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CN111141246A - Medicine bottle micropore testing device and method based on vacuum leak rate measurement principle - Google Patents

Medicine bottle micropore testing device and method based on vacuum leak rate measurement principle Download PDF

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Publication number
CN111141246A
CN111141246A CN201911363988.7A CN201911363988A CN111141246A CN 111141246 A CN111141246 A CN 111141246A CN 201911363988 A CN201911363988 A CN 201911363988A CN 111141246 A CN111141246 A CN 111141246A
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China
Prior art keywords
chamber
medicine bottle
vacuum
micropore
vacuum chamber
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Chinese (zh)
Inventor
冯天佑
陈联
成永军
习振华
李亚丽
孙冬花
丁栋
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Lanzhou Institute of Physics of Chinese Academy of Space Technology
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Lanzhou Institute of Physics of Chinese Academy of Space Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B21/00Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
    • G01B21/10Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring diameters
    • G01B21/14Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring diameters internal diameters
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L9/00Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
    • G01L9/12Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in capacitance, i.e. electric circuits therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01MTESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00Investigating fluid-tightness of structures
    • G01M3/02Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/26Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
    • G01M3/32Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators
    • G01M3/3236Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers
    • G01M3/3263Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers using a differential pressure detector

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Examining Or Testing Airtightness (AREA)

Abstract

The invention discloses a medicine bottle micropore testing device and method based on a vacuum leak rate measuring principle. The invention can obtain the geometric dimension and diameter of the irregular micron-sized small hole and has high test precision. The equivalent diameter of the micropore is calculated by measuring the vacuum leakage rate of the micropore, so that the difficulty of directly measuring the geometric dimension of the irregular micron-sized micropore is avoided; the effective volume of the vacuum chamber is adjusted through supports with different sizes, so that the proper volume of the vacuum chamber can be selected for micropores with different magnitudes, and the testing precision is improved; the pressure is measured by the capacitance film gauge, and a pressure change value with high precision can be obtained. The invention can test and obtain the equivalent diameter of the micropore of the medicine bottle and can also be used for testing the micropore and the crack of a similar container.

