A glove box glove leak rate detection apparatus and method

Abstract

The application discloses a glove box glove leak rate detection device and a detection method, a detection cabin, the detection cabin is provided with a cavity and a glove mounting piece, the glove mounting piece is located at one end of the cavity and is fastened and connected with the cavity; the glove mounting piece is provided with a convex part with a hollow circular opening, a glove to be detected, the convex part and the cavity jointly form a space to be detected; a vacuum pump is used for extracting air in the space to be detected; a nitrogen source cooperates with the vacuum pump and is used for injecting nitrogen into the space to be detected to reduce the oxygen content of the space to be detected; an oxygen adsorption circulation system further adsorbs and purifies oxygen in the cavity on the basis of oxygen removal by the vacuum pump and the nitrogen source, so as to provide a low-oxygen environment. By means of the above-mentioned device, the oxygen concentration changes of standard gloves and gloves to be detected are compared, the glove leak rate is calculated, and through multi-stage parameter correction and multiple sealing design, the background leak rate of the equipment is effectively reduced, and the reliability of the test result is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of individual radiation protection equipment detection, and particularly relates to a glove box glove leakage rate detection device and a detection method. BACKGROUND

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

[0003] Permeation, as one of the main mechanisms of the air permeability of glove materials, is the process of gas dissolving in the material and penetrating the material in the form of molecules, which is usually manifested as the adsorption of gas molecules from one side of the material and the diffusion to the other side. The permeation process does not cause physical damage, but affects the overall barrier properties of the gloves, and therefore the air permeability of the gloves is characterized by the leakage rate. The glove leakage rate test is an important indicator for detecting the barrier properties thereof, and the size of the leakage rate reflects the speed and degree of air substances passing through the glove material.

[0004] At present, the overall leakage rate test of the glove box mainly depends on the detection standards for the sealed box body, such as GB25915.7 and EJ / T1096, to detect the overall sealing performance of the glove box. However, these standards mainly aim at the overall sealing performance of the box body, and cannot specially evaluate the permeation leakage rate of the gloves themselves, and lack testing means for the air permeation properties of the gloves. The existing glove detection devices are mainly concentrated on air leakage, i.e. air tightness, and the change in air pressure is detected to determine whether the gloves have physical damage, but the leakage rate under the permeation mechanism of the gloves cannot be accurately measured, and the accurate evaluation of high barrier gloves cannot be met.

[0005] For example, patent CN105716799A proposes to detect glove leakage in a glove box by changes in cavity pressure or gas concentration, but it is only suitable for qualitative judgment and cannot quantify the leakage caused by permeation. Patent CN109655213A proposes a pressure detection method to detect whether the glove is damaged by air pressure changes, but for intact and undamaged gloves, the air pressure drop caused by permeation is small and difficult to detect. Other patents such as CN109374225A and CN202710252U focus on detecting the overall sealing of the glove box, and still cannot achieve individual leakage rate testing of the glove.

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

[0007] In view of the above problems, the present application is proposed. SUMMARY

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

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

[0010] a detection cabin, the detection cabin is provided with a cavity and a glove mounting piece, the outer surface of the cavity is provided with a connecting hole assembly, the connecting hole assembly comprises a plurality of connecting holes; the glove mounting piece is located at one end of the cavity and is tightly connected therewith; the glove mounting piece is provided with a convex part with a hollow circular opening, the outer peripheral surface of the convex part is provided with at least one annular groove, the outer side of the annular groove is provided with a sealing ring, the sealing ring clamps and fixes a glove to be detected on the annular groove, the glove to be detected, the convex part and the cavity together form a detection space;

[0011] a vacuum pump, the vacuum pump is arranged outside the cavity and is connected with the outer surface of the cavity through the connecting hole assembly, and is used for extracting air in the detection space;

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

[0013] an oxygen adsorption circulation system, the oxygen adsorption circulation system is connected with the vacuum pump and the cavity respectively, and further adsorbs and purifies the oxygen in the cavity on the basis of oxygen removal by the vacuum pump and the nitrogen source, so as to provide a low-oxygen environment;

[0014] a differential pressure gauge, the differential pressure gauge is arranged outside the cavity and is connected with the cavity through the connecting hole assembly, and is used for detecting the pressure difference in the detection space;

[0015] The oxygen analyzer is arranged outside the cavity and connected to the cavity through a connecting hole component. It 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 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 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 accommodate 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. 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 further provided outside the cavity, and the thermometer is connected to the cavity through a connecting hole assembly for detecting the gas temperature inside the cavity.

