrogen injection, and a low-oxygen environment is provided. According to the method, the oxygen concentration is rapidly reduced to the ppm level by adopting a physical method, a complex oxygen adsorption circulating system is not needed, high vacuum degree is not needed, the equipment cost is reduced, and the operation process is simplified.
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Description

Technical Field

[0001] The present invention relates to the technical field of individual radiation protection equipment detection, and in particular to a device and a detection method for detecting the leakage rate of gloves in a glove box by utilizing vacuum deoxygenation. Background Art

[0002] During the experiment and production process, the operation in the closed glove box places high demands on the sealing of gloves. Gloves are an important part of the glove box, forming a sealed box environment, protecting the safety of operators and maintaining a specific atmosphere in the box. Toxic, harmful or radioactive substances may exist in the glove box, and gloves must have good barrier properties to prevent external harmful substances from penetrating the gloves into the external environment and endangering the safety of workers. In addition, some experiments are carried out in an inert gas or low-oxygen environment, which also requires gloves to block the penetration of external air to prevent oxygen from entering the glove box and affecting the experimental atmosphere.

[0003] There are two main mechanisms for air or other substances to leak through glove materials: penetration and permeation. Penetration refers to the phenomenon that substances pass through the material due to damage or holes in the glove material, which is easier to detect. This type of gloves has been considered unqualified and cannot meet the requirements for safe use. Permeation refers to the process of substances passing through the glove material itself, which involves the steps of molecular adsorption, diffusion and desorption. The quantitative analysis of permeation leakage is relatively complicated. In order to measure the permeability of glove materials, the rate at which air penetrates the glove material is usually characterized by the leakage rate.

[0004] There is no specific testing standard for the permeability leakage rate of gloves in the prior art, and there is also a lack of specific testing devices that can accurately and quantitatively reflect the permeability of glove materials. Therefore, there is an urgent need for a specific device and method to test the leakage rate of gloves themselves.

[0005] In view of the above problems, the present invention is proposed. Summary of the invention

[0006] The invention discloses a device and a detection method for detecting the leakage rate of gloves in a glove box by utilizing vacuum deoxygenation, aiming to solve the technical problems existing in the prior art.

[0007] According to one aspect of the present invention, there is provided a device for detecting the leakage rate of gloves in a glove box by using vacuum deoxygenation, comprising:

[0008] The detection cabin is provided with a cavity and a glove mounting piece, the outer surface of the cavity is provided with a connection hole assembly, and the connection hole assembly includes a plurality of connection holes; the glove mounting piece is located at one end of the cavity and is fastened thereto; the glove mounting piece is provided with a protruding portion with a hollow circular opening, the outer peripheral surface of the protruding portion is provided with at least one annular groove, a sealing ring is provided on the outer side of the annular groove, and a sealing ring clamp fixes the glove to be detected on the annular groove, and the glove to be detected, the protruding portion and the cavity together form a space to be detected;

[0009] The deoxygenation system includes a vacuum pump and a nitrogen source. The vacuum pump and the nitrogen source are both arranged outside the cavity and connected to the outer surface of the cavity through a connecting hole assembly. The vacuum pump and the nitrogen source work together to reduce the oxygen content in the space to be detected by vacuuming and injecting nitrogen, thereby providing a low-oxygen environment.

[0010] The data acquisition system includes a differential pressure gauge and an oxygen analyzer. Both the differential pressure gauge and the oxygen analyzer are arranged outside the cavity and are connected to the outer surface of the cavity through a connecting hole assembly respectively. The differential pressure gauge and the oxygen analyzer are used to detect the pressure difference and oxygen content of the space to be detected and output corresponding detection data.

[0011] As a preferred technical solution, a circular blocking member is provided at the connection between the protrusion and the cavity, an internal thread is provided on the inner side of the protrusion, and an external thread is provided on the outer periphery of the blocking member, and the internal and external threads cooperate to make the blocking member tightly connected to the inner side of the protrusion to block the connection between the protrusion and the cavity; the blocking member divides the space to be detected into a first space to be detected and a second space to be detected, and the first space to be detected is formed between the glove to be detected, the protrusion and the blocking member, and the second space to be detected is formed between the blocking member and the cavity.

[0012] As a preferred technical solution, the protrusion is arranged as a step structure, including a first step and a second step, the second step is arranged close to the cavity, and an internal thread is arranged on the inner side of the second step.

