CN115839801B - A method for preparing a positive sample for sealing test - Google Patents
A method for preparing a positive sample for sealing testInfo
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- CN115839801B CN115839801B CN202111097299.3A CN202111097299A CN115839801B CN 115839801 B CN115839801 B CN 115839801B CN 202111097299 A CN202111097299 A CN 202111097299A CN 115839801 B CN115839801 B CN 115839801B
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Abstract
The application discloses a preparation method of a positive sample for tightness detection, which comprises the following steps of calculating the physical aperture of a capillary corresponding to a target equivalent aperture and the length required to be intercepted according to the relation between the equivalent aperture of the capillary and the physical aperture and the length of the capillary, intercepting the corresponding capillary according to the calculated physical aperture and length of the capillary, perforating the corresponding position of a packaging material by using a needle head, inserting the capillary, sealing the contact part of the capillary and the packaging material by using sealant, and waiting for glue to be solidified. The method provided by the application has the characteristics of simplicity and convenience in operation, low cost, stable performance, strong repeatability, wide application and the like.
Description
Technical Field
The invention belongs to the technical field of micropore processing, and particularly relates to a preparation method of a positive sample for tightness detection.
Background
The national drug administration of supervision (drug administration) in 2020 issued technical guidelines for research on the sealability of chemical injection packaging systems (trial runs) and required the sealability detection of injection preparations, and the detection method required the verification of sensitivity using positive samples with known defects, so the demand for preparing micropores with a certain pore diameter on pharmaceutical packaging materials is increasing. The sensitivity of the tightness detection method can reach 1-5 mu m generally, so that micron-sized leakage holes are needed to be prepared on the medicinal packaging material.
The most commonly used micropore preparation technology in the market at present is laser drilling, and the high energy of laser is utilized to make the material melt and gasify to generate micropores. The laser drilling technology has the following defects that 1, a laser drilling device needs expensive and precise instruments, a laser device is high in cost and limited in service life, the cost of the laser drilling is very high, 2, a professional technician is required to set test parameters according to different package material fumbling conditions, 3, the laser drilling principle is that high energy of laser acts on materials to enable the materials to be melted and gasified to generate micropores, the shape of the holes is difficult to achieve uniformity, the size of each hole needs to be measured, and professional measuring equipment is required for measurement, 4, due to the fact that the difference of different materials is large, each material needs to be developed by a special method, irregular melting is generated in a drilling process for materials with low melting points, such as co-extrusion films, PP, PE and the like, the pore diameter is difficult to control, the repeatability of positive sample preparation is poor, the success rate is low, 5, the effect of temperature and humidity of micropores generated by the laser drilling is required to be carefully stored, the effective period is relatively short, 6, the laser drilling can only have requirements on the thickness of the materials, and the position on the materials can be limited, 7, and the packaging can not be used for preparing packaging bags and packaging bags for infusion packaging in an integrated manner. The above disadvantages result in laser-drilled positive samples that can only be customized in a specific setting, are expensive, have long preparation cycles, cannot be reused for a long period of time, and are very inconvenient for routine testing.
Therefore, a microporous preparation method which is simple and convenient to operate, low in manufacturing cost, stable in performance, capable of preparing uniform pore diameters in a large scale and wide in application is very necessary for promoting the development of the tightness detection of medicines.
Disclosure of Invention
In order to solve the technical problems, the application provides a preparation method of a positive sample for tightness detection.
The preparation method of the positive sample for detecting the tightness provided by the invention comprises the following steps:
Calculating the capillary physical aperture corresponding to the target equivalent aperture and the length to be intercepted according to the relation between the capillary equivalent aperture and the capillary physical aperture and the length;
And cutting the corresponding capillary according to the calculated physical aperture and length of the capillary, punching holes at the corresponding positions of the package material by using a needle head, inserting the capillary, sealing the contact part of the capillary and the package material by using sealant, and waiting for curing of the glue.
