Container sealing performance detection device and detection method

Abstract

The invention provides a device and a method for detecting the sealing performance of a container, and relates to the fluid sealing performance of a research structure. The vibration source is arranged at the bottom of the detection box, the plurality of fluorescent cameras are arranged on the inner wall of the detection box, the limiting assembly is arranged in the detection box, the detection box is filled with a buffer solution, a detected container is placed on the inner side of the limiting assembly in the detection box, the detected container is filled with a detection agent, and the detection agent is arranged in the detection box. A detection module matched with the detection agent is arranged on the outer wall of the detected container. The sealing performance detection precision is high, and the detection cost is low.

Description

Technical Field

[0001] This invention relates to the study of fluid tightness of structures, and more specifically to a container tightness testing device and testing method. Background Technology

[0002] In the prior art, methods for testing the sealing performance of containers include pressure decay method, water immersion bubble method, and vacuum method. The pressure decay method involves filling the container with compressed gas, maintaining a preset pressure, and then monitoring the pressure change inside the container using a pressure sensor. The water immersion bubble method involves filling the container with compressed gas and then immersing it in water to observe whether bubbles are generated on the outer wall of the container. The vacuum method involves placing the container in a sealed vacuum chamber, evacuating the chamber, and then monitoring the pressure change inside the chamber using a vacuum gauge. The above-mentioned common testing methods can only detect non-micro leaks.

[0003] Currently, compared to the methods mentioned above, helium mass spectrometry leak detection has high accuracy, but its cost is also very high. The investment in vacuum units and mass spectrometers can reach hundreds of thousands of yuan. In addition, helium gas, as a consumable, is also expensive and cannot be reused. The equipment also has periodic calibration costs. There is an urgent need to develop a solution with high accuracy but low cost for leak detection. Summary of the Invention

[0004] The purpose of this invention is to develop a container sealing test device and method with high accuracy and low cost.

[0005] This invention is achieved through the following technical solution: A container sealing performance testing device, comprising: Testing box; The vibration source is located at the bottom of the testing box; Multiple fluorescence cameras are installed on the inner wall of the detection chamber; Limiting components are located inside the detection box; The detection chamber is filled with buffer solution, and the container to be tested is placed inside the limiting component inside the detection chamber. The container to be tested is filled with detection reagent, and the outer wall of the container to be tested is provided with a detection module that works with the detection reagent.

[0006] Optionally, the detection reagent is a fluorescently labeled antigen probe, which is a fluorescein-labeled chicken ovalbumin, and the detection module is a flexible antibody array uniformly coated on the test container. The flexible antibody array includes several films as a substrate. The films are made of polydimethylsiloxane and are seeded with anti-OVA monoclonal antibodies.

[0007] Optionally, the limiting component includes multiple vertically arranged annular silicone strips with equal spacing, multiple vertically arranged elongated silicone strips connecting adjacent silicone strips, and multiple horizontally arranged elongated silicone strips connecting the bottom annular silicone strip.

[0008] Optionally, the detection box is equipped with fluorescence cameras of a fluorescence imager on the bottom, top, and four side walls, and the vibration source includes an ultrasonic transducer located at the bottom of the detection box, which is electrically connected to an ultrasonic generator.

[0009] A method for detecting container sealing performance using a container sealing performance testing device includes the following steps: S1. Clean and dry the container to be inspected to ensure that there are no impurities or oil stains attached to it; S2. Fill the test container with the prepared fluorescently labeled antigen probe as the detection reagent, and attach the flexible antibody array as the detection module to the outer wall of the test container; S3. Measure the density of the container under test. Add NaCl or sucrose to the buffer solution in the test chamber to adjust the buffer solution density so that it is compatible with the container under test. S4. Place the container to be inspected into the inspection box, so that the container to be inspected is in the inner area of ​​the limiting component; S5. The vibration source generates vibrations of different frequencies, causing the buffer solution and the test container to vibrate, simulating the different frequencies of vibration experienced by the test container during transportation. At the same time, the fluorescence camera dynamically tracks and focuses on the flexible antibody array on the surface of the test container to perform fluorescence detection. S6. After completing the test, remove the test container and recover the fluorescently labeled antigen probe and the flexible antibody array on the outer wall that is not bound to the fluorescently labeled antigen probe; S7. Clean the test container with PBS cleaning solution containing polysorbate 20.