[0013] As a preferred technical solution, the first step is arranged away from the cavity, and the outer peripheral surface of the first step is provided with at least one annular groove.

[0014] As a preferred technical solution, the number of annular grooves is ≥3.

[0015] As a preferred technical solution, the diameters of the multiple annular grooves are different to adapt to the cuff sizes of different gloves to be tested.

[0016] As a preferred technical solution, a first connecting hole is provided on the outer peripheral surface of the first step, and the vacuum pump is connected to the first space to be detected through the first connecting hole.

[0017] As a preferred technical solution, the glove mounting piece is further provided with a flange portion connected to the protruding portion, and the flange portion is a circular flange structure, which is in direct contact with the end face of the cavity and is used for a fast connection with the cavity.

[0018] As a preferred technical solution, the detection chamber is also provided with a sealing cover, which is tightly connected to the other end of the cavity and is used to seal the cavity.

[0019] As a preferred technical solution, the data acquisition system also includes a thermometer, which is connected to the cavity through a connecting hole assembly and is used to detect the gas temperature inside the cavity.

[0020] According to another aspect of the present invention, a detection method for leak rate detection using the above device is also provided, comprising:

[0021] The glove mounting member, the blocking member and the sealing cover are sealed and connected to the cavity to form a first space to be detected and a second space to be detected; the vacuum pump, the nitrogen source, the differential pressure gauge and the oxygen analyzer are connected to the cavity through the connecting hole assembly;

[0022] The standard glove is mounted on the glove mounting part, and the internal oxygen content of the first to-be-detected space and the second to-be-detected space is reduced by controlling the vacuum pump and the nitrogen source, and a first oxygen concentration change value is detected by using a differential pressure gauge and an oxygen analyzer; based on the first oxygen concentration change value, a first leakage rate representing the background leakage of the cavity is estimated, and a corrected third leakage rate is estimated based on the first leakage rate;

[0023] The blocking member is removed, and the oxygen content inside the cavity is reduced by controlling the vacuum pump and the nitrogen source. The second oxygen concentration change value is detected and calculated by means of a differential pressure gauge and an oxygen analyzer. After installing the blocking member and replacing the standard glove with the glove to be tested, the blocking member is removed again, and the oxygen content inside the cavity is reduced by controlling the vacuum pump and the nitrogen source. The third oxygen concentration change value is detected and calculated by means of a differential pressure gauge and an oxygen analyzer. Based on the third leakage rate, the second oxygen concentration change value and the third oxygen concentration change value, the hourly leakage rate of the glove to be tested is calculated according to the following formula:

[0024]

[0025] Where:

[0026] OD2——The third oxygen concentration change value of the gloves to be tested, expressed in parts per million (ppm) by volume;

[0027] OD1 - the second oxygen concentration change using standard gloves, expressed in parts per million (ppm) by volume;

[0028] t——test duration, min;

[0029] T0——Corrected leakage rate taking into account the cavity (third leakage rate).

[0030] As a preferred technical solution, a vacuum pump and a nitrogen source reduce the oxygen content inside the chamber, including:

[0031] Two connecting pipelines are respectively provided between the vacuum pump and the cavity, and between the vacuum pump and the protruding portion, and a first switch valve and a second switch valve are respectively provided on the two connecting pipelines. The first switch valve is opened and the second switch valve is kept closed to extract the internal air of the first space to be detected;

[0032] Close the first switch valve, open the second switch valve, and extract the internal air of the second to-be-detected space;

[0033] A third switch valve is provided on the connection pipeline between the nitrogen source and the cavity, the second switch valve is closed and the third switch valve is opened to inject high-purity nitrogen into the cavity;

[0034] Repeat the above process and use an oxygen analyzer to observe the oxygen concentration value inside the cavity until it drops to the required oxygen content detection condition.

[0035] The technical solution adopted by the present invention can achieve at least one of the following beneficial effects:

[0036] 1. The present invention proposes an innovative method for detecting the leakage rate of gloves, that is, a device and method for detecting leakage using an oxygen-containing method is proposed to solve the leakage problem of gloves in a glove box. By providing a glove mounting member for fixing the gloves to be detected, a detection cabin connected to the glove mounting member, a cavity thereof, and a vacuum pump, a nitrogen source, a differential pressure gauge, and an oxygen analyzer connected to the cavity, based on specific detection steps, the air permeability of the gloves can be accurately detected, and the method is particularly suitable for gloves of various materials and calibers.

