Positive sample micro-well metering method and application thereof

Abstract

The application relates to the G01N field, in particular to a positive sample micropore metering method and application thereof. The steps of the positive sample micropore metering method at least include the following steps: (1) determining the position of the positive sample micropore under a normal field of view by using a microscope; (2) projecting a light path to irradiate the micropore position by a probe light head, and determining the channel condition; (3) determining the sample thickness by using a thickness gauge, selecting a proper light path, adjusting the lens focal point distance to be consistent with the thickness of the positive sample to-be-measured area, and finally performing 3D scanning reconstruction by using an ultra-depth-of-field 3D digital microscope. The metering method in the application can effectively measure the aperture of the soft packaging material without negative influence, and clearly restore the overall appearance of the micropore.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of G01N, in particular to a positive sample micropore metering method and application thereof. BACKGROUND

[0002] Droppers and capillaries are usually used for the preparation of positive samples of soft packaging materials. The pore diameter of a glass microdropper for preparing a positive sample can be as low as 0.1 μm, but the tip is very fragile and can be easily damaged during sample preparation. After the preparation is completed, the sealing integrity needs to be observed under an optical microscope after the dropper is sealed with epoxy resin. In addition, the residual air in the dropper will interfere with the test results, which will have a greater impact on the invasion of microorganisms and may produce false negative results.

[0003] In the field of sealing test of packaging materials, laser micropore processing technology has become the mainstream technical means in recent years. Its advantage lies in that the leak hole of the positive bottle prepared by laser technology has a geometric shape and irregular airflow channel close to the real defect. However, an accurate and effective metering method is needed to characterize the size of the pore diameter. The commonly used gas flow metering method cannot adapt to the pore diameter test of samples of all materials. For example, PVC soft bag, PP plastic infusion bottle, TPE composite film soft bag, polyethylene material medical single-dose eye drop bottle and other such positive samples, because they are completely sealed or have multiple interfaces, they cannot be directly metered and calibrated by gas flow. At the same time, when the gas flow is metered, the pressure changes, which will cause damage to the positive pore diameter of the above-mentioned materials. The action of pressure increases the pore diameter. At the same time, the conventional optical microscope cannot directly observe the bottom of the pore channel due to the depth of field. The prior art (CN02137742.1) provides a micropore automatic measurement method, which mainly uses a CCD camera to take a magnified image of the micropore, and then inputs the content into a computer, and then calculates the maximum value, minimum value and average value of the pore diameter of the micropore by area method and boundary point coordinate method. However, as described above, due to the depth of field, the bottom of the micropore cannot be directly observed, and the pore size at the bottom is of great significance to the air tightness test.

[0004] Therefore, there is an urgent need for a positive sample micropore metering method with high micropore diameter measurement accuracy, without causing soft material expansion, and capable of effectively dealing with various pore environments. SUMMARY

[0005] In order to solve the above problems, the present application provides a positive sample micropore metering method, steps at least include the following steps: (1) under normal vision, the position of the positive sample micropore is determined by using a microscope; (2) the micropore position is irradiated by a light path projected by an exploratory light head, and the channel condition is determined; (3) the sample thickness is determined by a thickness gauge, the appropriate light path is selected, the lens focal point distance is adjusted to be consistent with the thickness of the positive sample to-be-measured region, and finally 3D scanning reconstruction is performed by an ultra-depth-of-field 3D digital microscope.

[0006] As a preferred scheme, the positive sample is a CCIT positive sample.

[0007] As a preferred scheme, the positive sample is any one of a PVC soft bag, a PP plastic infusion bottle, a TPE composite film soft bag and a polyethylene material medical single-dose eye drop bottle.

[0008] In the present application, the measurement method of the positive sample has excellent micropore measurement accuracy for soft packaging materials such as PVC soft bags. The present applicant believes that in the measurement method in the present application, the inside of the aperture can be preliminarily judged by light irradiation, and then the micropore can be subjected to ultra-depth-of-field 3D scanning reduction by an appropriate light irradiation method, during which the micropore aperture of the packaging material can be basically contacted, so that the micropore deformation phenomenon caused by excessive pressure during the measurement of the gas flow is avoided.

[0009] As a preferred scheme, the exploratory light head structure mainly includes a main probe 1 and two side probes 2 fixedly connected on the two sides.

[0010] As a preferred scheme, the light irradiation of the main probe 1 is in the shape of a vertical downward inverted trapezoid, and the light irradiation of the side probe 2 is in the shape of an oblique line with an included angle of 20-80° with the horizontal line.

[0011] As a preferred scheme, the magnification of the microscope in step (1) is 1000-2000 times.

[0012] As a preferred scheme, the magnification of the microscope in step (1) is 1200-1800 times.