In some embodiments of the application, the relationship between capillary equivalent pore size and capillary physical pore size and length is:
wherein D is equivalent pore diameter (μm), D is capillary physical pore diameter (μm), and L is capillary length (mm).
In some embodiments of the present application, a method for obtaining a relationship between a capillary equivalent pore size and a capillary physical pore size and length includes the steps of:
Taking a capillary tube with a certain aperture, intercepting different lengths, metering the flow passing through the capillary tube under the conditions of a certain temperature and a certain pressure difference, and converting the flow into an equivalent aperture;
Obtaining data of a plurality of groups of capillary apertures, lengths and equivalent apertures;
And carrying out linear regression analysis on the multiple groups of data to obtain a relation between the equivalent aperture and the physical aperture and length of the capillary tube, which are suitable for tightness detection.
In some embodiments of the application, the capillary is a fused silica capillary, a polyimide coated capillary, a glass capillary, or a metal capillary.
In some embodiments of the application, the packaging material comprises, but is not limited to, a plastic ampoule, a co-extrusion film bag, a glass ampoule, an eye drop bottle, a penicillin bottle body, a rubber plug and pre-filling and sealing.
In some embodiments of the present application, the sealant includes, but is not limited to, instant adhesive, ultraviolet curing agent, epoxy adhesive, silicone adhesive, PE adhesive, polyacrylamide adhesive.
In some embodiments of the application, the capillary physical pore size range includes, but is not limited to, 2 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 40 μm, 50 μm, 75 μm, 100 μm, 250 μm, 500 μm.
In some embodiments of the application, the equivalent pore size range is 0.1-100 μm.
Compared with the prior art, the invention has the following advantages:
(1) The capillary used is low in price, easy to obtain and low in cost;
(2) The preparation method is simple, can be operated by oneself in a laboratory, and does not need special technology and instruments;
(3) The aperture accuracy is better than that of laser drilling, and the accuracy is high;
(4) Because the capillary tube has uniform diameter, the positive samples with uniform pore diameters can be prepared in batches only by cutting the same length;
(5) The capillary tube has stable performance, is not influenced by temperature, humidity and pressure, can be repeatedly used, and has long effective period;
(6) The package material is not limited, can be prepared on any package material, can be prepared on plastic package materials and rubber plugs by using sharp objects such as needle heads for punching, and can be prepared on glass package materials by means of laser drilling or mechanical drilling devices, but has no requirement on the size of the holes, and is convenient to operate;
(7) The preparation method can be used for preparing the blank coating material, can also be used for preparing finished products, and has wide application range;
(8) Can be prepared at any part of the packing material without limitation.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application as claimed.
Drawings
In order to more clearly illustrate the technical solution of the present application, the drawings that are needed in the embodiments will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic flow chart of a preparation method of a positive sample for tightness detection according to an embodiment of the present invention;
FIG. 2 is a fitted curve of capillary length versus flow rate for a physical aperture of 20 μm provided by an embodiment of the present invention;
FIG. 3 is a fitted curve of capillary length versus flow rate for a physical aperture of 30 μm provided by an embodiment of the present invention;
FIG. 4 is a fitted curve of capillary length versus flow rate for a physical aperture of 40 μm provided by an embodiment of the present invention;
fig. 5 is a graph showing an accuracy distribution of calculating equivalent pore diameters according to an embodiment of the present invention.
Detailed Description
In order to make the technical solution of the present application better understood by those skilled in the art, the technical solution of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Fig. 1 is a schematic flow chart of a preparation method of a positive sample for leak detection according to an embodiment of the present invention, and the preparation method of a positive sample for leak detection according to an embodiment of the present invention is described in detail below with reference to fig. 1.
As shown in fig. 1, the preparation method of the positive sample for leak detection specifically includes the following steps:
and S10, calculating the capillary physical aperture corresponding to the target equivalent aperture and the length to be intercepted according to the relation between the capillary equivalent aperture and the capillary physical aperture and the length.