[0037] 2. The present invention proposes a rigorous leakage rate test scheme, which not only takes into account the background leakage rate of the device, but also considers the change in gas volume inside the sealing structure after the gloves are installed. By comparing with the relative test method of standard gloves, the interference of internal volume change on the test results is avoided, and the accuracy of the leakage rate of the gloves to be tested is further improved through the leakage rate correction value.

[0038] 3. The device of the present invention has a simple structure, a small size, a low background leakage rate, is easy to operate, can reflect the permeability characteristics of the glove material to the greatest extent, and is suitable for convenient use in multiple occasions.

[0039] 4. The present invention provides a physical method based on controlling the change of cavity air pressure, which can quickly reduce the oxygen concentration in the cabin. Through a simple cycle of vacuum extraction and nitrogen injection, the oxygen concentration can be reduced to ppm level in a short time. It is fast and does not require the use of an oxygen adsorption circulation system, reducing maintenance costs.

[0040] 5. The present invention can achieve effective oxygen concentration control using a conventional vacuum pump without the need to achieve a high vacuum degree, so the equipment investment and operating costs are low. The device is easy to operate, does not require chemical reagent consumption and regeneration, and daily maintenance is economical and convenient. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments, which constitute a part of the present invention. The exemplary embodiments of the present invention and their descriptions explain the present invention and do not constitute improper limitations on the present invention. In the drawings:

[0042] Figure 1 A schematic diagram of the working principle of a device for detecting the leakage rate of gloves in a glove box by using vacuum deoxygenation according to the present invention;

[0043] Figure 2 It is a schematic diagram of the three-dimensional structure of the detection cabin of the present invention;

[0044] Figure 3 It is a schematic diagram of the three-dimensional structure of the sealing cover of the present invention installed in the detection cabin;

[0045] Figure 4 It is a schematic structural diagram of the standard glove or the glove to be tested of the present invention being installed on the glove mounting piece;

[0046] Figure 5 It is a schematic diagram of the standard glove or the glove to be tested of the present invention in a testing state;

[0047] Figure 6 The present invention is a schematic diagram of a detection process of a device for detecting the leakage rate of gloves in a glove box by utilizing vacuum deoxygenation.

[0048] Description of reference numerals:

[0049] 1. Detection cabin; 11. Cavity; 12. Glove mounting piece; 121. Flange; 122. Protrusion; 123. First connecting hole; 13. Connecting hole assembly; 131. Second connecting hole; 132. Third connecting hole; 133. Fourth connecting hole; 134. Fifth connecting hole; 135. Sixth connecting hole; 136. Seventh connecting hole; 14. Blocking piece; 15. Sealing cover; 16. Support base; 2. Vacuum pump; 21. First switch valve; 22. Second switch valve; 3. Nitrogen source; 31. Third switch valve; 4. Thermometer; 5. Differential pressure gauge; 6. Oxygen analyzer. DETAILED DESCRIPTION

[0050] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the specific embodiments of the present invention and the corresponding drawings. In the description of the present invention, it should be noted that the term "or" is usually used in the sense of including "and / or", unless the content clearly indicates otherwise.

[0051] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected" and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or a magnetic connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be internal communication between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. In addition, in the description of this application, the terms "first", "second", etc. are only used to distinguish the description and cannot be understood as indicating or implying relative importance.