[0010] Optionally, in step S2, after the fluorescently labeled antigen probe is filled into the test container, the air inside the test container is emptied, the internal pressure of the test container is greater than the pressure inside the test chamber, and the internal pressure of the test container after the fluorescently labeled antigen probe is filled does not exceed 1 MPa. In step S2, a flexible antibody array is attached to the potential leakage points of the tested container. The potential leakage points include the sealing points, welded points, and movable connection points of the tested container.

[0011] Optionally, in step S5, during fluorescence detection, the detection box is placed in a dark environment to avoid interference from external light during the fluorescence detection process. The AF module of the fluorescence camera dynamically tracks the vibration of the container and finely adjusts the focus.

[0012] Optionally, for images acquired by the fluorescence camera, the AI ​​system performs real-time image registration, removes background interference, and identifies fluorescent bright spots; The construction of the AI system includes data set collection, collecting several labeled images covering all scenarios suitable for the solution, including normal non-leaking samples, samples with various different leakage amounts, interference scenario samples when the inspected container is transparent or blocked by silicone strips, and vibration dynamic samples. Multiple fluorescence cameras collect images at a frequency of 0.1 Hz, and each image is attached with container parameters, vibration parameters, and true leakage amount labels. Then, data annotation is carried out, including leakage point location annotation, leakage amount classification annotation, and interference elimination annotation. Next, AI model training and model iteration are carried out to continuously optimize the generalization ability.

[0013] Optionally, the fluorescently labeled antigen probe can be reused, and the number of reuse times does not exceed 3 times. Detection is required before reuse. The steps are as follows: Drop 1 unit of unused fluorescently labeled antigen probe onto an unused flexible antibody array. The fluorescence intensity detected by a fluorescence imager is the standard intensity. Before reuse, drop 1 unit of the fluorescently labeled antigen probe to be reused onto an unused flexible antibody array, then detect its fluorescence intensity and compare it with the standard intensity. If it reaches 80% of the standard intensity, it is qualified and can be reused; otherwise, it is scrapped. The laser source of the fluorescence camera is the same in the above process.

[0014] Optionally, the flexible antibody array that has not bound to the fluorescently labeled antigen probe can be reused, and the number of reuse times does not exceed 5 times. Detection is required before reuse. The steps are as follows: Drop 1 unit of the standard solution of the fluorescently labeled antigen probe onto an unused flexible antibody array. The fluorescence intensity detected by a fluorescence imager is the standard intensity. Before reuse of the flexible antibody array, drop 1 unit of the standard solution of the fluorescently labeled antigen probe, then detect its fluorescence intensity and compare it with the standard intensity. If it reaches 80% of the standard intensity, it is qualified and can be reused; otherwise, it is scrapped. The laser source of the fluorescence camera is the same in the above process.

[0015] The beneficial effects of the present invention are as follows: The present invention innovatively uses a biological probe-immune sensing array for closed-loop leak detection, replacing traditional physical and chemical signals with specific antigen-antibody binding. The binding constant reaches 10⁻ 9 ~10⁻¹² mol / L, without background cross-reaction. If there is a leakage channel in the inspected container, the probe molecules leak out into the external buffer solution and will be captured by the flexible antibody sensing array at the corresponding position. Antigen-antibody binding occurs, exciting a fluorescence signal. A tiny leak can trigger a detectable signal. The detection accuracy is close to that of helium mass spectrometry leak detection, but the detection cost is greatly reduced. And on the premise of meeting the conditions, the detection consumables can be reused, further reducing the cost. The high precision of helium mass spectrometry leak detection depends on the cooperation of multiple modules. Compared with the helium mass spectrometry leak detection device, the device of the present solution is less sensitive to the environment and does not have bulky supporting equipment, making the device of the present solution mobile and the detection operation relatively flexible. The present solution also has a function of locating the leakage point, while most of the existing leak detection technologies can only qualitatively detect without positioning effect; In existing technologies, container sealing tests are generally static or quasi-static, which cannot simulate the sealing performance of a container when subjected to vibration during transportation. Vibration testing, on the other hand, is more reflective of the actual risks during container transportation than static testing. This solution is closer to real-world scenarios, simulating the vibrations caused by the container during transportation during the sealing test, thus improving the adaptability of the test results to the actual scenario. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the detection device.

[0018] Attached reference numerals: 1. Test chamber; 2. Vibration source; 3. Silicone strip; 4. Flexible rod; 5. Container under test; 6. Fluorescent camera. Detailed Implementation

[0019] In the following description, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments can be modified in various ways without departing from the spirit or scope of the invention. Therefore, the drawings and description are considered to be exemplary in nature and not restrictive.