The capillary tube is a uniform micro tube with a certain aperture, the inner layer of the capillary tube selected in the embodiment of the application is a hollow fused quartz layer, and the outer layer is a polymer coating. The capillary tube has stable performance, is not affected by temperature, humidity and pressure, has uniform aperture, has equivalent toughness, is not easy to damage, and has low price and easy obtainment.
The capillary itself has a certain physical pore size (D), but this physical size pore size is not the same concept as the equivalent pore size (D) in the tightness test. The equivalent pore diameter in the tightness test is obtained by measuring the gas flow (flow) through the micropores under the condition of a certain temperature and pressure difference, and the gas flow through the capillary under the condition of a certain temperature and pressure is related to the physical pore diameter (d) and the length (L) of the capillary. For a capillary with a certain diameter, the longer the length is, the smaller the flow is, the smaller the equivalent aperture D measured by the flow is, and for a capillary with a certain length, the larger the aperture is, the larger the equivalent aperture D measured by the flow is, so that when a capillary positive sample is prepared, the relationship between the equivalent aperture D and the physical aperture D and the length L of the capillary is required to be determined.
The method for determining the relationship between the equivalent aperture D and the physical aperture D and the length L of the capillary tube comprises the steps of taking the capillary tube with a certain aperture, intercepting different lengths, measuring the flow passing through the capillary tube under the condition of a certain temperature and a certain pressure difference, converting the flow into the equivalent aperture, obtaining a plurality of groups of data of the aperture, the length and the equivalent aperture of the capillary tube, and carrying out linear regression analysis on the plurality of groups of data to obtain the relationship between the equivalent aperture and the physical aperture and the length of the capillary tube, which are suitable for tightness detection. The relationship between the equivalent pore diameter of the capillary and the physical pore diameter and length of the capillary is as follows:
wherein D is equivalent pore diameter (μm), D is capillary physical pore diameter (μm), and L is capillary length (mm).
Further, the specific method for obtaining the relation between the equivalent aperture and the physical aperture and length of the capillary tube suitable for tightness detection by performing linear regression analysis on multiple groups of data comprises the following steps:
capillary material information is selected:
TABLE 1 capillary information
The operation steps are as follows:
(1) Obtaining the relation between flow and capillary length (L), namely taking capillaries with physical apertures of 20 mu m, 30 mu m and 40 mu m respectively, intercepting capillaries with different lengths, accurately measuring the lengths by using a vernier caliper, implanting the intercepted capillaries into a rubber plug of a card bottle, measuring the card bottle by using a flow measuring device to obtain 'measuring flow', and carrying out linear regression analysis on the gas flow and the capillary length to obtain a relation formula of flow and length.
The capillary lengths of 20 μm, 30 μm, 40 μm and the flow metering results are shown in tables 2, 3 and 4.
Table 2 calculation of equivalent pore diameter of 20 μm capillary and measurement result (d=20.8 μm)
Table 3 30 μm capillary calculation and measurement (d=30.25 μm)
Table 4 40 μm capillary calculation and measurement results (d=40.3 μm)
Fitting curves of capillary lengths of 20 μm, 30 μm, and 40 μm to flow metering results are shown in fig. 2,3, and 4, and fitting formulas are shown in table 5, and the formulas can be simplified to y=ax form due to the very small intercept of the formulas.
TABLE 5 fitting results
| Capillary physical aperture (mum) | Fitting formula | Simplified formula |
| 20.8 | flow=0.773(1/L)+0.006 | flow=0.773(1/L) |
| 30.25 | flow=3.1904(1/L)+0.0244 | flow=3.1904(1/L) |
| 40.3 | flow=10.22(1/L)+0.079 | flow=10.22(1/L) |
Wherein flow is gas flow (sccm), L is capillary length (mm).
(2) Deriving the relationship between the flow and the capillary physical aperture (d) and the length (L), wherein the simplified relationship is further related to the capillary physical aperture, and the following relationship can be obtained through linear fitting:
0.0088 is also small and negligible, further reducing the above equation to:
wherein flow is gas flow (sccm), L is capillary length (mm), and d is capillary physical pore size (μm).