[0027] According to another aspect of the present application, there is also provided a detection method for detecting the leakage rate by using the detection device, comprising:

[0028] The glove mounting member, the blocking member and the sealing cover are sealingly 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 member, the oxygen content in the cavity is reduced by controlling the vacuum pump, the nitrogen source and the oxygen adsorption circulation system, and the first oxygen concentration change value is detected by the differential pressure gauge and the oxygen analyzer; the first leakage rate representing the background leakage of the cavity is estimated based on the first oxygen concentration change value, and the third leakage rate is estimated based on the first leakage rate;

[0030] The blocking member is removed, the oxygen content in 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 the differential pressure gauge and the oxygen analyzer; after the blocking member is installed and the standard glove is replaced by the glove to be detected, the blocking member is removed again, the oxygen content in 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 the differential pressure gauge and the oxygen analyzer; the hourly leakage rate of the glove to be detected is calculated based on the third leakage rate, the second oxygen concentration change value and the third oxygen concentration change value according to the following formula:

[0031]

[0032] In the formula:

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

[0034] ΔO1 is the second oxygen concentration change value of the standard glove, expressed in volume parts per million (ppm);

[0035] t is the test duration, min;

[0036] T0 is the corrected leakage rate (third leakage rate) considering the cavity.

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

[0038] The vacuum pump and the cavity are respectively provided with two connecting pipelines, the first switch valve and the second switch valve are arranged on the two connecting pipelines respectively, the seventh connecting hole is arranged on the blocking piece, the second switch valve is connected with the seventh connecting hole through the second connecting hole, the internal air of the space formed by the standard glove, the glove mounting piece and the blocking piece is extracted by opening the second switch valve and keeping the first switch valve in the closed state;

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

[0040] The third switch valve is adjusted so that one end of the oxygen adsorption circulation system is connected with the vacuum pump, the other end of the oxygen adsorption circulation system is connected with the communication pipeline of the eighth connecting hole, the fifth switch valve is arranged on the communication pipeline, the fifth switch valve is opened, the oxygen in the cavity is adsorbed and purified through multiple circulation of the oxygen adsorption circulation system;

[0041] The oxygen concentration value in the cavity is observed by using the oxygen analyzer until it is reduced to the required oxygen content detection condition.

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

[0043] 1、 The present application develops a leakage rate detection method based on oxygen content measurement according to the particularity of the glove box glove, through setting the glove mounting piece for fixing the glove to be detected, the detection cabin connected with the glove mounting piece, the cavity thereof and the vacuum pump, the nitrogen source, the oxygen adsorption circulation system, the differential pressure gauge and the oxygen analyzer connected with the cavity, based on specific detection steps, the air permeability of the glove can be accurately detected, and it is especially suitable for gloves of various materials and caliber sizes.

[0044] 2、 The present application uses the synergistic effect of the vacuum pump and the nitrogen source and the double effect of the oxygen adsorption circulation system, so that the oxygen content in the test cabin can be effectively reduced to the ppm level, thereby creating a stable and low-oxygen detection environment, and the detection precision is significantly improved. This design can better reflect the real air permeability of the glove material.

[0045] 3、 The device structure of the present application is compact, multiple sealing designs such as blocking pieces and sealing rings are used, the background leakage rate of the equipment is effectively reduced, and the detection result is more true and reliable. In addition, through the relative test method of the standard glove, the interference of the volume change in the sealing structure on the test result can be excluded.

[0046] 4、The present application sets up multistage steps and multivariable correction, especially corrects the cavity background leakage rate and the sealing structure after the glove installation, ensures the detection precision of the glove leakage rate. The method provides a complete and reliable glove leakage rate detection scheme, helps to accurately evaluate the leakage performance of the glove material, and provides a scientific basis for the safe operation of the glove box. BRIEF DESCRIPTION OF DRAWINGS

[0047] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiment description will be briefly introduced as follows, which form a part of the present application. The schematic embodiments of the present application and the description and explanation thereof do not constitute an improper limitation on the present application. In the drawings:

[0048] Figure 1 It is a working principle schematic diagram of a glove box glove leakage rate detection device of the present application;

[0049] Figure 2 It is a cross-sectional structure schematic diagram of a detection cabin cavity along A-A of the present application;

[0050] Figure 3 It is a structure schematic diagram of a glove installation piece of the present application;

[0051] Figure 4 It is a structure schematic diagram of a blocking piece of the present application;

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

[0053] Figure 6 It is a structure schematic diagram of a standard glove or a to-be-detected glove installed on a glove installation piece of the present application;

[0054] Figure 7 It is a schematic diagram of a standard glove or a to-be-detected glove in a detection state of the present application;

[0055] Figure 8 It is a detection flowchart schematic diagram of a glove box glove leakage rate detection device of the present application.