[0020] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings.

[0021] like Figure 1 As shown, the present invention discloses a container sealing test device, including a test box 1, a vibration source 2 at the bottom of the test box 1, a limiting component inside the test box 1, a container 5 to be tested placed inside the test box 1, a buffer solution filled inside the test box 1, and the limiting component restricts the movement range of the container 5 to prevent it from contacting the inner wall of the test box 1.

[0022] The detection box 1 is equipped with fluorescence cameras 6 on the bottom, top and four side walls of the fluorescence imager. The laser emitter on the fluorescence camera 6 emits 488nm blue laser.

[0023] The vibration source 2 includes an ultrasonic transducer located at the bottom of the test box 1. The ultrasonic transducer is electrically connected to an ultrasonic generator. Different high-frequency oscillation signals emitted by the ultrasonic generator are converted into different high-frequency mechanical oscillations by the ultrasonic transducer and propagated to the buffer solution, causing the buffer solution and the tested container 5 to vibrate, simulating the different frequencies of vibration experienced by the tested container 5 during transportation.

[0024] The limiting component includes a limiting cage with a top opening, consisting of multiple small-diameter and transparent silicone strips 3. Multiple annular silicone strips 3 are arranged vertically at equal intervals. Multiple vertically arranged elongated silicone strips 3 are connected between adjacent silicone strips 3. Multiple horizontally arranged elongated silicone strips 3 are connected to the annular silicone strips 3 at the bottom to seal the bottom of the limiting cage.

[0025] The limiting cage is located in the middle of the detection box 1. Flexible rods 4 are provided at the top and bottom edges of the limiting cage and are connected to the inner wall of the detection box 1. The position of the limiting component is basically fixed by multiple flexible rods 4. At the same time, since the flexible rods 4 are made of flexible material and the limiting component itself is made of silicone, the limiting component can still move flexibly inside the detection box 1 but cannot contact the inner wall of the detection box 1.

[0026] The container 5 being tested is filled with a detection reagent, and the outer wall of the container 5 is equipped with a detection module that works in conjunction with the detection reagent.

[0027] The detection reagent is a fluorescently labeled antigen probe, which is a fluorescein-labeled chicken ovalbumin (OVA-FITCconjugate) at a concentration of 10 μg / mL.

[0028] The detection module is a flexible antibody array uniformly applied to the test container 5. The flexible antibody array includes several films as a substrate. The films are made of polydimethylsiloxane (PDMS). The films are electrostatically adsorbed onto the test container 5. The edges of the films and the test container 5 are sealed with medical silicone. Anti-OVA monoclonal antibodies are seeded on the films at a density of 1 μg / cm².

[0029] The buffer solution in test chamber 1 is PBS buffer solution. NaCl or sucrose is added to the buffer solution to adjust the buffer solution density so that it matches the test container 5, so that the test container 5 is suspended in the middle after being placed in the buffer solution.

[0030] The excitation spectrum peak of FITC is concentrated in the range of 490~496nm (blue light band), but it still has a strong excitation efficiency at 488nm, about 90% of the peak value. This is because 488nm is a commonly used output wavelength of argon ion lasers and is a standard excitation source for industrial-grade fluorescence imagers. The equipment is mature and the cost is controllable. Choosing 488nm is the optimal balance between equipment adaptability and excitation efficiency. The emission spectrum peak of FITC is 520~525nm green fluorescence (green light band).

