CN105092234A - System and method applying isolation tank for liquid dosing system filter core on-line integrity tests - Google Patents
System and method applying isolation tank for liquid dosing system filter core on-line integrity tests Download PDFInfo
- Publication number
- CN105092234A CN105092234A CN201510578250.8A CN201510578250A CN105092234A CN 105092234 A CN105092234 A CN 105092234A CN 201510578250 A CN201510578250 A CN 201510578250A CN 105092234 A CN105092234 A CN 105092234A
- Authority
- CN
- China
- Prior art keywords
- valve
- filtrator
- mouth
- filter core
- outlet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention provides a liquid dosing system filter core on-line integrity test system applying an isolation tank. The invention further provides a liquid dosing system filter core on-line integrity test method based on the on-line integrity test system and applying the isolation tank. Through the method, disadvantages in the prior art are solved, filter core on-line integrity test functions and protection on aseptic environments after disinfection of a liquid dosing system are realized, a problem that damage to a filter core caused by disinfection of the filter core can not be timely discovered is prevented, and the aseptic environment of the system can further not be damaged. The method and the effects satisfy requirements of more and more manufacturers in pharmacy industries.
Description
Technical field
The present invention relates to the application system of a kind of gas sealing chamber in the online integrity test of liquid mixing system filter core and method, for ensureing aseptic during the online integrity test of the filter core of pharmaceutical industry fully-automatic liquid make-up system, belonging to dosing control technology field.
Background technology
Pharmaceutical industry liquid mixing system valve is many, pipeline is complicated, requires high to system gnotobasis, must ensure that the integrality of filter core before liquor charging is good, do online integrity test to these needs before liquor charging to filter core.
During traditional filter core online integrity detection, the outlet of filtrator is connected with the comb of liquid mixing system, and comb is connected with total row in whole workshop, certain pressure can be there is in total row in workshop, gas in total row or liquid can pour in down a chimney in liquid mixing system, and then pollute the gnotobasis of liquid mixing system, the gnotobasis of the outlet of filtrator and filter core rear end is destroyed.
Summary of the invention
The technical problem to be solved in the present invention is: isolation when realizing filter core online integrity test between filtrator rear end and liquid mixing system comb, ensures aseptic during the online integrity test of filter core.
In order to solve the problems of the technologies described above, a technical scheme of the present invention there is provided a kind of online integrity testing system of liquid mixing system filter core applying sealing chamber, it is characterized in that: comprise filtrator, pressurized air is via electro connecting pressure gauge, integrity tester and valve two are arranged mouth with the gas of filtrator and are connected, the gas row mouth of filtrator also via valve one with always arrange mouth and be connected, liquid is successively via valve three, valve four and pressure transducer one connect the import of filtrator, water for injection/pressurized air/pure steam connects the import of filtrator via valve four and pressure transducer one, the outlet of filtrator connects valve five, valve aspect on May Day connects medicine liquid outlet via valve six, connect via valve seven on the other hand and always arrange mouth, pipeline between valve five and the outlet of filtrator is provided with pressure transducer two, pipeline between valve five and valve seven is provided with temperature sensor, one end of valve eight is connected with the pipeline between temperature sensor with valve seven, the other end of valve eight connects the import of sealing chamber, the outlet of sealing chamber via valve nine with always arrange mouth and be connected, the gas vent of sealing chamber connects the gas feed of respirator, the outlet of respirator is connected with gas outlet via valve ten on the one hand, on the other hand via valve 11 with always arrange mouth and be connected, the freeing port of respirator via valve 12 with always arrange mouth and be connected,
Valve one, valve two, valve three, valve four, valve five, valve six, valve seven, valve eight, valve nine, valve ten, valve 11, valve 12 are connected with valve island, valve island connects PLC, PLC and is also connected with pressure transducer one, pressure transducer two, temperature sensor and electro connecting pressure gauge.