[0056] Explanation of reference signs:

[0057] 1. detection cabin; 11. cavity; 12. glove mounting; 121. flange part; 122. protruding part; 13. connecting hole assembly; 131. first connecting hole; 132. second connecting hole; 133. third connecting hole; 134. fourth connecting hole; 135. fifth connecting hole; 136. sixth connecting hole; 14. blocking piece; 141. seventh connecting hole; 142. first handle; 15. sealing cover; 151. eighth connecting hole; 152. second handle; 16. support base; 2. vacuum pump; 21. first on-off valve; 22. second on-off valve; 23. third on-off valve; 3. nitrogen source; 31. fourth on-off valve; 4. thermometer; 5. differential pressure gauge; 6. oxygen analyzer; 7. oxygen adsorption circulation system; 71. fifth on-off valve. DETAILED DESCRIPTION

[0058] In order to make the objects, technical solutions and advantages of the present application clearer, the technical solutions of the present application will be described clearly and completely below in conjunction with specific embodiments of the present application and corresponding drawings. In the description of the present application, it should be noted that the term "or" is generally used in the sense of including "and / or" unless the context clearly indicates otherwise.

[0059] In the description of the present application, it should be noted that unless otherwise explicitly specified and limited, the terms "mounting", "connection" and "linking" should be understood in a broad sense, for example, can be fixed connection, can also be detachable connection, or integrally connected; can be mechanical connection, can also be magnetic connection; can be directly connected, can also be indirectly connected through an intermediate medium, can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances. In addition, in the description of the present application, the terms "first", "second" and the like are only used for distinguishing description, and cannot be understood as indicating or implying relative importance.

[0060] Obviously, the described embodiments are only a part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0061] In order to solve the problems existing in the prior art, the glove box glove leak rate detection device provided by the embodiments of the present application is shown in Figures 1-7 As shown, it comprises a detection cabin 1, and 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 connected with the detection cabin 1 respectively. The detection cabin 1 comprises a cavity 11, and the outer surface of the cavity 11 is provided with a connecting hole assembly 13 comprising six connecting holes for connecting external equipment with the inside of the cavity 11. Figure 2As shown, the six connecting holes are respectively a first connecting hole 131, a second connecting hole 132, a third connecting hole 133, a fourth connecting hole 134, a fifth connecting hole 135 and a sixth connecting hole 136. The vacuum pump 2 is connected with the cavity 11 through the first connecting hole 131 and the second connecting hole 132, and is used to realize an efficient oxygen removal process by adjusting the air pressure inside the detection cabin 1, that is, to extract the air inside the cavity 11, reduce the oxygen content in the cavity 11, and thus form a low-oxygen environment, so as to accurately detect the glove leakage rate of the glove box. A first switch valve 21 is arranged on the connecting pipeline of the vacuum pump 2 and the first connecting hole 131, and is used to control the on-off of the above connecting pipeline; a second switch valve 22 is arranged on the connecting pipeline of the vacuum pump 2 and the second connecting hole 132, and is used to control the on-off of the pipeline. The nitrogen source 3 is connected with the cavity 11 through the third connecting hole 133, and is used to provide a low-oxygen environment for the inside of the cavity 11, and assist the vacuum pump 2 to realize a more stable and accurate oxygen removal 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, and further reduces the oxygen concentration. A fourth switch valve 31 is arranged on the connecting pipeline of the nitrogen source 3 and the third connecting hole 133, and 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 arranged, which circulates the air in the cavity 11 for multiple times to adsorb and purify the residual oxygen; a third switch valve 23 is further arranged on the connecting pipeline of the vacuum pump 2 and the first connecting hole 131, and preferably, the third switch valve 23 is a conductive switch valve. The third switch valve 23 is arranged on the connecting pipeline of the oxygen adsorption circulation system 7 and the vacuum pump 2, and is used to control the state of a specific pipeline, that is, it can control the connection or disconnection of the oxygen adsorption circulation system 7 and the vacuum pump 2, or control the connection or disconnection of the vacuum pump 2 and the first connecting hole 131. The other end of the oxygen adsorption circulation system 7 is connected with one of the end portions of the cavity 11 through an eighth connecting hole 151. The thermometer 4 is connected with the cavity 11 through the fourth connecting hole 134, and is used to monitor the temperature inside the cavity 11 in real time, so as to ensure that the glove box glove leakage rate detection process is carried out under stable and suitable temperature conditions. The differential pressure gauge 5 is connected with the cavity 11 through the fifth connecting 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 with the cavity 11 through the sixth connecting hole 136, and can accurately detect the trace oxygen level inside the cavity 11 in real time, and provide core data support for the leakage rate detection.