Description

Medicine bottle micropore testing device and method based on vacuum leak rate measurement principle
Technical Field
The invention relates to the technical field of micropore and fracture diameter measurement, in particular to a medicine bottle micropore testing device and method based on a vacuum leak rate measurement principle.
Background
The medicine bottle for containing the medicine is widely applied to the medicine industry, and the medicine in the medicine bottle can be protected from the outside, so that the efficacy is kept. When holes or crevices exist in the vial, bacteria may enter the vial through them, contaminating the drug. Researchers obtain micropores with different specifications on the medicine bottle through a laser drilling method and are used for researching the relation between the size of the micropore and the invasion of bacteria. However, since the edges of the micro-holes obtained by laser drilling are irregular and have micron-scale dimensions, it is difficult to obtain appropriate results by directly measuring the geometric dimensions of the micro-holes by using conventional electric, pneumatic and optical methods. The method is limited by the existing irregular micropore size measurement means, and other methods are considered to avoid the problem.
Disclosure of Invention
In view of the above, the invention provides a medicine bottle micropore testing device and method based on a vacuum leak rate measurement principle, which can obtain the geometric dimension diameter of an irregular micron-sized pore and have high testing precision.
The invention relates to a medicine bottle micropore testing device based on a vacuum leak rate measurement principle, which comprises an air source, a valve I, a valve II, a valve III, a pressurizing chamber, a capacitance film gauge I, a capacitance film gauge II, a sealing ring, a vacuum chamber and a mechanical pump, wherein the air source is connected with the valve I;
the gas source is connected with the pressurizing chamber through a valve I and is used for filling gas with required pressure into the pressurizing chamber; the mechanical pump is connected with the pressurizing chamber through a valve II and is connected with the vacuum chamber through a valve III, and the mechanical pump is used for realizing the evacuation of the pressurizing chamber and the vacuum chamber;
the bottle mouth of the tested medicine bottle is positioned in the pressurizing chamber, the micropores are positioned in the vacuum chamber, and the connecting parts of the tested medicine bottle, the pressurizing chamber and the vacuum chamber are sealed and fixed through sealing rings;
the capacitance film gauge I is arranged on the pressure charging chamber and is used for realizing pressure measurement of the pressure charging chamber; and the capacitance film gauge II is arranged on the vacuum chamber and used for realizing the pressure measurement of the vacuum chamber.
Preferably, a support is arranged in the vacuum chamber and is used for supporting the tested medicine bottle and adjusting the volume of the vacuum chamber.
Preferably, the support is made of an aluminum alloy material.
Preferably, the pressurizing chamber and the vacuum chamber are cylindrical structures, are made of stainless steel materials and are designed according to the requirement of obtaining extremely high vacuum, and the background leakage and deflation rate is not more than 1 multiplied by 10-8Pa·m3/s。
The invention also provides a medicine bottle micropore testing method based on the vacuum leak rate measuring principle, the testing device is adopted for testing, and the method comprises the following steps:
step 1, a tested medicine bottle is placed into a vacuum chamber and a pressurizing chamber and is sealed and fixed by a sealing ring, a micropore of the tested medicine bottle is positioned in the vacuum chamber, and a bottle mouth is positioned in the pressurizing chamber;
step 2, vacuumizing the vacuum chamber and the pressurizing chamber, stopping vacuumizing the pressurizing chamber when the pressure of the pressurizing chamber is less than 10Pa, and opening a gas source to charge gas with required pressure into the pressurizing chamber;
step 3, stopping inflating when the pressure of the pressurizing chamber reaches the required pressure, stopping evacuating the vacuum chamber, and recording the pressure change of the vacuum chamber in the testing time;
step 4, calculating to obtain the vacuum leakage rate QL of the micropores of the medicine bottle according to the pressure change of the vacuum chamber in the test time, and further obtaining the conductance U of the micropores;
and 5, calculating the diameters of the round holes corresponding to the flow guide U in the two states according to the viscous flow state and the molecular flow state respectively, wherein the diameter of the micropore of the medicine bottle is between the diameters of the two round holes.
Has the advantages that:
the equivalent diameter of the micropore is calculated by measuring the vacuum leakage rate of the micropore, so that the difficulty of directly measuring the geometric dimension of the irregular micron-sized micropore is avoided; although the invention can not obtain accurate diameter value, it can obtain more accurate numerical range, which is very close to the true value, and the measuring precision is much higher than the prior art.
The effective volume of the vacuum chamber is adjusted through supports with different sizes, so that the proper volume of the vacuum chamber can be selected for micropores with different magnitudes, and the testing precision is improved; the pressure is measured by the capacitance film gauge, and a pressure change value with high precision can be obtained.
The invention can test and obtain the equivalent diameter of the micropore of the medicine bottle and can also be used for testing the micropore and the crack of a similar container.
Drawings
FIG. 1 is a schematic structural diagram of a testing apparatus according to the present invention.
Wherein, 1-gas source; 2-valve I; 3-valve II; 4-a plenum chamber; 5-capacitance film gauge I; 6-tested medicine bottle; 7-a sealing ring; 8-micropores; 9-supporting; 10-a vacuum chamber; 11-capacitance film gauge II; 12-valve III; 13-mechanical pump.
Detailed Description
