Leakage rate detection device and detection method for gloves of glove box

Abstract

The invention discloses a leakage rate detection device and method for gloves of a glove box, and the device comprises a detection cabin which is provided with a cavity and a glove installation part, and the glove installation part is located 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 vacuum pump is used for extracting air in the to-be-detected space; the nitrogen source works cooperatively with the vacuum pump and is used for injecting nitrogen into the to-be-detected space so as to reduce the oxygen content of the to-be-detected space; and the oxygen adsorption circulating system further adsorbs and purifies oxygen in the cavity on the basis of collaborative oxygen removal of the vacuum pump and the nitrogen source so as to provide a low-oxygen environment. By means of the device, the glove leakage rate is calculated by comparing the oxygen concentration change of the standard glove and the to-be-detected glove, and by means of multi-stage parameter correction and multi-sealing design, the glove leakage rate is improved, and the reliability of the glove leakage rate is improved. The equipment background leakage rate is effectively reduced, and the reliability of a test result is improved.

Description

Technical Field

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

[0002] In glove box operations, glove box gloves are usually used for experiments or production operations in a closed environment. Their materials include butyl rubber, chloroprene rubber, natural rubber, chlorosulfonated polyethylene, EPDM rubber, and rubber containing lead or tungsten. The gloves are installed on the glove box and are completely sealed and connected to the box body through a certain sealing method to ensure effective isolation of the working environment from the outside world. On the one hand, the environment in the glove box may contain toxic, harmful or radioactive substances, requiring gloves to have good barrier properties to prevent harmful substances from penetrating the gloves and threatening the safety of workers; on the other hand, some operations need to be carried out in an inert gas environment, and gloves should also have high barrier properties to prevent the penetration of air, especially oxygen, to avoid affecting the stability of experimental materials and processes.

[0003] Permeation is one of the main mechanisms of the permeability of glove materials. It refers to the process in which gas dissolves in the material and penetrates the material in molecular form. It is usually manifested as gas molecules adsorbed from one side of the material and reaching the other side through diffusion. The permeation process will not cause physical damage, but it will affect the overall barrier performance of the gloves. Therefore, the leakage rate is used to characterize its air permeability. The glove leakage rate test is an important indicator for detecting its barrier performance. The size of the leakage rate reflects the speed and degree of substances in the air passing through the glove material.

[0004] At present, the overall leakage rate test of the glove box is mainly based on the testing standards of the sealed box, such as GB25915.7 and EJ / T1096, to test the overall sealing of the glove box. However, these standards are mainly aimed at the overall sealing of the box, and cannot specifically evaluate the permeability leakage rate of the gloves themselves, and lack testing methods for the air permeability characteristics of the gloves. Existing glove testing devices mostly focus on air leakage, that is, air tightness, and judge whether the gloves are physically damaged by detecting changes in air pressure, but cannot accurately measure the leakage rate under the glove permeation mechanism, and cannot meet the requirements for accurate evaluation of high-barrier gloves.

[0005] For example, patent CN105716799A proposes to detect the leakage of gloves in glove boxes by changing the cavity pressure or gas concentration, but it is only applicable to qualitative judgment and cannot quantify the leakage caused by penetration. Patent CN109655213A proposes a pressure detection method to detect whether the gloves are damaged by the change of air pressure, but for intact gloves, the pressure drop caused by penetration is small and difficult to detect. Other patents such as CN109374225A and CN202710252U focus on the overall sealing detection of glove boxes, but still cannot achieve the leakage rate test of gloves alone.

[0006] Existing testing methods mainly include pressure drop method and water immersion method, which can only test the integrity of gloves, and there is no special detection method for air leakage caused by the penetration process.

[0007] In view of the above problems, the present invention is proposed. Summary of the invention

[0008] The invention discloses a leakage rate detection device and a detection method for gloves in a glove box, aiming to solve the technical problems existing in the prior art.

[0009] According to one aspect of the present invention, a leakage rate detection device for a glove box glove is provided, comprising:

[0010] 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;

[0011] A vacuum pump is disposed outside the cavity and connected to the outer surface of the cavity through a connecting hole assembly to extract air from the space to be detected;

[0012] A nitrogen source is disposed outside the cavity, connected to the outer surface of the cavity through a connecting hole, and cooperates with the vacuum pump to inject nitrogen into the space to be detected to reduce the oxygen content in the space to be detected;

[0013] The oxygen adsorption circulation system is connected to the vacuum pump and the cavity respectively. On the basis of the coordinated deoxygenation of the vacuum pump and the nitrogen source, the oxygen inside the cavity is further adsorbed and purified to provide a low-oxygen environment;

[0014] A differential pressure gauge is arranged outside the cavity and connected to the cavity through a connecting hole assembly, and is used to detect the pressure difference of the space to be detected;

[0015] Oxygen analyzer: The oxygen analyzer is arranged outside the cavity and connected to the cavity through a connecting hole assembly, and is used to detect the oxygen content in the space to be detected and output corresponding detection data.