[0062] As shown in FIG. 1, Figures 2-5 As shown in FIG. 1, Figure 2 and Figure 3As shown, the glove mounting member 12 comprises a flange portion 121 and a protruding portion 122. The flange portion 121 is a circular flange structure, and a plurality of mounting holes are uniformly distributed on the flange for bolts or screws to pass through and fixedly connected with one end of the cavity 11. The protruding portion 122 is used for fixing the gloves to be detected, and is provided in a hollow circular opening structure, and a plurality of annular grooves are provided on the outside of the protruding portion 122 for mounting the gloves to be detected. Further, the number of annular grooves is provided as at least three, and the diameters of the three annular grooves are provided as three different interface sizes, for example, 160mm, 180mm, and 200mm. According to needs, other diameter sizes can also be provided. O-rings are provided at the annular grooves, and when the gloves to be detected are mounted, the cuffs are placed at the positions of the annular grooves, and are fixed by the O-rings, and at the same time, the O-rings can maximize the reduction of oxygen leakage at the glove mounting member 12, and achieve a good sealing effect. The inside of the protruding portion 122 is provided in a stepped structure, the inside of the protruding portion 122 corresponding to the annular grooves is a first step, and the inside of the protruding portion 122 between the annular grooves and the flange portion 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 provided on the inside of the second step.

[0063] As shown in Figure 2 and Figure 4 As shown, the detection cabin 1 is also provided with a blocking member 14 located at the communication position of the protruding portion 122 and the cavity 11. The blocking member 14 is provided in a circular shape, and the outer periphery of the blocking member 14 is in contact with the inside of the second step of the protruding portion 122. An external thread is provided on the outer periphery of the blocking member 14, and matches the internal thread on the inside of the second step. A first handle 142 is also provided on the blocking member 14, and the blocking member 14 can be screwed with the inside of the protruding portion 122 through the first handle 142 to block the hollow circular opening structure of the glove mounting member 12. In the glove mounting state, the blocking member 14 blocks the communication position of the gloves and the cavity 11, and plays a blocking and sealing role. When the blocking member 14 is screwed through the first handle 142, the space formed by the gloves and the protruding portion 122 is communicated with the cavity 11. A seventh connecting hole 141 is also provided on the blocking member 14, and the second connecting hole 132 and the seventh connecting hole 141 are connected through a pipeline, so that the vacuum pump 2 can extract air from the space formed by the gloves to be detected, 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] As shown in Figure 5As shown, the detection cabin 1 is also provided with a sealing cover 15 at the other end of the cavity 11, which is fixedly connected with the other end of the cavity 11 and used for closing the cavity 11 to ensure the air tightness of the internal environment of the cavity 11, so as to maintain the specific conditions such as low oxygen and low pressure in the glove leakage rate detection process and avoid the interference of 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 arranged to be convenient for disassembly or replacement, facilitating maintenance and prolonging the service life of the detection device. Further preferably, the sealing cover 15 is also provided with a second handle 152 for facilitating disassembly or replacement. The sealing cover 15 is also provided with an eighth connecting hole 151 connected with the oxygen adsorption circulation system 7 through a pipeline, so that the oxygen adsorption circulation system 7 is connected with the bottom of the cavity 11. The above-mentioned pipeline is also provided with a fifth on-off valve 71 for controlling the opening and closing of the above-mentioned pipeline.

[0065] The above-mentioned structure design can accurately detect the leakage rate of the glove box gloves by creating a low-oxygen environment and detecting relevant data in real time.