[0052] Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0053] In order to solve the problems existing in the prior art, an embodiment of the present invention provides a device for detecting the leakage rate of gloves in a glove box by using vacuum deoxygenation, such as Figure 1-Figure 6 As shown, the detection chamber 1 includes a vacuum pump 2, a nitrogen source 3, a thermometer 4, a differential pressure gauge 5 and an oxygen analyzer 6 respectively connected to the detection chamber 1. The detection chamber 1 includes a cavity 11, and the outer surface of the cavity 11 is provided with a connection hole assembly 13, including 6 connection holes, for connecting external equipment to the inside of the cavity 11. Figure 2As shown, the six connection holes are the second connection hole 131, the third connection hole 132, the fourth connection hole 133, the fifth connection hole 134, the sixth connection hole 135 and the seventh connection hole 136. The vacuum pump 2 and the nitrogen source 3 together form the deoxygenation system of the device. The vacuum pump 2 is connected to the cavity 11 through the third connection hole 132, and is used to achieve an efficient deoxygenation process by adjusting the air pressure inside the detection chamber 1, that is, to extract the air inside the cavity 11 and reduce the oxygen content in the cavity 11, thereby forming a low oxygen environment, so as to accurately detect the leakage rate of the glove box gloves. A second switch valve 22 is provided on the connecting pipeline between the vacuum pump 2 and the third connection hole 132, which is used to control the on-off of its pipeline. The nitrogen source 3 is connected to the cavity 11 through the fourth connection hole 133, and is used to provide a low oxygen environment inside the cavity 11, and assist the vacuum pump 2 to achieve a more stable and accurate deoxygenation effect, that is, after the vacuum pump 2 is evacuated, the nitrogen source 3 replaces the residual oxygen by injecting nitrogen into the cavity 11 to further reduce the oxygen concentration. A third switch valve 31 is provided on the connecting pipeline between the nitrogen source 3 and the fourth connection hole 133, which is used to control the on-off of the above pipeline. The thermometer 4 is connected to the cavity 11 through the fifth connection hole 134, and is used to monitor the temperature inside the cavity 11 in real time to ensure that the glove box glove leakage rate detection process is carried out under stable and appropriate temperature conditions. The differential pressure gauge 5 is connected to the cavity 11 through the sixth connection hole 135, and is used to monitor the relative pressure difference of the gas inside the cavity 11 in real time. The oxygen analyzer 6 is connected to the cavity 11 through the seventh connection hole 136, and can detect the trace oxygen level inside the cavity 11 in real time and accurately, providing core data support for leakage rate detection. The thermometer 4, the differential pressure gauge 5 and the oxygen analyzer 6 together form the data acquisition system of the device.

[0054] like Figure 2-Figure 5 As shown, the detection chamber 1 also includes a glove mounting member 12, a blocking member 14 and a sealing cover 15. Figure 2As shown, the glove mounting member 12 includes a flange portion 121, a protrusion 122 and a first connecting hole 123. The flange 121 is a circular flange structure, and a plurality of mounting holes are evenly distributed on the flange for bolts or screws to pass through and fixedly connected to one end of the cavity 11. The protrusion 122 is used to fix the gloves to be tested, and is set to a hollow circular opening structure, and a plurality of annular grooves are arranged on the outside thereof for mounting the gloves to be tested. Furthermore, the number of annular grooves is set to at least three, and the diameters of the three annular grooves are set to three different interface sizes, such as 160mm, 180mm, and 200mm. Other diameter sizes can also be set as needed. An O-ring is arranged at the above-mentioned annular groove. When the gloves to be tested are installed, the cuffs are placed at the above-mentioned annular groove position and fixed by the O-ring. At the same time, the O-ring can minimize the oxygen leakage at the glove mounting member 12 to achieve a good sealing effect. The outer peripheral surface of the protrusion 122 is also provided with a first connection hole 123, which is used to provide a communication channel between the external device and the inner space of the protrusion 122. The vacuum pump 2 is connected to the inner space of the protrusion 122 through the first connection hole 123, and a first switch valve 21 is provided on the connecting pipeline between the vacuum pump 2 and the second connection hole 131, which is used to control the on-off of the above-mentioned connecting pipeline. The inside of the protrusion 122 is set as a step structure, the inside of the protrusion 122 corresponding to the above-mentioned annular groove is a first step, the first connection hole 123 is set on the outer peripheral surface of the first step, the inside of the protrusion 122 between the above-mentioned annular groove and the flange part 121 is a second step, the diameter of the first step is smaller than the diameter of the second step, and the inner side of the second step is provided with an internal thread.

[0055] like Figure 2 As shown, the detection cabin 1 is also provided with a blocking member 14, which is located at the connection between the protrusion 122 and the cavity 11. The blocking member 14 is arranged in a circular shape, and its outer periphery contacts the inner side of the second step of the protrusion 122. The outer periphery of the blocking member 14 is provided with an external thread, which matches the internal thread inside the second step. The blocking member 14 is also provided with a handle, through which the blocking member 14 can be screwed to connect with the inner side of the protrusion 122, so as to block the hollow circular opening structure of the glove mounting member 12. When the glove is installed, the blocking member 14 blocks the connection between the glove and the cavity 11, playing a role of blocking and sealing; when the blocking member 14 is screwed by the handle, the space formed by the installed glove and the protrusion 122 is connected with the cavity 11 when it is removed.