[0031] The testing method of the above-mentioned container sealing testing device includes the following steps: S1. Clean and dry the container to be inspected to ensure that there are no impurities or oil stains attached to it; S2. Fill the prepared fluorescently labeled antigen probe into the test container and attach the flexible antibody array to the outer wall of the test container; S3. Measure the density of the container under test. Add NaCl or sucrose to the buffer solution in the test chamber to adjust the buffer solution density so that it is compatible with the container under test. S4. Place the container to be inspected into the inspection chamber, so that the container to be inspected is in the inner area of ​​the limiting cage; S5. The vibration source generates vibrations of different frequencies, causing the buffer solution and the test container to vibrate, simulating the different frequencies of vibration experienced by the test container during transportation. At the same time, the fluorescence camera dynamically tracks and focuses on the flexible antibody array on the surface of the test container to perform fluorescence detection. S6. After completing the test, remove the test container and recover the fluorescently labeled antigen probe and the flexible antibody array on the outer wall that is not bound to the fluorescently labeled antigen probe; S7. Clean the test container with PBS cleaning solution containing polysorbate 20; In step S2, after the fluorescently labeled antigen probe is filled into the test container, the air inside the test container is emptied. The internal pressure of the test container is greater than the pressure inside the test chamber. After the fluorescently labeled antigen probe is filled, the internal pressure of the test container does not exceed 1 MPa. In step S2, ensure that a flexible antibody array is attached to the potential leakage points of the tested container. Potential leakage points include the sealing points, welded points, and movable connection points of the tested container. In step S5, during fluorescence detection, the detection box is placed in a dark environment to avoid interference from external light during the fluorescence detection process. The AF module of the fluorescence camera dynamically tracks the vibration of the container and finely adjusts the focus. For images acquired by the fluorescence camera, the AI ​​system performs real-time image registration, removes background interference, and identifies fluorescent bright spots. The construction of the AI ​​system includes dataset acquisition, which involves acquiring several labeled images covering all scenarios for solution adaptation to avoid model overfitting. These images include normal samples without omissions, samples with various leakage amounts, interference scenario samples when the tested container is transparent and when it is covered by silicone strips, and vibration dynamic samples. Six fluorescence cameras acquire images at a frequency of 0.1Hz. Each image is accompanied by container parameters (material, shape, etc.), vibration parameters, and a true value label for leakage amount. Then, data annotation is performed, including leak point location annotation, leakage amount classification annotation (leakage level), and interference elimination annotation. Finally, the AI ​​model is trained and iterated to continuously optimize generalization. In step S5, if there is a leakage channel in the container being tested, the fluorescently labeled antigen probe molecules will leak into the external buffer solution and be captured by the flexible antibody sensing array at the corresponding position. The antigen and antibody will bind, excite the fluorescence signal, and even a tiny leak can trigger a detectable signal. The fluorescently labeled antigen probe can be reused, and the number of reuse times does not exceed 3 times. Before reuse, it needs to be detected. The steps are as follows: Drop 1 unit of unused fluorescently labeled antigen probe onto the unused flexible antibody array. The fluorescence intensity detected by the fluorescence imager is the standard intensity. Before reuse, drop 1 unit of the fluorescently labeled antigen probe to be reused onto the unused flexible antibody array, then detect its fluorescence intensity and compare it with the standard intensity. If it reaches 80% of the standard intensity, it is qualified and can be reused; otherwise, it will be scrapped. The laser source of the fluorescence camera is the same in the above process; The flexible antibody array not bound to the fluorescently labeled antigen probe can be reused, and the number of reuse times does not exceed 5 times. Before reuse, it needs to be detected. The steps are as follows: Drop 1 unit of OVA-FITC standard solution (with a determined concentration) onto the unused flexible antibody array. The fluorescence intensity detected by the fluorescence imager is the standard intensity. Before the flexible antibody array is reused, drop 1 unit of OVA-FITC standard solution, then detect its fluorescence intensity and compare it with the standard intensity. If it reaches 80% of the standard intensity, it is qualified and can be reused; otherwise, it will be scrapped. The laser source of the fluorescence camera is the same in the above process.

[0032] The above embodiments are only preferred embodiments of the present invention and do not limit the technical solutions of the present invention. Any technical solution that can be achieved based on the above embodiments without creative labor shall be regarded as falling within the scope of the patent right protection of the present invention.

Claims

1. A container tightness detection device characterized by comprising: Include: Detection box; Vibration source, set in the bottom of the detection box; A plurality of fluorescence cameras, set in the inner wall of the detection box; Limiting component, set in the detection box; Wherein, the detection box is filled with buffer solution, the limiting component inside the detection box is placed in the container to be detected, the container to be detected is filled with detection agent, and the outer wall of the container to be detected is provided with a detection module matched with the detection agent.

2. The container tightness detecting apparatus according to claim 1, wherein The detection agent is a fluorescently labeled antigen probe, which is a fluorescein-labeled chicken egg albumin, and the detection module is a flexible antibody array uniformly pasted on the container to be detected, the flexible antibody array includes a plurality of films as substrates, the films are made of polydimethylsiloxane, and the films are seeded with anti-OVA monoclonal antibodies.

3. The container tightness detecting apparatus according to claim 1, wherein The limiting component includes a plurality of annular silica gel strips arranged vertically at equal intervals, a plurality of long strip-shaped silica gel strips arranged vertically are connected between adjacent silica gel strips, and a plurality of long strip-shaped silica gel strips arranged horizontally are connected on the annular silica gel strip at the bottom.