[0016] As a preferred technical solution, the connecting hole assembly includes a first connecting hole and a second connecting hole, and the vacuum pump is connected to the first connecting hole and the second connecting hole respectively to form a pipeline connected to the cavity.

[0017] As a preferred technical solution, a third switch valve is provided on the connecting pipeline between the vacuum pump and the first connecting hole, and one end of the oxygen adsorption circulation system is connected to the vacuum pump through the third switch valve.

[0018] As a preferred technical solution, a sealing cover is provided at one end of the cavity away from the glove mounting piece, and an eighth connecting hole is provided on the sealing cover. The oxygen adsorption circulation system is connected to the end of the cavity through the eighth connecting hole.

[0019] 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. The internal and external threads cooperate to ensure that the blocking member is firmly connected to the inner side of the protrusion to block the connection between the protrusion and the cavity.

[0020] 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.

[0021] 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.

[0022] As a preferred technical solution, the number of annular grooves is ≥3.

[0023] 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.

[0024] As a preferred technical solution, the connecting hole assembly also includes a third connecting hole, a fifth connecting hole and a sixth connecting hole. The nitrogen source is connected to the cavity through the third connecting hole, and the differential pressure gauge and the oxygen analyzer are connected to the cavity through the fifth connecting hole and the sixth connecting hole respectively.

[0025] 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.

[0026] As a preferred technical solution, a thermometer is also provided outside the cavity, and the thermometer is connected to the cavity through a connecting hole assembly, and is used to detect the gas temperature inside the cavity.

[0027] According to another aspect of the present invention, a detection method for leak rate detection using the above detection device is also provided, comprising:

[0028] The glove mounting member, the blocking member and the sealing cover are sealed and connected to the cavity; the vacuum pump, the nitrogen source, the differential pressure gauge and the oxygen analyzer are connected to the cavity through the connecting hole assembly; one end of the oxygen adsorption circulation system is connected to the vacuum pump through the third switch valve, and the other end is connected to the cavity through the eighth connecting hole on the sealing cover;

[0029] The standard glove is mounted on the glove mounting part, and the oxygen content inside the cavity is reduced by controlling the vacuum pump, the nitrogen source and the oxygen adsorption circulation system, and a first oxygen concentration change value is detected by using a differential pressure meter 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;

[0030] The blocking member is removed, and the oxygen content inside the cavity is reduced by controlling the vacuum pump, the nitrogen source, and the oxygen adsorption circulation system. 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:

[0031]

[0032] Where:

[0033] ΔO2——the change in the third oxygen concentration of the glove to be tested, expressed in parts per million (ppm) by volume;

[0034] ΔO1 – the change in oxygen concentration using standard gloves, expressed in parts per million (ppm) by volume;

[0035] t——test duration, min;

[0036] T0——Corrected leakage rate taking into account the cavity (third leakage rate).

[0037] As a preferred technical solution, the vacuum pump, the nitrogen source and the oxygen adsorption circulation system reduce the oxygen content through the following steps, including:

[0038] The vacuum pump and the cavity are respectively provided with two connecting pipelines, the two connecting pipelines are respectively provided with a first switch valve and a second switch valve, the blocking member is provided with a seventh connecting hole, the second switch valve is connected to the seventh connecting hole through the second connecting hole, the second switch valve is opened and the first switch valve is kept closed to extract the internal air of the space formed by the standard glove, the glove mounting member and the blocking member;

[0039] The second switch valve is closed, and the first switch valve, the third switch valve and the fourth switch valve are opened, the vacuum pump extracts the internal air of the cavity, and the nitrogen source injects nitrogen into the cavity;

[0040] The third switch valve is adjusted so that one end of the oxygen adsorption circulation system is connected to the vacuum pump, and a fifth switch valve is provided on the connecting pipeline between the other end of the oxygen adsorption circulation system and the eighth connecting hole. The fifth switch valve is opened, and the oxygen adsorption circulation system is circulated multiple times to adsorb and purify the oxygen in the cavity.