[0056] like Figure 4As shown, the detection chamber 1 is also provided with a sealing cover 15 at the other end of the cavity 11. The sealing cover 15 is fixedly connected to the other end of the cavity 11 and is used to seal the cavity 11 to ensure the airtightness of the internal environment of the cavity 11, so as to maintain specific conditions such as low oxygen and low pressure during the glove leakage rate detection process to avoid interference from external factors. Preferably, the sealing cover 15 adopts a precise sealing structure and is tightly matched with the cavity 11 through bolts or other fastening devices to ensure the sealing effect. Further preferably, the sealing cover 15 is configured to be easy to disassemble or replace, facilitate maintenance and servicing, and extend the service life of the detection device.

[0057] The above structural design creates a low oxygen environment and detects relevant data in real time to accurately detect the leakage rate of the glove box gloves.

[0058] The detection chamber 1 is connected to the vacuum pump 2 and the nitrogen source 3, and cooperates to quickly reduce the oxygen concentration by vacuuming. The vacuum pump 2 reduces the oxygen content in the cavity 11 by pumping air, and the nitrogen source 3 injects nitrogen into the cavity 11 after the vacuum pump 2 works to further replace the oxygen and maintain a low oxygen environment. The low oxygen environment control is based on the Clapeyron equation (PV=nRT). At a constant temperature, the pressure (P) is reduced by reducing the amount of substance (n) in the gas in the chamber, thereby achieving rapid deoxygenation.

[0059] During operation, after the blocking member 14 is installed, the volume inside the cavity 11 is fixed. According to the Clapeyron equation:

[0060] PV=nRT

[0061] Where P is the pressure in the cavity 11, V is the volume in the cavity 11, n is the amount of air in the cavity 11, and R is the molar gas constant. Ignoring temperature fluctuations and volume changes at room temperature, V, R, and T are all constants, and P∝n.

[0062] In terms of data monitoring, the gloves to be tested are first connected to the cavity 11 through the glove mounting member 12. The design of the blocking member 14 and the sealing cover 15 enhances the airtightness of the cavity 11 to avoid interference of the external environment on the test results. The cavity 11 is connected to the thermometer 4, the differential pressure gauge 5 and the oxygen analyzer 6. During the glove leakage rate detection process, relevant data are detected and collected to provide accurate data support for the detection of the glove leakage rate.

[0063] When detecting the leakage rate of the gloves in the glove box, in order to ensure the consistency of the detection conditions, especially to ensure the consistency of the internal volume formed by the gloves to be detected and the cavity 11 during the detection, first, the blocking member 14 is fixed between the glove mounting member 12 and the cavity 11, and the first oxygen concentration change value after the standard gloves are installed is detected by using the standard gloves and the above-mentioned detection device structure, so as to calculate the first leakage rate as the background leakage rate, and the background leakage rate is used to estimate the corrected leakage rate, that is, the third leakage rate; secondly, the blocking member 14 is removed, and the second oxygen concentration change value of the standard gloves is detected; thirdly, after the standard gloves are removed and the gloves to be detected are installed, the third oxygen concentration change value before and after the blocking member 14 is removed is detected again with the help of the above-mentioned detection device, and the required leakage rate result of the gloves to be detected is calculated according to the formula through the second oxygen concentration change value, the third oxygen concentration change value, the first leakage rate (that is, the background leakage rate) and the corrected leakage rate (the third leakage rate).

[0064] In some preferred embodiments, the above-mentioned standard gloves are made of high barrier materials such as butyl rubber.

[0065] In some preferred embodiments, in order to further control the size of the detection space, reduce the gas volume of the environment in which the gloves are detected, reduce the potential oxygen leakage of the detection device's own materials, and improve the detection accuracy, the cavity 11 is set to a cylindrical barrel. Preferably, in order to meet the detection requirements of various glove box gloves, the diameter of the cavity 11 is designed to be 200mm-300mm, which is larger than the cuff size of various existing glove box gloves; the axial length of the cavity 11 is designed to be 850mm-950mm, which is larger than the length of various existing glove box gloves.

[0066] In some preferred embodiments, the thermometer 4 adopts a thermocouple structure to measure the temperature of the gas inside the cavity 11 during the detection process.