[0066] The detection cabin 1 is connected with the vacuum pump 2, the nitrogen source 3 and the oxygen adsorption circulation system 7, which cooperate to quickly reduce the oxygen concentration through vacuum pumping. The vacuum pump 2 reduces the oxygen content in the cavity 11 through air pumping, the nitrogen source 3 injects nitrogen into the cavity 11 after the vacuum pump 2 works to further displace oxygen, and 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) of the gas in the cabin, so as to realize rapid oxygen removal. When operating, the volume inside the cavity 11 is fixed after the blocking piece 14 is installed. According to the Clapeyron equation:

[0067] PV=nRT

[0068] Wherein P is the pressure in the cavity 11, V is the volume in the cavity 11, n is the amount of substance of air in the cavity 11, and R is the molar gas constant. At a constant temperature, the temperature fluctuation and the volume change are ignored, V, R and T are constants, and then P∝n.

[0069] In terms of data monitoring, the gloves to be detected are first connected with the cavity 11 through the glove mounting piece 12. The design of the blocking piece 14 and the sealing cover 15 enhances the air tightness of the cavity 11 and avoids the interference of the external environment on the detection result. The cavity 11 is connected with the thermometer 4, the pressure difference meter 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] In order to ensure the consistency of the detection conditions, especially the consistency of the internal volume formed by the glove to be detected and the cavity 11 during detection, first, the blocking piece 14 is fixed between the glove mounting piece 12 and the cavity 11. Using the standard glove and the above-mentioned detection device structure, the first oxygen concentration change value after installing the standard glove is detected, 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, i.e. the third leakage rate. Second, the blocking piece 14 is removed, and the second oxygen concentration change value of the standard glove is detected. Third, the standard glove is removed, and the glove to be detected is installed. Then, the third oxygen concentration change value before and after the removal of the blocking piece 14 is detected by the above-mentioned detection device. Through the second oxygen concentration change value, the third oxygen concentration change value, and the first leakage rate (i.e. the background leakage rate) and the corrected leakage rate (the third leakage rate) values, the required leakage rate result of the glove to be detected is calculated according to the formula.

[0071] In some preferred embodiments, the above-mentioned standard glove is made of high barrier material 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 during glove detection, reduce the potential oxygen leakage of the detection device itself, and improve the detection accuracy, the cavity 11 is designed in a cylindrical barrel shape. Preferably, in order to meet the detection needs of various glove box gloves, the diameter of the cavity 11 is designed to be 200-300 mm, which is larger than the sleeve size of various existing glove box gloves; the axial length of the cavity 11 is designed to be 850-950 mm, which is larger than the length of various existing glove box gloves.

[0073] In some preferred embodiments, 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 material.

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

[0075] In some preferred embodiments, the thermometer 4 adopts a thermocouple structure to measure the temperature of the gas inside the cavity 11 during detection.

[0076] In some preferred embodiments, the differential pressure gauge 5 adopts a micro differential pressure sensor to measure the relative pressure difference of the gas inside the cavity 11 during detection.

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

[0078] In some preferred embodiments, the detection cabin 1 further comprises a plurality of support bases 16 for providing a firm foundation for the entire device, ensuring that the equipment remains balanced during operation, avoiding tilting or displacement due to external forces or internal pressure changes. Preferably, the number of support bases 16 is 2-4.

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

[0080] S1: The glove mounting member 12, the blocking member 14, and the sealing cover 15 are sealingly connected with the cavity 11, forming a first space to be measured between the glove, the glove mounting member 12, and the blocking member 14, and forming a second space to be measured 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 pressure difference meter 5, and the oxygen analyzer 6 are connected with 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; a pipeline is connected between the second connecting hole 132 and the seventh connecting hole 141, so that the vacuum pump 2 is further connected with 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 with the third switch valve 23 through a pipeline, and the other end is connected with the sealing cover 15 through the eighth connecting hole 151, so as to be connected with the bottom end of the cavity 11.

[0081] S2: The first oxygen concentration and the second oxygen concentration are detected through the above structure, the first oxygen concentration change value is obtained by calculation, and the background leakage rate (first leakage rate) and the corrected leakage rate (third leakage rate) are estimated based on the above first oxygen concentration change value.

[0082] S21: A standard glove is installed, so that the standard glove is placed in the ring groove closest to the flange 121, and the other two ring grooves are fixed with O-rings, so that the standard glove is in a sealed state with the glove mounting member 12.