[0041] Use an oxygen analyzer to observe the oxygen concentration value inside the cavity until it drops to the required oxygen content detection condition.

[0042] The technical solution adopted by the present invention can achieve at least one of the following beneficial effects:

[0043] 1. Aiming at the particularity of gloves in glove box, the present invention develops a leakage rate detection method based on oxygen content measurement. By setting a glove mounting part for fixing the gloves to be tested, a detection cabin connected to the glove mounting part, a cavity thereof, and a vacuum pump, a nitrogen source, an oxygen adsorption circulation system, 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.

[0044] 2. The present invention uses the synergistic effect of the vacuum pump and the nitrogen source and the dual effect of the oxygen adsorption circulation system to effectively reduce the oxygen content in the test chamber to the ppm level, thereby creating a stable, low-oxygen detection environment and significantly improving the detection accuracy. This design can better reflect the actual air permeability performance of the glove material.

[0045] 3. The device of the present invention has a compact structure and uses multiple sealing designs such as blocking parts and sealing rings, which effectively reduces the background leakage rate of the equipment and makes the test results more real and reliable. In addition, through the relative test method of standard gloves, the interference of the internal volume change of the sealing structure on the test results can be eliminated.

[0046] 4. The present invention ensures the detection accuracy of the glove leakage rate by setting up multi-level steps and multi-parameter corrections, especially correcting the cavity background leakage rate and the sealing structure after the gloves are installed. This method provides a complete and reliable glove leakage rate detection solution, which helps to accurately evaluate the leakage performance of glove materials and provides a scientific basis for the safe operation of the glove box. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] 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:

[0048] Figure 1 A schematic diagram of the working principle of a leakage rate detection device for gloves in a glove box of the present invention;

[0049] Figure 2 It is a schematic diagram of the cross-sectional structure of the detection chamber cavity along AA of the present invention;

[0050] Figure 3 It is a structural schematic diagram of the glove mounting piece of the present invention;

[0051] Figure 4 It is a schematic structural diagram of a blocking member of the present invention;

[0052] Figure 5 It is a schematic diagram of the three-dimensional structure of the sealing cover of the present invention;

[0053] Figure 6 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;

[0054] Figure 7 It is a schematic diagram of the standard glove or the glove to be tested of the present invention in a testing state;

[0055] Figure 8 The present invention is a schematic diagram of the detection process of a leakage rate detection device for gloves in a glove box.

[0056] Description of reference numerals:

[0057] 1. Detection cabin; 11. Cavity; 12. Glove mounting piece; 121. Flange; 122. Protrusion; 13. Connection hole assembly; 131. First connection hole; 132. Second connection hole; 133. Third connection hole; 134. Fourth connection hole; 135. Fifth connection hole; 136. Sixth connection hole; 14. Blocking piece; 141. Seventh connection hole; 142. First handle; 15. Sealing cover; 151. Eighth connection hole; 152. Second handle; 16. Support base; 2. Vacuum pump; 21. First switch valve; 22. Second switch valve; 23. Third switch valve; 3. Nitrogen source; 31. Fourth switch valve; 4. Thermometer; 5. Differential pressure gauge; 6. Oxygen analyzer; 7. Oxygen adsorption circulation system; 71. Fifth switch valve. DETAILED DESCRIPTION

[0058] 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.

[0059] 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.

[0060] 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.

[0061] In order to solve the problems existing in the prior art, an embodiment of the present invention provides a leakage rate detection device for gloves in a glove box, such as Figure 1-Figure 7 As shown, the detection chamber 1 includes a vacuum pump 2, a nitrogen source 3, a thermometer 4, a differential pressure gauge 5, an oxygen analyzer 6 and an oxygen adsorption circulation system 7 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 respectively the first connection hole 131, the second connection hole 132, the third connection hole 133, the fourth connection hole 134, the fifth connection hole 135 and the sixth connection hole 136. The vacuum pump 2 is connected to the cavity 11 through the first connection hole 131 and the second 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 first switch valve 21 is provided on the connection pipeline between the vacuum pump 2 and the first connection hole 131, which is used to control the on-off of the above-mentioned connection pipeline; a second switch valve 22 is provided on the connection pipeline between the vacuum pump 2 and the second 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 third connecting 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 further reduces the oxygen concentration by injecting nitrogen into the cavity 11 to replace the residual oxygen. A fourth switch valve 31 is provided on the connecting pipeline between the nitrogen source 3 and the third connecting hole 133, which is used to control the on-off of the above pipeline. In order to further reduce the oxygen content in the cavity 11, an oxygen adsorption circulation system 7 is also provided to circulate the air in the cavity 11 multiple times to adsorb and purify the remaining oxygen; a third switch valve 23 is also provided on the connecting pipeline between the vacuum pump 2 and the first connecting hole 131. Preferably, the third switch valve 23 is a conductive switch valve. The third switch valve 23 is also located on the connecting pipeline between the oxygen adsorption circulation system 7 and the vacuum pump 2. The third switch valve 23 is used to control the state of a specific pipeline, that is, it can control the connection or disconnection between the oxygen adsorption circulation system 7 and the vacuum pump 2, or control the connection or disconnection between the vacuum pump 2 and the first connecting hole 131. The other end of the oxygen adsorption circulation system 7 is connected to one of the ends of the cavity 11 through the eighth connecting hole 151. The thermometer 4 is connected to the cavity 11 through the fourth connecting 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 fifth connecting hole 135, and is used to monitor the measurement of 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 sixth connecting 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.