[0067] In some preferred embodiments, the differential pressure meter 5 uses a micro differential pressure sensor to measure the relative pressure difference of the gas inside the cavity 11 during the detection process.

[0068] In some preferred embodiments, the sealing cover 15 is connected to the cavity 11 via a sealing clamp.

[0069] In some preferred embodiments, the detection chamber 1 further includes a plurality of support bases 16, which are used to provide a solid foundation for the entire device, ensure that the device remains balanced during operation, and avoid tilting or displacement caused by external forces or internal pressure changes. Preferably, the number of support bases 16 is 2-4.

[0070] The present invention also provides a detection method for detecting the leakage rate of gloves in a glove box, comprising the following steps:

[0071] S1: The glove mounting member 12, the blocking member 14 and the sealing cover 15 are sealed and connected to the cavity 11, a first space to be tested is formed between the glove, the glove mounting member 12 and the blocking member 14, and a second space to be tested is formed between the blocking member 14, the cavity 11 and the sealing cover 15; the vacuum pump 2, the nitrogen source 3, the thermometer 4, the differential pressure gauge 5 and the oxygen analyzer 6 are connected to the cavity 11 through the third connecting hole 132, the fourth connecting hole 133, the fifth connecting hole 134, the sixth connecting hole 135 and the seventh connecting hole 136 respectively.

[0072] S2: Detect the first oxygen concentration and the second oxygen concentration value through the above structure, obtain the first oxygen concentration change value through calculation, and estimate the background leakage rate (first leakage rate) and the corrected leakage rate (third leakage rate) based on the above first oxygen concentration change value.

[0073] S21: Install the standard glove so that the rolled edge of the standard glove is placed in the annular groove closest to the flange 121, and use O-rings to fix the other two annular grooves so that the standard glove and the glove mounting member 12 are sealed.

[0074] S22 : opening the first switch valve 21 , and the vacuum pump 2 extracts air in the first test space formed by the standard glove, the glove mounting member 12 , and the blocking member 14 through the first connecting hole 123 .

[0075] S23: Close the first switch valve 21, open the second switch valve 22, and the vacuum pump 2 extracts the air inside the cavity 11, that is, the air in the second test space, through the third connecting hole 132; use the differential pressure gauge 5 to monitor the gas pressure inside the cavity 11, and when the gas pressure inside the cavity 11 drops to ≤-90kPa~-99kPa, close the second switch valve 22.

[0076] S24: the third switch valve 31 is opened, and the nitrogen source 3 injects high-purity nitrogen into the cavity 11 through the fourth connecting hole 133. When the pressure in the cavity 11 returns to normal pressure, the third switch valve 31 is closed.

[0077] S25: Repeat S22 to S24 2 to 4 times, and use the oxygen analyzer 6 to observe the oxygen concentration value inside the cavity 11. When the oxygen concentration value drops to ≤50ppm, use the vacuum pump 2 and the differential pressure gauge 5 to adjust the relative pressure inside the cavity 11 to the detection condition, that is, (-1100 to -900) Pa; preferably, the oxygen concentration value is reduced to ≤10ppm.

[0078] S26: After the above detection conditions are stable, the oxygen analyzer 6 is used to record the first oxygen concentration, and the timer (not shown in the figure) is used to count. After a certain period of time, the oxygen analyzer 6 is used to record the second oxygen concentration, and the first oxygen concentration change value is obtained by the first oxygen concentration and the second oxygen concentration value, and the background leakage rate (first leakage rate) of the cavity 11 is calculated based on the first oxygen concentration change value. Preferably, the certain period of time is 30 minutes to 60 minutes.

[0079] S27: using the background leakage rate (first leakage rate) mentioned above, combined with the volume of the cavity 11 itself and the volume of the standard glove after expansion, the corrected leakage rate (third leakage rate) is estimated.

[0080] S3: Through the above structure detection and calculation, the second oxygen concentration change value of the standard glove and the third oxygen concentration change value of the glove to be tested are obtained, and the leakage rate of the glove to be tested is calculated based on the above second oxygen concentration change value, the third oxygen concentration change value and the above corrected leakage rate (third leakage rate).

[0081] S31: Figure 5 As shown, the blocking member 14 is unscrewed and pushed into the cavity 11 through the standard glove, so that the first space to be tested is connected with the second space to be tested, and the relative pressure inside the cavity 11 is adjusted to the test condition, i.e. (-1100~-900) Pa, by using the vacuum pump 2 and the differential pressure gauge 5. Due to the negative pressure, the standard glove will automatically expand inside the cavity 11. Figure 6 shown.