[0013] As a preferred scheme, the light path is any one of coaxial light, coaxial side light, ring light, ring side light, mixed light and full light; the specific schemes of the corresponding various light paths are shown in the accompanying drawings. Figures 1-3

[0014] ​In the present application, the 3D scanning comprehensiveness is effectively improved by the multiple light path irradiation modes designed by the setting of the probe head, and the appearance of pores in the irradiation process is avoided, so that the overall micro-hole 3D morphology can be completely restored. The applicant believes that: when the irradiation light of the main probe 1 is in a vertical downward inverted trapezoidal shape; the irradiation light of the side probe 2 is in a slanted line type, and the included angle with the horizontal line is 20-80°, the rotation of the light source of the side probe can further adjust the overall illumination area of the irradiation top end, and the light intensity of the required part can be formed by the rotation of the side light, thereby effectively performing aperture measurement.

[0015] As a preferred scheme, the specific operation method for determining the thickness of the sample in step (3) by the thickness gauge is: coupling agent is coated on the area to be measured, the thickness gauge probe is tightly attached to the area coated with ultrasonic coupling agent, the thickness of the positive sample at the place is measured by ultrasonic wave transmission and is calibrated.

[0016] As a preferred scheme, the scanning time for 3D scanning reconstruction by the ultra-depth-of-field 3D digital microscope in step (3) is 1-6 minutes.

[0017] As a preferred scheme, the scanning time for 3D scanning reconstruction by the ultra-depth-of-field 3D digital microscope in step (3) is 2-4 minutes.

[0018] As a preferred scheme, the model of the ultra-depth-of-field 3D digital microscope is VHX-970F, which is purchased from Keyence Corporation.

[0019] As a preferred scheme, the model of the thickness gauge is UM-2D, the test accuracy is ±10 microns, and it is purchased from Shenzhen Zhuo Yue Instrument and Meter Co., Ltd.

[0020] As a preferred scheme, the coupling agent is purchased from Jining High-tech Zone Jinuote Medical Gel Factory, and the product name is medical ultrasonic coupling agent.

[0021] As a preferred scheme, the pore condition is any one of smooth pores, rough pores and super-deep pores.

[0022] As a preferred scheme, the smooth pore is a micro-hole with a pore depth of 200-1000 microns, and the pore wall in the micro-hole has no obvious protrusion, and the pore surface is smooth.

[0023] As a preferred scheme, the rough pore is a micro-hole with a pore depth of 200-1000 microns, and the pore wall in the micro-hole has obvious protrusion, and the pore surface is uneven.

[0024] As a preferred scheme, the super-deep pore is a positive sample micro-hole with a pore depth greater than 1000 microns.

[0025] As a preferred scheme, when the hole condition is a smooth hole, coaxial light or coaxial side light is used as the main light source of the light probe, and then 3D scanning is performed on the smooth hole.

[0026] As a preferred scheme, when the hole condition is a rough hole, ring light or ring side light is used as the main light source of the light probe, and then 3D scanning is performed on the rough hole.

[0027] As a preferred scheme, when the hole condition is an ultra-deep hole, full light or mixed light is used as the main light source of the light probe, and then 3D scanning is performed on the ultra-deep hole.

[0028] In the present application, different illumination methods are used for different hole conditions, which effectively improves the test efficiency of micro-hole measurement and can cope with micro-hole conditions of various materials and various conditions. The applicant believes that the use of multiple illumination methods can effectively avoid incomplete scanning caused by rough holes and deep holes.

[0029] The second aspect of the present application provides an application of the above-mentioned positive sample micro-hole measurement method, including the application of the method in a packaging material air tightness detection method.

[0030] Advantages:

[0031] 1. The positive sample micro-hole measurement method provided in the present application can effectively overcome the difficulty in measuring the micro-hole of the packaging material made of PVC soft bag, PP plastic bag and other materials when using the gas flow method, and can reduce the influence of the measurement process on the accuracy caused by the increase in the micro-hole diameter due to pressure.

[0032] 2. The positive sample micro-hole measurement method provided in the present application can effectively ensure that the micro-hole of each positive sample can be measured without causing pollution and damage to the micro-hole of the positive sample, thereby further enhancing the accuracy of the measurement.

[0033] 3. The positive sample micro-hole measurement method provided in the present application can use multiple light paths to perform 3D reconstruction on multiple complex holes of the positive sample, thereby truly restoring the morphology of the hole without causing any influence, and further ensuring the true size of each hole diameter. BRIEF DESCRIPTION OF DRAWINGS

[0034] Figure 1 It is a schematic diagram of the illumination of the coaxial light and the coaxial side light in the present application.

[0035] Figure 2 It is a schematic diagram of the illumination of the ring light and the ring side light in the present application.

[0036] Figure 3The schematic diagram of full light and mixed light irradiation in the present application.

[0037] Figure 4 The schematic diagram of actual test effect in the present application.

[0038] In the figure: 1-main probe, 2-lateral probe, 3-coaxial light, 4-coaxial lateral light, 5-ring light, 6-ring lateral light, 7-full light, 8-mixed light. DETAILED DESCRIPTION

[0039] Example 1

[0040] The first aspect of the embodiment 1 provides a positive sample micropore metering method, and the steps include the following steps: (1) determining the position of the positive sample micropore under normal vision by using a microscope; (2) determining the hole condition by projecting a light path to irradiate the micropore position through an illuminating light head; (3) determining the sample thickness by using a thickness gauge, selecting a suitable light path, adjusting the lens focal point distance to be consistent with the thickness of the positive sample to-be-measured region, and finally performing 3D scanning reconstruction by using an ultra-depth-of-field 3D digital microscope.