The relationship between the equivalent pore diameter D and the physical pore diameter (D) and the length (L) of the capillary tube is deduced by correlating the formula with a pore diameter measurement formula, wherein the pore diameter measurement formula is derived from a calculation formula of the relationship between the flow rate and the pore diameter of Lenox laser company, is a general formula for measuring a positive sample with tightness, lenox laser is a USP approved pore diameter measurement company, and USP1207 refers to the pore diameter and flow rate corresponding data provided by the general formula. The aperture metering formula is:
Substituting the flow (flow) with the capillary physical aperture (d) and length (L) relationship yields the following relationship:
Inlet Pressure (PSIA), pi=14.7 PSIA at standard atmospheric pressure;
0.01749 constants in gas flow calculation;
Factor, when delta P/Pi is more than or equal to 0.5, factor=1, delta P is the pressure difference between the inside and the outside of the packaging container;
molecular weight of gas, air molecular weight m.w. =29;
temp DEG R is the Rankine temperature, and the Rankine temperature 536.67 at the room temperature of 25 ℃ is taken;
The simplified formula is obtained:
wherein D is equivalent pore diameter (μm), D is capillary physical pore diameter (μm), L is capillary length (mm)
(3) And verifying the accuracy of the formula, namely, performing multiple simplification processing in the whole formula derivation process, and verifying the accuracy of the formula. And (3) verifying operation, namely bringing the physical aperture and the length of the capillary tube intercepted in the step (1) into a formula to calculate an equivalent aperture, and comparing the equivalent aperture with a metering equivalent aperture obtained by flow metering to judge the accuracy. See tables 2,3, 4 for specific values.
Wherein, the
As can be seen from fig. 5, by analyzing 86 samples, the distribution range of the pore diameter accuracy calculated according to the above formula is 94.4% -112.1%, and the tolerance of microporous preparation is 3 μm, 5 μm is ±1 μm,10 μm is ±2 μm according to industry standard, and the accuracy is 94.4% -112.1% which can completely meet the requirements.
S20, cutting the corresponding capillary according to the calculated physical aperture and length of the capillary, punching holes at the corresponding positions of the packing material by using a needle head, inserting the capillary, sealing the contact part of the capillary and the packing material by using sealant, and waiting for curing of the glue.
In some embodiments of the present application, the capillary used is a fused silica capillary, a polyimide coated capillary, a glass capillary, a metal capillary, or the like. The capillary physical pore size ranges may be 2 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 40 μm, 50 μm, 75 μm, 100 μm, 250 μm, 500 μm. The equivalent pore size may range from 0.1 to 100 μm.
In some embodiments of the application, the application range of the packaging material comprises, but is not limited to, plastic ampoule, co-extrusion film bag, glass ampoule, eye drop bottle, penicillin bottle body, rubber plug and pre-filling and sealing.
In some embodiments of the present application, the sealant selected may be a flash adhesive, an ultraviolet curing agent, an epoxy adhesive, a silicone adhesive, a PE adhesive, or a polyacrylamide adhesive.
The above embodiments have been described in detail, which are intended to be illustrative and not limiting, and several embodiments can be enumerated in the limited scope, so that variations and modifications do not depart from the general inventive concept.
Other embodiments of the application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure of the application herein. This application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the application being indicated by the following claims.
The above embodiments of the present application do not limit the scope of the present application.