[0082] S32: After the above detection conditions are stable, the third oxygen concentration is recorded by the oxygen analyzer 6, and the timer (not shown in the figure) is used to count. After a certain period of time, the fourth oxygen concentration is recorded by the oxygen analyzer 6, and the difference between the third oxygen concentration and the fourth oxygen concentration is used as the second oxygen concentration change value under the standard gloves. Preferably, the certain period of time is 30 minutes to 60 minutes.

[0083] S33: Through the standard gloves, the blocking member 14 is screwed and connected to the inner side of the protruding portion 122 of the glove mounting member 12, thereby blocking the hollow circular opening structure of the glove mounting member 12 and playing a sealing role. At this time, the standard gloves are removed and the gloves to be tested are installed.

[0084] S34: Repeat S22 to S24 for 1 to 2 times for the gloves to be tested, and use the oxygen analyzer 6 to observe the oxygen concentration value inside the cavity 11. When the oxygen concentration value drops to ≤50ppm, Figure 5 As shown, the blocking member 14 is pushed into the cavity 11, and the relative pressure inside the cavity 11 is adjusted to the detection condition, i.e. (-1100 to -900) Pa, by using the vacuum pump 2 and the differential pressure gauge 5; preferably, the oxygen concentration value is reduced to ≤10ppm. Figure 6As shown, due to the negative pressure, the glove to be tested will automatically expand inside the cavity 11.

[0085] S35: After the above detection conditions are stable, the fifth oxygen concentration is recorded by the oxygen analyzer 6, and the timer (not shown in the figure) is used to count. After a certain period of time, the sixth oxygen concentration is recorded by the oxygen analyzer 6, and the difference between the fifth oxygen concentration and the sixth oxygen concentration is used as the third oxygen concentration change value under the standard gloves. Preferably, the certain period of time is 30 minutes to 60 minutes.

[0086] S36: Calculate the hourly leakage rate of the gloves to be tested using the following formula:

[0087]

[0088] Where:

[0089] ΔO2——the change in the third oxygen concentration of the glove to be tested, expressed in parts per million (ppm) by volume;

[0090] ΔO1 – the change in oxygen concentration using standard gloves, expressed in parts per million (ppm) by volume;

[0091] t——test duration, min;

[0092] T0——Consider the corrected leakage rate of the device (third leakage rate).

[0093] The embodiments of the present invention are described above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned specific implementation modes, which are merely illustrative rather than restrictive. Under the guidance of the present invention, ordinary technicians in this field can also make many forms without departing from the scope of protection of the present invention and the claims, all of which are within the protection of the present invention.

Claims

1. A device for detecting the leakage rate of gloves in a glove box by using vacuum deoxygenation, characterized in that: include: The detection cabin is provided with a cavity and a glove mounting member, and the outer surface of the cavity is provided with a connection hole assembly, and the connection hole assembly includes a plurality of connection holes; The glove mounting piece is located at one end of the cavity and is fastened thereto; the glove mounting piece is provided with a protruding portion with a hollow circular opening, the outer peripheral surface of the protruding portion is provided with at least one annular groove, a sealing ring is provided on the outer side of the annular groove, the sealing ring clamp fixes the glove to be tested on the annular groove, and the glove to be tested, the protruding portion and the cavity together form a space to be tested; A deoxygenation system, the deoxygenation system comprising a vacuum pump and a nitrogen source, the vacuum pump and the nitrogen source are both arranged outside the cavity and connected to the outer surface of the cavity through the connecting hole assembly respectively; the vacuum pump and the nitrogen source work together to reduce the oxygen content of the space to be detected by vacuuming and injecting nitrogen, thereby providing a low oxygen environment; A data acquisition system, the data acquisition system includes a differential pressure gauge and an oxygen analyzer, the differential pressure gauge and the oxygen analyzer are both arranged outside the cavity and connected to the outer surface of the cavity through the connecting hole assembly respectively; the differential pressure gauge and the oxygen analyzer are used to detect the pressure difference and oxygen content of the space to be detected, and output corresponding detection data.