[0083] S22: The second switch valve 22 is opened, and the vacuum pump 2 extracts the air in the first space to be measured formed by the standard glove, the glove mounting member 12, and the blocking member 14 through the second connecting hole 132.

[0084] S23: The second switch valve 22 is closed, the third switch valve 23 and the first switch valve 21 are opened, so that the pipeline between the vacuum pump 2 and the first connecting hole 131 is connected, the fourth switch valve 31 is opened, the vacuum pump 2 extracts the air in the cavity 11, i.e. the air in the second space to be measured, through the first connecting hole 131, and the nitrogen source 3 injects high-purity nitrogen into the cavity 11 through the third connecting hole 133; the oxygen concentration in the cavity 11 is observed by the oxygen analyzer 6, and when the oxygen concentration in the cavity 11 reaches a small degree of decline and is relatively stable, the fourth switch valve 31 is closed.

[0085] S24: open the fifth switch valve 71, adjust the third switch valve 23 so that the oxygen adsorption circulation system 7 is in communication with the vacuum pump 2, through multiple cycles of the oxygen adsorption circulation system 7, further adsorb and purify the remaining oxygen in the cavity 11, use the oxygen analyzer 6 to observe the oxygen concentration value inside the cavity 11, when the oxygen concentration value is reduced 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: 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~ -900) Pa.

[0087] S26: after the above detection condition is stable, record the first oxygen concentration using the oxygen analyzer 6, use the timer (not marked in the figure) to time, after a certain time, record the second oxygen concentration using the oxygen analyzer 6, obtain the first oxygen concentration change value through the first oxygen concentration and the second oxygen concentration value, calculate the background leakage rate of the cavity 11 (the first leakage rate) based on the above first oxygen concentration change value. Preferably, the certain time is 30min~60min.

[0088] S27: use the above background leakage rate (the first leakage rate), combined with the volume of the cavity 11 itself and the volume after the standard glove expands, to estimate the corrected leakage rate (the third leakage rate).

[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 detected, based on the above second oxygen concentration change value, the third oxygen concentration change value and the above corrected leakage rate (the third leakage rate) to calculate the leakage rate of the glove to be detected.

[0090] S31: as shown in Figure 6 , 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 piece 14 is unscrewed and pushed into the cavity 11, so that the first to be measured space is in communication with the second to be measured space, due to the negative pressure, the standard glove will automatically expand inside the cavity 11, as shown in Figure 7 .

[0091] S32: adjust the third switch valve 23 so that the oxygen adsorption circulation system 7 is in communication with the vacuum pump 2, open the first switch valve 21 and the fifth switch valve 71, through multiple cycles of the oxygen adsorption circulation system 7, further adsorb and purify the remaining oxygen in the cavity 11, use the oxygen analyzer 6 to observe the oxygen concentration value inside the cavity 11, when the oxygen concentration value is reduced 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: The relative pressure inside the cavity 11 is regulated to the detection condition, i.e. (-1100~ -900) Pa, by using the vacuum pump 2 and the differential pressure gauge 5.

[0093] S34: After the detection condition is stable, the third oxygen concentration is recorded by using the oxygen analyzer 6, and the timer (not shown in the figure) is used to time, and after a certain time, the fourth oxygen concentration is recorded by using the oxygen analyzer 6, and the difference between the third oxygen concentration and the fourth oxygen concentration is taken as the second oxygen concentration change value under the standard glove. Preferably, the certain time is 30 min~60 min.

[0094] S35: The blocking piece 14 is screwed through the standard glove, connected to the inner side of the protruding part 122 of the glove mounting piece 12, and blocks the hollow circular opening structure of the glove mounting piece 12, playing a sealing role. At this time, the standard glove is removed, and the glove to be tested is installed.

[0095] S36: For the glove to be tested, S22~S25 is repeated, after the detection condition is stable, the fifth oxygen concentration is recorded by using the oxygen analyzer 6, and the timer (not shown in the figure) is used to time, and after a certain time, the sixth oxygen concentration is recorded by using the oxygen analyzer 6, and the difference between the fifth oxygen concentration and the sixth oxygen concentration is taken as the third oxygen concentration change value under the standard glove. Preferably, the certain time is 30 min~60 min.

[0096] S37: The hourly leakage rate of the glove to be tested is calculated by using the following formula:

[0097]

[0098] In the formula:

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

[0100] ΔO1 - the second oxygen concentration change value of the standard glove, expressed in volume parts per million (ppm);

[0101] t - test duration, min;

[0102] T0 - consider the device correction leakage rate (third leakage rate).