The invention is described in detail below by way of example with reference to the accompanying drawings.
The invention provides a medicine bottle micropore testing device based on a vacuum leak rate measuring principle, which comprises an air source 1, a valve I2, a valve II 3, a valve III 12, a pressurizing chamber 4, a capacitance film gauge I5, a capacitance film gauge II11, a tested medicine bottle 6, a sealing ring 7, a support 9, a vacuum chamber 10, a mechanical pump 13 and corresponding pipelines as shown in figure 1.
The gas source 1 is connected with the pressurizing chamber 4 through a valve I2 and is used for filling gas with required pressure into the pressurizing chamber 4; the mechanical pump 13 is connected with the pressurizing chamber 4 through a valve II 3 and is used for realizing the evacuation of the pressurizing chamber 4; the pressurizing chamber 4 is used for placing an opening part (namely a bottle mouth) of the tested medicine bottle 6 and providing inlet pressure for vacuum leak rate measurement of the micropore 8 on the tested medicine bottle; the capacitance film gauge I5 is arranged on the pressure chamber 4 and is used for realizing pressure measurement of the pressure chamber 4; the tested medicine bottle 6 is a tested object and is placed on a support 9 in the vacuum chamber, the opening part (namely, a bottle mouth) of the tested medicine bottle is positioned in a pressurizing chamber 4, the part where the micropore 8 is positioned in a vacuum chamber 10, and the connecting part of the tested medicine bottle, the pressurizing chamber and the vacuum chamber is sealed, fixed and isolated through a sealing ring 7, namely, the tested medicine bottle is communicated with the vacuum chamber only through the micropore, and the pressurizing chamber is also communicated with the vacuum chamber only through the micropore on the tested medicine bottle; the support 9 is arranged at the bottom of the vacuum chamber and is used for supporting the tested medicine bottle 8 and preventing the medicine bottle from being pressed to move and even colliding with the wall of the vacuum chamber to cause damage; the vacuum chamber 10 provides an outlet vacuum environment for the vacuum leak rate measurement of the micropores 8, and the capacitance film gauge II11 is installed on the vacuum chamber 10 and used for realizing the pressure measurement of the vacuum chamber; the mechanical pump 13 is connected with the vacuum chamber 10 through a valve III 12 and is used for realizing the vacuum pumping of the vacuum chamber; a mechanical pump 13 is used to effect evacuation of the plenum chamber 4 and the vacuum chamber 10.
Wherein the pressurizing chamber 4 and the vacuum chamber 10 are cylindrical structures, are made of stainless steel materials, and are designed according to the requirements of extremely high vacuum, and the background leakage and deflation rate is not more than 1 × 10-8Pa·m3The volume of the vacuum chamber 10 is about 1L/s. The support 9 is made of aluminum alloy materials, the upper part and the lower part of the support are flat, and the support is guaranteed to be stably contacted with the vacuum chamber 10 and the bottom surface of the tested medicine bottle 6. The support comprises a series of alloy blocks with different heights and sectional areas, the corresponding alloy blocks are selected according to the size of the tested medicine bottle and the equivalent diameter of the micropore, the effective volume of the vacuum chamber is adjusted, and the tested medicine bottle is supported, so that the pressure change of the vacuum chamber in the measuring range of the capacitance film gauge 11 in the testing process is enabled to be less than 5% and the pressure difference change quantity at two ends of the micropore is enabled to be less than 5%.
The diameter of the tested medicine bottle 6 is generally between 10mm and 32mm, the length is between 18mm and 126mm, and the equivalent diameter of the micropores on the medicine bottle is between 0.1 mu m and 20 mu m.
The measuring method adopting the measuring device comprises the following steps:
step 1, selecting a proper size to support according to the micropores of a tested medicine bottle, and placing the medicine bottle at the bottom of a vacuum chamber;
step 2, putting the tested medicine bottle into a vacuum chamber and a pressurizing chamber, fixedly isolating the tested medicine bottle by using a sealing ring, and contacting the bottom of the tested medicine bottle with a support to ensure that the micropore of the medicine bottle is positioned in the vacuum chamber and the open part of the medicine bottle is positioned in the pressurizing chamber;
step 3, vacuumizing the vacuum chamber and the pressurizing chamber, stopping vacuumizing the pressurizing chamber when the pressure of the pressurizing chamber is less than 10Pa, and filling gas with required pressure (generally, the storage environment pressure of the medicine bottle or the pressure required by the research on the medicine bottle);
step 4, when the pressure of the pressurizing chamber is the pressure of the storage environment of the medicine bottle, stopping inflating, stopping evacuating the vacuum chamber, and recording the pressure change of the vacuum chamber in the testing time;
step 5, calculating the vacuum leakage rate Q of the micropores of the medicine bottle according to the pressure change of the vacuum chamber in the test timeLThen, the conductance of the micropores (taking test gas air as an example) is calculated according to the formula (1):
Figure BDA0002337928680000051
in the formula, U is the conductance of the micropore to air under the test condition, and the unit is m3/s;pinPressurizing the lateral pressure (i.e. plenum pressure), p, of the microporesoutThe pressure at the vacuum side of the micropore (i.e. the pressure in the vacuum chamber) is expressed in Pa. Wherein p isoutTaking the maximum value or the average value of the vacuum chamber in the measurement process.
Because the cross-sectional area of the micropores of the medicine bottle is far smaller than the area of the wall of the medicine bottle, the conductance of gas passing through the circular holes can be calculated according to the circular hole model. In the vacuum technique, the flow state of the gas is different, the calculation model of the circular hole conductance is also different, and the flow state of the gas is different from the average pressure of the gas in the circular hole