2. The device according to claim 1, characterized in that A circular blocking member is provided at the connection point between the protrusion and the cavity, an internal thread is provided on the inner side of the protrusion, and an external thread is provided on the outer periphery of the blocking member, the internal and external threads cooperate to make the blocking member tightly connected to the inner side of the protrusion to block the connection between the protrusion and the cavity; the blocking member divides the space to be detected into a first space to be detected and a second space to be detected, the first space to be detected is formed between the glove to be detected, the protrusion and the blocking member, and the second space to be detected is formed between the blocking member and the cavity.

3. The device according to claim 2, characterized in that The protrusion is arranged in a step structure, including a first step and a second step, the second step is arranged close to the cavity, and the inner side of the second step is provided with the internal thread.

4. The device according to claim 3, characterized in that The first step is arranged away from the cavity, and the outer peripheral surface of the first step is provided with at least one annular groove.

5. The device according to claim 1, characterized in that The number of the annular grooves is ≥3.

6. The device according to claim 5, characterized in that The diameters of the plurality of annular grooves are different so as to adapt to the cuff sizes of the gloves to be tested.

7. The device according to claim 3, characterized in that A first connecting hole is provided on the outer peripheral surface of the first step, and the vacuum pump is connected to the first to-be-detected space through the first connecting hole.

8. The device according to any one of claims 1 to 7, characterized in that: The glove mounting piece is also provided with a flange portion connected to the protruding portion, and the flange portion is a circular flange structure, which is in direct contact with the end surface of the cavity and is used for fastening connection with the cavity.

9. The device according to any one of claims 1 to 7, characterized in that: The detection chamber is also provided with a sealing cover, which is firmly connected to the other end of the cavity and is used to seal the cavity.

10. The device according to any one of claims 1 to 7, characterized in that: The data acquisition system also includes a thermometer, which is connected to the cavity through the connecting hole assembly and is used to detect the temperature of the gas inside the cavity.

11. A method for detecting leakage rate using the device according to any one of claims 1 to 10, characterized in that: include: The glove mounting member, the blocking member and the sealing cover are sealed and connected to the cavity to form the first to-be-detected space and the second to-be-detected space; Connecting the vacuum pump, the nitrogen source, the differential pressure gauge and the oxygen analyzer to the cavity through the connecting hole assembly; Installing a standard glove on the glove mounting part, reducing the internal oxygen content of the first to-be-detected space and the second to-be-detected space by controlling the vacuum pump and the nitrogen source, and detecting and obtaining a first oxygen concentration change value by means of the differential pressure gauge and the oxygen analyzer; estimating a first leakage rate representing the background leakage of the cavity based on the first oxygen concentration change value, and estimating a corrected third leakage rate based on the first leakage rate; The blocking member is removed, and the oxygen content inside the cavity is reduced by controlling the vacuum pump and the nitrogen source, and the second oxygen concentration change value is detected and calculated by means of the differential pressure gauge and the oxygen analyzer; after the blocking member is installed and the standard glove is replaced with the glove to be tested, the blocking member is removed again, and the oxygen content inside the cavity is reduced by controlling the vacuum pump and the nitrogen source, and the third oxygen concentration change value is detected and calculated by means of the differential pressure gauge and the oxygen analyzer; based on the third leakage rate, the second oxygen concentration change value and the third oxygen concentration change value, the hourly leakage rate of the glove to be tested is calculated according to the following formula: Where: ΔO2——the third oxygen concentration change value of the glove to be tested, expressed in parts per million (ppm) by volume; ΔO1——the second oxygen concentration change value using standard gloves, expressed in parts per million (ppm) by volume; t——test duration, min; T0 - taking into account the corrected leak rate of the cavity (third leak rate).

12. The detection method according to claim 11, characterized in that: The vacuum pump and the nitrogen source reduce the oxygen content inside the chamber, including: Two connecting pipelines are respectively provided between the vacuum pump and the cavity, and between the vacuum pump and the protruding portion, wherein a first switch valve and a second switch valve are respectively provided on the two connecting pipelines, and the first switch valve is opened and the second switch valve is kept closed to extract the internal air of the first to-be-detected space; Close the first switch valve, open the second switch valve, and extract the internal air of the second to-be-detected space; A third switch valve is provided on the connecting pipeline between the nitrogen source and the cavity, and the second switch valve is closed and the third switch valve is opened to inject high-purity nitrogen into the cavity; The above process is repeated, and the oxygen concentration value inside the cavity is observed using the oxygen analyzer until it drops to the required oxygen content detection condition.

Citation Information

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