Claims (6)
1. The preparation method of the positive sample for the tightness detection is characterized by comprising the following steps of:
Calculating the capillary physical aperture corresponding to the target equivalent aperture and the length to be intercepted according to the relation between the capillary equivalent aperture and the capillary physical aperture and the length;
intercepting a corresponding capillary according to the calculated physical aperture and length of the capillary, punching holes at corresponding positions of the packaging material by using a needle head, inserting the capillary, sealing the contact part of the capillary and the packaging material by using sealant, and waiting for curing the glue to obtain the composite material;
the relationship between the equivalent pore diameter of the capillary and the physical pore diameter and length of the capillary is as follows:
wherein D is equivalent aperture, the unit is mu m, D is capillary physical aperture, the unit is mu m, L is capillary length, and the unit is mm;
The method for acquiring the relation between the equivalent pore diameter of the capillary and the physical pore diameter and length of the capillary comprises the following steps:
Taking a capillary tube with a certain aperture, intercepting different lengths, metering the flow passing through the capillary tube under the conditions of a certain temperature and a certain pressure difference, and converting the flow into an equivalent aperture;
Obtaining data of a plurality of groups of capillary apertures, lengths and equivalent apertures;
And carrying out linear regression analysis on the multiple groups of data to obtain a relation between the equivalent aperture and the physical aperture and length of the capillary tube, which are suitable for tightness detection.
2. The method for preparing a positive sample for leak detection according to claim 1, wherein the capillary is a fused silica capillary, a polyimide coated capillary, a glass capillary, or a metal capillary.
3. The method for preparing a positive sample for leak detection according to claim 1, wherein the packaging material is a plastic ampoule, a co-extrusion film bag, a glass ampoule, an eye drop bottle, a penicillin bottle body, a rubber plug or a prefilled package.
4. The method for preparing a positive sample for leak detection according to claim 1, wherein the sealant is a quick-setting adhesive, an ultraviolet curing agent, an epoxy resin adhesive, a silicone adhesive, a PE adhesive, or a polyacrylamide adhesive.
5. The method for preparing a positive sample for leak detection according to claim 1, wherein the capillary physical pore size is in a range of 2 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 40 μm, 50 μm, 75 μm, 100 μm, 250 μm or 500 μm.
6. The method for preparing a positive sample for leak detection according to claim 1, wherein the capillary equivalent pore diameter is in the range of 0.1 to 100. Mu.m.
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| RU2280246C1 (en) * | 2004-12-16 | 2006-07-20 | Саратовский военный институт радиационной, химической и биологической защиты (СВИРХБЗ) | Capillary batcher for steam-gas mixtures |
| CN209589350U (en) * | 2019-07-26 | 2019-11-05 | 济南三泉中石实验仪器有限公司 | A kind of producing device of aseptic packaging positive control sample |
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| TW593960B (en) * | 2002-12-06 | 2004-06-21 | Huei-Chiun Shiu | Method for installing heat pipe capillary and device therefor |
| US7752895B2 (en) * | 2006-11-30 | 2010-07-13 | Chevron Oronite S.A. | Method for using an alternate pressure viscometer |
| CN103899908A (en) * | 2014-02-27 | 2014-07-02 | 大连阿姆泰科自动化装备有限公司 | Gas flow fixing device and manufacturing method thereof |
| CN113092027B (en) * | 2021-04-06 | 2022-04-26 | 湖北科伦药业有限公司 | Method for checking tightness of polypropylene ampoule bottle by air pressure method |
| CN113092010B (en) * | 2021-04-06 | 2022-04-26 | 湖北科伦药业有限公司 | Method for checking sealing performance of polypropylene ampoule bottle by biological method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2280246C1 (en) * | 2004-12-16 | 2006-07-20 | Саратовский военный институт радиационной, химической и биологической защиты (СВИРХБЗ) | Capillary batcher for steam-gas mixtures |
| CN209589350U (en) * | 2019-07-26 | 2019-11-05 | 济南三泉中石实验仪器有限公司 | A kind of producing device of aseptic packaging positive control sample |
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Inventor after: Jia Yuxiang Inventor after: Zhang Sai Inventor after: Huang Chunyan Inventor after: Jia Ru Inventor after: Yang Shuang Inventor after: Jiao Meixia Inventor after: Wang Yue Inventor before: Jia Yuxiang Inventor before: Zhang Sai Inventor before: Huang Chunyan Inventor before: Jia Ru Inventor before: Yang Shuang Inventor before: Jiao Meixia Inventor before: Wang Yue |
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