Another technical scheme of the present invention there is provided a kind of online Integrity Testing of liquid mixing system filter core of the application sealing chamber based on above-mentioned online integrity testing system, it is characterized in that, comprises the following steps:
Confirm before the first step, integrity test
1) air supply pressure is normal, the reading >=0.5MPa of electro connecting pressure gauge;
2) system sterilizing terminates, and comprises filtrator, sealing chamber and respirator, and enters auto state;
3) associated pipe and cartridge pressure discharge;
4) integrity tester accesses and is ready to;
Second step, filter core are wetting:
1) pressure of filter element and associated conduit, sealing chamber is discharged;
2) water for injection cooled passes in filtrator via valve four, first discharge from total row's mouth after gas row's mouth and valve one of filter, after keeping water for injection to be circulated to the time span one of setting, discharge from total row's mouth after the outlet of filter, valve five and valve seven again, after being circulated to the time span two of setting, stop passing into water for injection;
3) pressurized air passes in filtrator via valve four, discharge from total row's mouth after gas row's mouth and valve one of filter on the one hand and purge, discharge from total row's mouth after the outlet of filter, valve five and valve seven on the other hand and purge, to remove the water for injection of pipeline residual, meanwhile, the residual water for injection of filtrator rear end enters in sealing chamber via valve eight;
3rd step, to be tested by integrity tester, valve seven is closed, valve eight is opened, valve ten is opened, pressurized air enters filtrator via valve two, pass in respirator after entering sealing chamber via valve five and valve eight again, communicated with room by respirator filter core, keep with no pressure;
If the test result of the 4th step integrity tester is qualified, then enter the 6th step, if the test result of integrity tester is defective, then select again to soak, retest or more renew cartridge, select again wetting after, jump to second step, after selection retests, jump to the 3rd step, select, more after renew cartridge, to jump to the 5th step;
5th step, sterilizing is carried out to filter core
1) pressurized air is passed in filtrator via valve four, discharge from total row's mouth after gas row's mouth and valve one of filter on the one hand and purge, discharge from total row's mouth after the outlet of filter, valve five and valve seven on the other hand and purge, after purging the time span three continuing setting, residual water for injection is drained;
2) discharge the pressure of filtrator and associated pipe, until obtain force value≤0.02MPa by pressure transducer one and pressure transducer two, after the time span four of delay adjustments, change the filter core of filtrator;
3) pure steam is passed in filtrator via valve four, sterilizing is carried out to the filter core in filtrator, continue the time span five of setting;
4) pressurized air is passed in filtrator via valve four, utilize the filter core of the purged filter of pressurized air, and by after steam discharging, jump to second step;
6th step, pressurized air is passed in filtrator via valve four; after utilizing pressurized air to purge the time span six of setting to filtrator; by emptying for residual water for injection; again pressurising protection is carried out to filtrator and associated pipe, make to obtain force value >=0.15MPa by pressure transducer one and pressure transducer two.
7th step, end test.
Method provided by the invention overcomes the deficiency of existing scheme; achieve the online integrity test function of the filter core after liquid mixing system sterilizing and the protection to gnotobasis; avoid sterilizing to cause filter core and to damage and can not the problem of Timeliness coverage, the gnotobasis of system can not be destroyed again simultaneously.Method of the present invention and effect meet the demand of increasing pharmaceutical industry producer.
Accompanying drawing explanation
Fig. 1 is online integrity testing system schematic diagram;
Fig. 2 is online integrity test control flow chart provided by the invention.
Embodiment
For making the present invention become apparent, hereby with preferred embodiment, and accompanying drawing is coordinated to be described in detail below.
As shown in Figure 1, a kind of online integrity testing system of liquid mixing system filter core applying sealing chamber provided by the invention, comprise filtrator 1, pressurized air is via electro connecting pressure gauge 7, integrity tester and valve two B arrange mouth with the gas of filtrator 1 and are connected, the gas row mouth of filtrator 1 also via valve one A with always arrange mouth and be connected, liquid is successively via valve three C, valve four D and pressure transducer 1 connect the import of filtrator 1, water for injection/pressurized air/pure steam connects the import of filtrator 1 via valve four D and pressure transducer 1, the outlet of filtrator 1 connects valve five E, valve five E mono-aspect connects medicine liquid outlet via valve six F, connect via valve seven G on the other hand and always arrange mouth, pipeline between valve five E and the outlet of filtrator 1 is provided with pressure transducer 25, pipeline between valve five E and valve seven G is provided with temperature sensor 6, one end of valve eight H is connected with the pipeline between temperature sensor 6 with valve seven G, the other end of valve eight H connects the import of sealing chamber 2, the outlet of sealing chamber 2 via valve nine I with always arrange mouth and be connected, the gas vent of sealing chamber 2 connects the gas feed of respirator 3, the outlet of respirator 3 is connected with gas outlet via valve ten J on the one hand, on the other hand via valve 11 K with always arrange mouth and be connected, the freeing port of respirator 3 via valve 12 L with always arrange mouth and be connected,
Valve one A, valve two B, valve three C, valve four D, valve five E, valve six F, valve seven G, valve eight H, valve nine I, valve ten J, valve 11 K, valve 12 L are connected with valve island, valve island connects PLC, PLC and is also connected with pressure transducer 1, pressure transducer 25, temperature sensor 6 and electro connecting pressure gauge 7.