[0062] 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 2 and Figure 3As shown, the glove mounting member 12 includes a flange portion 121 and a protrusion 122. 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 glove to be tested, and is arranged as a hollow circular opening structure, and a plurality of annular grooves are arranged on the outside thereof for mounting the glove to be tested. Furthermore, the number of annular grooves is arranged to be at least three, and the diameters of the three annular grooves are arranged to be three different interface sizes, such as 160mm, 180mm, and 200mm. Other diameter sizes can also be arranged as needed. An O-ring is arranged at the above-mentioned annular groove. When the glove to be tested is installed, its cuff is 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 inside of the protrusion 122 is arranged as a step structure. The inside of the protrusion 122 corresponding to the above-mentioned annular groove is a first step, and 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 an internal thread is arranged inside the second step.

[0063] like Figure 2 and Figure 4 As shown, the detection chamber 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 on the inner side of the second step. The blocking member 14 is also provided with a first handle 142, 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 blocking and sealing role; when the blocking member 14 is screwed by the first handle 142, the space formed by the installed glove and the protrusion 122 is connected with the cavity 11 when it is removed. A seventh connecting hole 141 is also provided on the blocking member 14, and the second connecting hole 132 is connected to the seventh connecting hole 141 by a pipeline, so that the vacuum pump 2 can extract air from the space formed by the glove to be tested, the glove mounting member 12 and the blocking member 14 through the second connecting hole 132, the seventh connecting hole 141 and the pipeline therebetween.

[0064] like Figure 5As shown, the detection cabin 1 is also provided with a sealing cover 15 at the other end of the cavity 11, and the sealing cover 15 is fixedly connected to the other end of the cavity 11, which is used to close the cavity 11 and 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, convenient for maintenance and maintenance, and prolong the service life of the detection device. Further preferably, a second handle 152 is also provided on the sealing cover 15 for easy disassembly or replacement. The sealing cover 15 is also provided with an eighth connecting hole 151, which is connected to the oxygen adsorption circulation system 7 through a pipeline, so that the oxygen adsorption circulation system 7 is connected to the bottom of the cavity 11. A fifth switch valve 71 is also provided on the above pipeline to control the on-off of the above pipeline.

[0065] 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.

[0066] The detection chamber 1 is connected to the vacuum pump 2, the nitrogen source 3 and the oxygen adsorption circulation system 7, and cooperates to quickly reduce the oxygen concentration by vacuuming. The vacuum pump 2 reduces the oxygen content in the cavity 11 by exhausting air. The nitrogen source 3 injects nitrogen into the cavity 11 after the vacuum pump 2 works to further replace the oxygen. The oxygen adsorption circulation system 7 further adsorbs and purifies the remaining oxygen to 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. During operation, after the blocking member 14 is installed, the volume inside the cavity 11 is fixed. According to the Clapeyron equation:

[0067] PV=nRT

[0068] 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.

[0069] 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.

[0070] 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).

[0071] In some preferred embodiments, the above-mentioned standard gloves are made of high barrier materials such as butyl rubber.

[0072] 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.

[0073] In some preferred implementation schemes, in order to increase the air barrier property of the cavity 11 and improve the detection accuracy, the cavity 11 is made of stainless steel.

[0074] In some preferred embodiments, the inner surface of the cavity 11 is coated with a coating, such as an Al2O3 coating, to improve air barrier properties.

[0075] 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.

[0076] 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.

[0077] In some preferred embodiments, the sealing cover 15 is connected to the cavity 11 via a sealing clamp.