[0103] The embodiments of the present application are described above in combination with the drawings, but the present application is not limited to the above specific embodiments, and the above specific embodiments are only illustrative, not limiting, and those skilled in the art can make many forms under the inspiration of the present application without departing from the purpose of the present application and the scope protected by the claims, which all belong to the protection of the present application.

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 member is located at one end of the cavity and is fastened thereto; the glove mounting member 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, the outer side of the annular groove is provided with a sealing ring, and the sealing ring clamp fixes the glove to be tested on the annular groove. The glove to be tested, the protruding portion and the cavity together form a space to be tested; a vacuum pump, the vacuum pump being disposed outside the cavity and connected to the outer surface of the cavity through the connecting hole assembly, for extracting air from the space to be inspected; the connecting hole assembly comprising a first connecting hole and a second connecting hole, the vacuum pump being connected to the first connecting hole and the second connecting hole, respectively, to form a pipeline connected to the cavity; a nitrogen source, the nitrogen source being disposed outside the cavity, connected to the outer surface of the cavity through the connecting hole, and working in conjunction with the vacuum pump to inject nitrogen into the space to be detected to reduce the oxygen content in the space to be detected; an oxygen adsorption circulation system, the oxygen adsorption circulation system being connected to the vacuum pump and the cavity, respectively, and further adsorbing and purifying oxygen inside the cavity on the basis of the coordinated deoxygenation by the vacuum pump and the nitrogen source to provide a hypoxic environment; a third on-off valve being provided on the connecting pipe between the vacuum pump and the first connecting hole, and one end of the oxygen adsorption circulation system being connected to the vacuum pump via the third on-off valve; A differential pressure gauge is provided 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 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.

3. The detection device according to claim 2, 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 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.

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

5. The detection device according to claim 4, 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.

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

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

8. The detection device according to claim 7, characterized in that The connecting hole assembly further 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. The differential pressure gauge and the oxygen analyzer are connected to the cavity through the fifth connecting hole and the sixth connecting hole, respectively.

9. The detection device according to claim 8, characterized in that The glove mounting piece is further provided with a flange portion connected to the protruding portion. 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.

10. The detection device according to claim 9, 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.

11. A method for leak rate detection using the detection device according to claim 10, characterized in that: include: The glove mounting member, the blocking member, and the sealing cover are sealedly 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 switching valve, and the other end is connected to the cavity through the eighth connecting hole on the sealing cover; Mounting a standard glove on the glove mounting member, 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 using the differential pressure gauge and the oxygen analyzer; estimating a first leak rate representing a background leakage condition of the cavity based on the first oxygen concentration change value, and estimating a corrected third leak rate based on the first leak rate; The blocking member is removed, and the oxygen content in 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 using 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 in the cavity is reduced by controlling the vacuum pump and the nitrogen source. The third oxygen concentration change value is detected and calculated using 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 using the glove to be tested, expressed in parts per million (ppm) by volume; ΔO1 - the change in the second oxygen concentration using standard gloves, expressed in parts per million (ppm) by volume; t——test duration, min; T0 - the corrected leak rate taking into account the cavity.

12. The detection method according to claim 11, 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 chamber are respectively provided with two connecting pipes, each of which is provided with a first on-off valve and a second on-off valve. The blocking member is provided with a seventh connecting hole, and the second on-off valve is connected to the seventh connecting hole through the second connecting hole. The second on-off valve is opened while the first on-off valve remains closed to extract air from the space formed by the standard glove, the glove mounting member, and the blocking member. A fourth on-off valve is provided on the connecting pipeline between the nitrogen source and the third connecting hole. When the second on-off valve is closed and the first on-off valve, the third on-off valve and the fourth on-off valve are opened, the vacuum pump extracts the air inside the cavity, and the nitrogen source injects nitrogen into the cavity. Adjusting the third on-off valve so that one end of the oxygen adsorption circulation system is connected to the vacuum pump, and a fifth on-off valve is provided on the pipeline connecting the other end of the oxygen adsorption circulation system to the eighth connecting hole, opening the fifth on-off valve, and allowing the oxygen adsorption circulation system to circulate multiple times to adsorb and purify oxygen in the chamber; The oxygen analyzer is used to observe the oxygen concentration value inside the cavity until it drops to the required oxygen content detection condition.

Images