Composition graphs 2, present invention also offers a kind of online Integrity Testing of liquid mixing system filter core of the application sealing chamber based on above-mentioned online integrity testing system, comprises the following steps:
Confirm before the first step, integrity test
1 air supply pressure is normal, the reading >=0.5MPa of electro connecting pressure gauge 7;
2 system sterilizings terminate, and comprise filtrator 1, sealing chamber 2 and respirator 3, and enter auto state;
3 associated pipe and cartridge pressure discharge;
4 integrity testers access and are ready to;
Second step, filter core are wetting:
1 release filtrator 1 filter core and associated conduit, sealing chamber 2 pressure;
The water for injection of 2 coolings passes in filtrator 1 via valve four D, first discharge from total row's mouth after gas row's mouth and valve one A of filter 1, after keeping water for injection to be circulated to 30s, discharge from total row's mouth after the outlet, valve five E and valve seven G of filter 1 again, after being circulated to the 30s of setting, stop passing into water for injection;
3 pressurized air pass in filtrator 1 via valve four D, discharge from total row's mouth after gas row's mouth and valve one A of filter 1 on the one hand and purge, discharge from total row's mouth after the outlet, valve five E and valve seven G of filter 1 on the other hand and purge, to remove the water for injection of pipeline residual, meanwhile, the residual water for injection of filtrator 1 rear end enters in sealing chamber 2 via valve eight H;
3rd step, to be tested by integrity tester, valve seven G is closed, valve eight H is opened, valve ten J is opened, pressurized air enters filtrator 1 via valve two B, pass in respirator 3 after entering sealing chamber 2 via valve five E and valve eight H again, communicated with room by respirator 3 filter core, keep with no pressure;
If the test result of the 4th step integrity tester is qualified, then enter the 6th step, if the test result of integrity tester is defective, then select again to soak, retest or more renew cartridge, select again wetting after, jump to second step, after selection retests, jump to the 3rd step, select, more after renew cartridge, to jump to the 5th step;
5th step, sterilizing is carried out to filter core
Pressurized air passes in filtrator 1 via valve four D by 1, discharge from total row's mouth after gas row's mouth and valve one A of filter 1 on the one hand and purge, discharge from total row's mouth after the outlet, valve five E and valve seven G of filter 1 on the other hand and purge, purge after continuing 30s, residual water for injection is drained;
The pressure of 2 release filtrators 1 and associated pipe, until obtain force value≤0.02MPa by pressure transducer 1 and pressure transducer 25, changes the filter core of filtrator 1 after time delay 20s;
Pure steam passes in filtrator 1 via valve four D by 3, carries out sterilizing to the filter core in filtrator 1, continues 30min;
Pressurized air passes in filtrator 1 via valve four D by 4, utilizes the filter core of the purged filter 1 of pressurized air, and by after steam discharging, jumps to second step;
6th step, pressurized air is passed in filtrator 1 via valve four D, after utilizing pressurized air to purge 30s to filtrator 1, by emptying for residual water for injection, again pressurising protection is carried out to filtrator 1 and associated pipe, make to obtain force value >=0.15MPa by pressure transducer 1 and pressure transducer 25;
7th step, end test.
In whole liquid mixing system operational process, if the pressure < 0.5MPa that electro connecting pressure gauge 7 obtains, then after time delay 30s, system can run time-out automatically, guarantees that starting valve normally opens; After control power supply sky holds escape, system can run time-out automatically, and after above-mentioned several heavy warning is got rid of, system can recover normal operation again.
Claims (2)
1. apply the online integrity testing system of liquid mixing system filter core of sealing chamber for one kind, it is characterized in that: comprise filtrator (1), pressurized air is via electro connecting pressure gauge (7), integrity tester and valve two (B) are arranged mouth with the gas of filtrator (1) and are connected, the gas row mouth of filtrator (1) also via valve one (A) with always arrange mouth and be connected, liquid is successively via valve three (C), valve four (D) and pressure transducer one (4) connect the import of filtrator (1), water for injection/pressurized air/pure steam connects the import of filtrator (1) via valve four (D) and pressure transducer one (4), the outlet of filtrator (1) connects valve five (E), valve five (E) connects medicine liquid outlet via valve six (F) on the one hand, connect via valve seven (G) on the other hand and always arrange mouth, pipeline between valve five (E) and the outlet of filtrator (1) is provided with pressure transducer two (5), pipeline between valve five (E) and valve seven (G) is provided with temperature sensor (6), one end of valve eight (H) is connected with the pipeline between temperature sensor (6) with valve seven (G), the other end of valve eight (H) connects the import of sealing chamber (2), the outlet of sealing chamber (2) via valve nine (I) with always arrange mouth and be connected, the gas vent of sealing chamber (2) connects the gas feed of respirator (3), the outlet of respirator (3) is connected with gas outlet via valve ten (J) on the one hand, on the other hand via valve 11 (K) with always arrange mouth and be connected, the freeing port of respirator (3) via valve 12 (L) with always arrange mouth and be connected,
Valve one (A), valve two (B), valve three (C), valve four (D), valve five (E), valve six (F), valve seven (G), valve eight (H), valve nine (I), valve ten (J), valve 11 (K), valve 12 (L) are connected with valve island, valve island connects PLC, PLC and is also connected with pressure transducer one (4), pressure transducer two (5), temperature sensor (6) and electro connecting pressure gauge (7).