Figure BDA0002337928680000056
Related to the product of the aperture d:
Figure BDA0002337928680000053
is viscous flow
Figure BDA0002337928680000054
As a molecular stream
Figure BDA0002337928680000055
Is viscous flow-molecular flow
Therefore, the diameter of the round hole corresponding to the viscous flow state and the molecular flow state is respectively calculated according to the viscous flow state and the molecular flow state, and the diameter of the micropore of the medicine bottle is between the two diameters of the round hole.
Step 6, calculating the corresponding diameter of the circular hole according to a viscous flow state circular hole flow conductance calculation formula (formula 2) and a molecular flow state circular hole flow conductance calculation formula (formula 3); the diameter of the vial's micropores is between the two circular hole diameters.
Figure BDA0002337928680000052
Uo.f.20℃=91.2d2(3)
In the formula of Un.20℃Is the conductance of micropores to air of 20 ℃ in a viscous flow state, and the unit is m3S; d is the diameter of the micropores in m; u shapeo.f.20℃Is the conductance of micropores to air at 20 ℃ in the molecular flow state, and the unit is m3/s。
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A medicine bottle micropore testing device based on a vacuum leak rate measurement principle is characterized by comprising an air source (1), a valve I (2), a valve II (3), a valve III (12), a pressurizing chamber (4), a capacitance film gauge I (5), a capacitance film gauge II (11), a sealing ring (7), a vacuum chamber (10) and a mechanical pump (13);
the gas source (1) is connected with the pressurizing chamber (4) through a valve I (2) and is used for filling gas with required pressure into the pressurizing chamber (4); the mechanical pump (13) is connected with the pressure chamber (4) through a valve II (3) and is connected with the vacuum chamber (10) through a valve III (12) and is used for realizing the evacuation of the pressure chamber (4) and the vacuum chamber (10);
the bottleneck of the tested medicine bottle (6) is positioned in the pressurizing chamber (4), the micropore (8) is positioned in the vacuum chamber (10), and the connecting part of the tested medicine bottle (6), the pressurizing chamber (4) and the vacuum chamber (10) is sealed and fixed through a sealing ring (7);
the capacitance film gauge I (5) is arranged on the pressure charging chamber (4) and is used for realizing pressure measurement of the pressure charging chamber (4); the capacitance film gauge II (11) is arranged on the vacuum chamber (10) and is used for realizing the pressure measurement of the vacuum chamber.
2. The medicine bottle micropore testing device based on the vacuum leak rate measurement principle as claimed in claim 1, wherein a support (9) is further provided in the vacuum chamber (10), said support (9) is used for supporting the tested medicine bottle (6) and adjusting the volume of the vacuum chamber (10).
3. The medicine bottle micropore testing device based on the vacuum leak rate measuring principle as claimed in claim 2, wherein the support (9) is made of an aluminum alloy material.
4. The apparatus for testing the micro-holes of medicine bottles based on the vacuum leak rate measuring principle as claimed in claim 1, wherein the pressurizing chamber (4) and the vacuum chamber (10) are made of cylindrical structures, stainless steel materials are selected, the apparatus is designed according to the requirements of obtaining extremely high vacuum, and the background leak gas release rate is not more than 1 x 10-8Pa·m3/s。
5. A method for testing the micropores of a medicine bottle based on the vacuum leak rate measurement principle is characterized in that the testing device according to any one of claims 1 to 4 is used for testing, and comprises the following steps:
step 1, a tested medicine bottle is placed into a vacuum chamber and a pressurizing chamber and is sealed and fixed by a sealing ring, a micropore of the tested medicine bottle is positioned in the vacuum chamber, and a bottle mouth is positioned in the pressurizing chamber;
step 2, vacuumizing the vacuum chamber and the pressurizing chamber, stopping vacuumizing the pressurizing chamber when the pressure of the pressurizing chamber is less than 10Pa, and opening a gas source to charge gas with required pressure into the pressurizing chamber;
step 3, stopping inflating when the pressure of the pressurizing chamber reaches the required pressure, stopping evacuating the vacuum chamber, and recording the pressure change of the vacuum chamber in the testing time;
step 4, calculating the vacuum leakage rate Q of the micropores of the medicine bottle according to the pressure change of the vacuum chamber in the test timeLFurther obtaining the flow conductance U of the micropore;
and 5, calculating the diameters of the round holes corresponding to the flow guide U in the two states according to the viscous flow state and the molecular flow state respectively, wherein the diameter of the micropore of the medicine bottle is between the diameters of the two round holes.
CN201911363988.7A 2019-12-26 2019-12-26 Medicine bottle micropore testing device and method based on vacuum leak rate measurement principle Pending CN111141246A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113532770A (en) * 2021-07-26 2021-10-22 重庆工商大学 Device and method for measuring micropore leakage amount of injection glass container

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CN102426079A (en) * 2011-10-28 2012-04-25 清华大学 Simulation system and method for leakage detection of space station by adopting direction gauge
US20130298643A1 (en) * 2012-05-10 2013-11-14 Mahle Powertrain, Llc Evaporative emissions leak tester and leak test method
CN205826240U (en) * 2016-06-24 2016-12-21 中国科学院光电研究院 A kind of vacuum seal dividing potential drop leakage rate measurement device

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Publication number Priority date Publication date Assignee Title
CN113532770A (en) * 2021-07-26 2021-10-22 重庆工商大学 Device and method for measuring micropore leakage amount of injection glass container

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Application publication date: 20200512