[0041] In the embodiment, the positive sample is a CCIT positive sample.

[0042] In the embodiment, the positive sample is a PVC soft bag.

[0043] In the embodiment, as shown in Figures 1-3 The illuminating light head structure mainly includes a main probe 1 and two lateral probes 2 fixedly connected on both sides; the illuminating light of the main probe 1 is in the shape of an inverted trapezoid vertically downward; and the illuminating light of the lateral probe 2 is in the shape of an oblique line with an angle of 60° with the horizontal line.

[0044] In the embodiment, the magnification of the microscope in step (1) is 1400 times.

[0045] In the embodiment, the light path is coaxial light.

[0046] In the embodiment, the specific operation method for determining the sample thickness by using the thickness gauge in step (3) is that the coupling agent is coated on the to-be-measured thickness region, the probe of the thickness gauge is tightly attached to the region coated with the ultrasonic coupling agent, the thickness of the positive sample at the region is measured by using the ultrasonic transmission and is calibrated.

[0047] In the embodiment, the scanning time of the ultra-depth-of-field 3D digital microscope for 3D scanning reconstruction is 3 minutes.

[0048] In the embodiment, the model of the ultra-depth-of-field 3D digital microscope is VHX-970F, which is purchased from Keyence Corporation.

[0049] In this embodiment, the thickness gauge is UM-2D, the test precision is ±10 microns, and is purchased from Shenzhen Zhuo Yi Instrument and Meter Co., Ltd.

[0050] In this embodiment, the coupling agent is purchased from Jining High-tech Zone Jinnot Medical Gel Factory, and the product name is medical ultrasonic coupling agent.

[0051] In this embodiment, the hole condition is a smooth hole.

[0052] Example 2

[0053] The specific implementation manner of this embodiment is the same as that of embodiment 1, except that the hole condition is a rough hole, and the light path used is annular light.

[0054] Example 3

[0055] The specific implementation manner of this embodiment is the same as that of embodiment 1, except that the hole condition is an ultra-deep hole, and the light path used is full light.

[0056] Through the implementation and the attached Figures 1-4 It can be known that the positive sample micropore metering method and application provided by the application have a good package material micropore aperture measurement method, and effectively avoid the micropore aperture deformation caused by pressure, are suitable for popularization in the package material air tightness test field, and have a broad development prospect.

Claims

1. A method of positive sample micro-well metering, the method comprising: The steps comprise at least the following steps: (1) determining the position of the positive sample micropore under normal vision by using a microscope; (2) determining the channel condition by projecting light on the micropore position through an illuminating light head; (3) determining the sample thickness by using a thickness gauge, selecting a suitable light path, adjusting the lens focal point distance to be consistent with the thickness of the positive sample to be measured, and finally performing 3D scanning reconstruction by using an ultra-depth 3D digital microscope; ​ The positive sample is a CCIT positive sample; the positive sample is a PVC soft bag; The illuminating light head structure comprises a main probe (1) and two side probes (2) fixedly connected on the two sides; the main probe (1) irradiates light rays in a vertical downward inverted trapezoidal shape; the side probes (2) irradiate light rays in a slant line type, and the included angle with the horizontal line is 20-80°; When the channel condition is a smooth hole, coaxial light or coaxial side light is used as the main light source of the illuminating light head, and then 3D scanning is performed on the smooth hole; When the channel condition is a rough hole, ring light or ring side light is used as the main light source of the illuminating light head, and then 3D scanning is performed on the rough hole; When the channel condition is an ultra-deep hole, full light or mixed light is used as the main light source of the illuminating light head, and then 3D scanning is performed on the ultra-deep hole.

2. The positive sample micro-well metering method of claim 1, wherein: The magnification of the microscope in step (1) is 1000-2000 times.

3. The positive sample micro-well metering method according to any one of claims 1-2, characterized in that: In step (3), the specific operation method for determining the sample thickness by using a thickness gauge is as follows: coupling agent is coated on the area to be measured, the probe of the thickness gauge is tightly attached to the area coated with ultrasonic coupling agent, and the positive sample in the area coated with ultrasonic coupling agent is measured and calibrated by using ultrasonic transmission.

4. The positive sample micro-well metering method of claim 3, wherein: The scanning time of the ultra-depth 3D digital microscope for 3D scanning reconstruction in step (3) is 1-6 minutes.

5. The positive sample micro-well metering method of claim 1, wherein: The ultra-deep hole is a positive sample micropore with a channel depth greater than 1000 microns.

6. Use of the positive sample microwell metrology method according to any one of claims 1 to 5, characterized in that: The application of the method in a packaging material air tightness detection method.

Images