[0078] 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.

[0079] The present invention also provides a detection method for detecting the leakage rate of gloves in a glove box, comprising the following steps:

[0080] 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 first connecting hole 131, the second connecting hole 132, the third connecting hole 133, the fourth connecting hole 134, the fifth connecting hole 135 and the sixth connecting hole 136 respectively; the pipeline between the second connecting hole 132 and the seventh connecting hole 141 is connected, so that the vacuum pump 2 is further connected to the space formed by the glove mounting member 12 and the blocking member 14; one end of the oxygen adsorption circulation system 7 is connected to the third switch valve 23 through a pipeline, and the other end is connected to the sealing cover 15 through the eighth connecting hole 151, so as to achieve connection with the bottom end of the cavity 11.

[0081] 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.

[0082] 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.

[0083] S22 : Open the second switch valve 22 , 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 second connecting hole 132 .

[0084] S23: close the second switch valve 22, open the third switch valve 23 and the first switch valve 21, so that the pipeline between the vacuum pump 2 and the first connecting hole 131 is connected, open the fourth switch valve 31, and the vacuum pump 2 extracts the air inside the cavity 11 through the first connecting hole 131, that is, the air in the second test space, and the nitrogen source 3 injects high-purity nitrogen into the cavity 11 through the third connecting hole 133; observe the decrease in oxygen concentration in the cavity 11 through the oxygen analyzer 6, and when the oxygen concentration in the cavity 11 reaches a small decrease and is relatively stable, close the fourth switch valve 31.

[0085] S24: Open the fifth switch valve 71, adjust the third switch valve 23, so that the oxygen adsorption circulation system 7 is connected to the vacuum pump 2, and the oxygen adsorption circulation system 7 circulates multiple times to further adsorb and purify the remaining oxygen in the cavity 11, and use the oxygen analyzer 6 to observe the oxygen concentration value inside the cavity 11. When the oxygen concentration value drops to ≤50ppm, close the oxygen adsorption circulation system 7, the second switch valve 22 and the fifth switch valve 71; preferably, the oxygen concentration value is reduced to ≤10ppm.

[0086] S25: Using the vacuum pump 2 and the differential pressure gauge 5, the relative pressure inside the cavity 11 is adjusted to the detection condition, that is, (-1100 to -900) Pa.

[0087] 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.

[0088] 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.

[0089] 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).

[0090] S31: Figure 6 As shown, the vacuum pump 2 fills a certain amount of nitrogen into the standard glove through the second connecting hole 132 and the seventh connecting hole 171; through the standard glove, the blocking member 14 is unscrewed and pushed into the cavity 11, so that the first space to be tested is connected with the second space to be tested. Due to the negative pressure, the standard glove will automatically expand inside the cavity 11, as shown in FIG. Figure 7 shown.

[0091] S32: Adjust the third switch valve 23 so that the oxygen adsorption circulation system 7 is connected to the vacuum pump 2, open the first switch valve 21 and the fifth switch valve 71, and circulate the oxygen adsorption circulation system 7 multiple times to further adsorb and purify the remaining oxygen in the cavity 11, and use the oxygen analyzer 6 to observe the oxygen concentration value inside the cavity 11. When the oxygen concentration value drops to ≤50ppm, close the oxygen adsorption circulation system 7, the second switch valve 22 and the fifth switch valve 71; preferably, the oxygen concentration value is reduced to ≤10ppm.

[0092] S33: Using the vacuum pump 2 and the differential pressure gauge 5, the relative pressure inside the cavity 11 is adjusted to the detection condition, that is, (-1100 to -900) Pa.

[0093] S34: 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.

[0094] S35: 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.

[0095] S36: For the gloves to be tested, S22 to S25 are repeated. After the above test 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.

[0096] S37: Calculate the hourly leakage rate of the gloves to be tested using the following formula:

[0097]

[0098] Where:

[0099] ΔO2——the change in the third oxygen concentration of the glove to be tested, expressed in parts per million (ppm) by volume;

[0100] ΔO1 – the change in oxygen concentration using standard gloves, expressed in parts per million (ppm) by volume;

[0101] t——test duration, min;

[0102] T0——Consider the corrected leakage rate of the device (third leakage rate).