4. The container tightness detecting apparatus according to claim 1, wherein The bottom, top and four side walls of the detection box are provided with fluorescence cameras of a fluorescence imager, and the vibration source includes an ultrasonic transducer arranged at the bottom of the detection box, which is electrically connected with an ultrasonic generator.

5. A method of detecting a container according to any one of claims 1 to 4, wherein Including the following steps: S1. The container to be detected is washed and dried to ensure that the container to be detected is free of impurities and oil stains; S2. Fill the prepared fluorescently labeled antigen probe as the detection agent into the container to be detected, and paste the flexible antibody array as the detection module on the outer wall of the container to be detected; S3. Measure the density of the container to be detected, and adjust the density of the buffer solution in the detection box by adding NaCl or sucrose to match the container to be detected; S4. Put the container to be detected into the detection box, so that the container to be detected is in the inside area of the limiting component; S5. The vibration source generates vibrations of different frequencies to make the buffer solution and the container to be detected vibrate, simulate the different frequency vibrations suffered by the container to be detected during transportation, and at the same time, the fluorescence cameras dynamically track and focus on the flexible antibody array on the surface of the container to be detected for fluorescence detection; S6. After the detection is completed, the container to be detected is taken out and the fluorescently labeled antigen probe and the flexible antibody array not combined with the fluorescently labeled antigen probe on the outer wall are recovered; S7. The container to be detected is cleaned with PBS cleaning solution containing polysorbate 20.

6. The method of detecting a container according to claim 5, wherein In the step S2, after the fluorescently labeled antigen probe is filled into the container to be detected, the air in the container to be detected is exhausted, the internal pressure of the container to be detected is greater than the internal pressure of the detection box, and the internal pressure of the container to be detected after the fluorescently labeled antigen probe is filled is not more than 1MPa; In the step S2, ensure that the potential leakage of the container to be detected is pasted with the flexible antibody array, and the potential leakage includes the sealing place, the welding place and the movable connection place of the container to be detected.

7. The method of detecting a container according to claim 5, wherein In the step S5, during the fluorescence detection, the detection box is placed in a light-free environment to avoid interference of external light during the fluorescence detection process, and the AF module of the fluorescence camera dynamically tracks the vibration of the container to adjust the focal length.

8. The method of claim 5, wherein For the images collected by the fluorescence camera, the AI system performs image registration, background interference subtraction and recognition of fluorescent bright spots in real time. The building of the AI system includes data set collection, collecting a plurality of labeled images, covering all scenarios adapted by the scheme, including normal no-leak samples, a plurality of different leakage amount samples, interference scene samples when the detected container is transparent and the silica gel strip is blocked, vibration dynamic samples, a plurality of fluorescence cameras collect at a frequency of 0.1 Hz, each image is attached with container parameters, vibration parameters, and leakage amount true value label, then data labeling is performed, including leak point positioning labeling, leakage amount classification labeling, and interference exclusion labeling, and then AI model training, model iteration and continuous optimization of generalization are performed.

9. The method of claim 5, wherein The fluorescently labeled antigen probe can be reused no more than 3 times, and before reuse, it needs to be detected, the steps are: adding 1 unit of unused fluorescently labeled antigen probe to the unused flexible antibody array, the fluorescence intensity detected by the fluorescence imager is the standard intensity, before reuse, 1 unit of the fluorescently labeled antigen probe to be reused is added to the unused flexible antibody array, and the fluorescence intensity is detected and compared with the standard intensity, and if it reaches 80% of the standard intensity, it is qualified for reuse, otherwise it is scrapped, and the laser source of the fluorescence camera in the above process is the same.

10. The method of claim 5, wherein The flexible antibody array not combined with the fluorescently labeled antigen probe can be reused no more than 5 times, and before reuse, it needs to be detected, the steps are: adding 1 unit of fluorescently labeled antigen probe standard solution to the unused flexible antibody array, the fluorescence intensity detected by the fluorescence imager is the standard intensity, before reuse of the flexible antibody array, 1 unit of fluorescently labeled antigen probe standard solution is added, and the fluorescence intensity is detected and compared with the standard intensity, and if it reaches 80% of the standard intensity, it is qualified for reuse, otherwise it is scrapped, and the laser source of the fluorescence camera in the above process is the same.

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