[0103] 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 glove box glove leakage rate detection device, 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 vacuum pump, which is arranged outside the cavity and connected to the outer surface of the cavity through the connecting hole assembly, and is used to extract air from the space to be detected; A nitrogen source, which is disposed outside the cavity, connected to the outer surface of the cavity through the connecting hole, and cooperates with the vacuum pump to inject nitrogen into the space to be detected to reduce the oxygen content of the space to be detected; An oxygen adsorption circulation system, wherein the oxygen adsorption circulation system is connected to the vacuum pump and the cavity respectively, and further adsorbs and purifies the oxygen inside the cavity on the basis of the coordinated deoxygenation of the vacuum pump and the nitrogen source to provide a low oxygen environment; A differential pressure gauge, which is arranged outside the cavity and connected to the cavity through the connecting hole assembly, and is used to detect the pressure difference of the space to be detected; An oxygen analyzer is arranged outside the cavity and connected to the cavity through the connecting hole assembly, and is used to detect the oxygen content of the space to be detected and output corresponding detection data.

2. The detection device according to claim 1, characterized in that: The connecting hole assembly includes a first connecting hole and a second connecting hole, and the vacuum pump is connected to the first connecting hole and the second connecting hole respectively to form a pipeline connected to the cavity.

3. The detection device according to claim 2, characterized in that: A third switch valve is provided on the connecting pipeline between the vacuum pump and the first connecting hole, and one end of the oxygen adsorption circulation system is connected to the vacuum pump through the third switch valve.

4. The detection device according to claim 1, characterized in that: A sealing cover is provided at one end of the cavity away from the glove mounting piece, and an eighth connecting hole is provided on the sealing cover. The oxygen adsorption circulation system is connected to the end of the cavity through the eighth connecting hole.

5. The detection 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, and the internal and external threads cooperate to ensure that the blocking member is firmly connected to the inner side of the protrusion to block the connection between the protrusion and the cavity.

6. The detection device according to claim 5, 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.

7. The detection device according to claim 6, 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.

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

9. The detection device according to claim 8, 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.

10. The detection device according to claim 1, characterized in that: The connecting hole assembly also includes a third connecting hole, a fifth connecting hole and a sixth connecting hole. The nitrogen source is connected to the cavity through the third connecting hole, and the differential pressure gauge and the oxygen analyzer are connected to the cavity through the fifth connecting hole and the sixth connecting hole, respectively.

11. The detection device according to any one of claims 1 to 10, 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.

12. The detection device according to any one of claims 1 to 10, characterized in that: A thermometer is also provided outside the cavity, and the thermometer is connected to the cavity through the connecting hole assembly, and is used to detect the temperature of the gas inside the cavity.

13. A detection method for leak rate detection using the detection device according to any one of claims 1 to 12, characterized in that: include: The glove mounting member, the blocking member and the sealing cover are sealed and connected to the cavity; the vacuum pump, the nitrogen source, the differential pressure gauge and the oxygen analyzer are connected to the cavity through the connecting hole assembly; one end of the oxygen adsorption circulation system is connected to the vacuum pump through the third switch valve, and the other end is connected to the cavity through the eighth connecting hole on the sealing cover; Installing a standard glove on the glove mounting part, reducing the oxygen content inside the cavity by controlling the vacuum pump, the nitrogen source and the oxygen adsorption circulation system, 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, the nitrogen source and the oxygen adsorption circulation system, and the second oxygen concentration change value is detected and calculated by means of the differential pressure gauge and the 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, 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).

14. The detection method according to claim 13, characterized in that: The vacuum pump, the nitrogen source and the oxygen adsorption circulation system reduce the oxygen content by the following steps, including: The vacuum pump and the cavity are respectively provided with two connecting pipelines, the two connecting pipelines are respectively provided with a first switch valve and a second switch valve, the blocking member is provided with a seventh connecting hole, the second switch valve is connected to the seventh connecting hole through the second connecting hole, the second switch valve is opened and the first switch valve is kept closed to extract the internal air of the space formed by the standard glove, the glove mounting member and the blocking member; The second switch valve is closed, and the first switch valve, the third switch valve and the fourth switch valve are opened, the vacuum pump extracts the internal air of the cavity, and the nitrogen source injects nitrogen into the cavity; The third switch valve is adjusted so that one end of the oxygen adsorption circulation system is connected to the vacuum pump, and a fifth switch valve is provided on the connecting pipeline between the other end of the oxygen adsorption circulation system and the eighth connecting hole, and the fifth switch valve is opened to circulate the oxygen adsorption circulation system for multiple times to adsorb and purify the oxygen in the cavity; The oxygen analyzer is used to observe the oxygen concentration value inside the cavity until it drops to the required oxygen content detection condition.

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