2., based on the online Integrity Testing of liquid mixing system filter core of the application sealing chamber of online integrity testing system as claimed in claim 1, it is characterized in that, comprise the following steps:
Confirm before the first step, integrity test
1) air supply pressure is normal, the reading >=0.5MPa of electro connecting pressure gauge;
2) system sterilizing terminates, and comprises filtrator, sealing chamber and respirator, and enters auto state;
3) associated pipe and cartridge pressure discharge;
4) integrity tester accesses and is ready to;
Second step, filter core are wetting:
1) pressure of filtrator (1) filter core and associated conduit, sealing chamber (2) is discharged;
2) water for injection cooled passes in filtrator (1) via valve four (D), first discharge from total row's mouth after gas row's mouth and valve one (A) of filter (1), after keeping water for injection to be circulated to the time span one of setting, discharge from total row's mouth after outlet again through filter (1), valve five (E) and valve seven (G), after being circulated to the time span two of setting, stop passing into water for injection;
3) pressurized air passes in filtrator (1) via valve four (D), discharge from total row's mouth after gas row's mouth and valve one (A) of filter (1) on the one hand and purge, discharge from total row's mouth after outlet on the other hand through filter (1), valve five (E) and valve seven (G) and purge, to remove the water for injection of pipeline residual, meanwhile, the residual water for injection of filtrator (1) rear end enters in sealing chamber (2) via valve eight (H);
3rd step, to be tested by integrity tester, valve seven (G) is closed, valve eight (H) is opened, valve ten (J) is opened, pressurized air enters filtrator (1) via valve two (B), pass in respirator (3) after entering sealing chamber (2) via valve five (E) and valve eight (H) again, communicated with room by respirator (3) filter core, keep with no pressure;
If the test result of the 4th step integrity tester is qualified, then enter the 6th step, if the test result of integrity tester is defective, then select again to soak, retest or more renew cartridge, select again wetting after, jump to second step, after selection retests, jump to the 3rd step, select, more after renew cartridge, to jump to the 5th step;
5th step, sterilizing is carried out to filter core
1) pressurized air is passed in filtrator (1) via valve four (D), discharge from total row's mouth after gas row's mouth and valve one (A) of filter (1) on the one hand and purge, discharge from total row's mouth after outlet on the other hand through filter (1), valve five (E) and valve seven (G) and purge, after purging the time span three continuing setting, residual water for injection is drained;
2) pressure of filtrator (1) and associated pipe is discharged, until obtain force value≤0.02MPa by pressure transducer one (4) and pressure transducer two (5), after the time span four of delay adjustments, change the filter core of filtrator (1);
3) pure steam is passed in filtrator (1) via valve four (D), sterilizing is carried out to the filter core in filtrator (1), continue the time span five of setting;
4) pressurized air is passed in filtrator (1) via valve four (D), utilize the filter core of the purged filter of pressurized air (1), and by after steam discharging, jump to second step;
6th step, pressurized air is passed in filtrator (1) via valve four (D); after utilizing pressurized air to purge the time span six of setting to filtrator (1); by emptying for residual water for injection; again pressurising protection is carried out to filtrator (1) and associated pipe, make to obtain force value >=0.15MPa by pressure transducer one (4) and pressure transducer two (5).
7th step, end test.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510578250.8A CN105092234B (en) | 2015-09-11 | 2015-09-11 | Using the online integrity testing system of liquid mixing system filter core and method of sealing chamber |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510578250.8A CN105092234B (en) | 2015-09-11 | 2015-09-11 | Using the online integrity testing system of liquid mixing system filter core and method of sealing chamber |
Publications (2)
Publication Number | Publication Date |
---|---|
CN105092234A true CN105092234A (en) | 2015-11-25 |
CN105092234B CN105092234B (en) | 2017-11-03 |
Family
ID=54573165
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201510578250.8A Active CN105092234B (en) | 2015-09-11 | 2015-09-11 | Using the online integrity testing system of liquid mixing system filter core and method of sealing chamber |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN105092234B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108613776A (en) * | 2018-07-16 | 2018-10-02 | 纳盛洁净技术(苏州)有限公司 | A kind of hydrophobic filter integrity test device |
CN109364279A (en) * | 2018-09-06 | 2019-02-22 | 丽珠集团利民制药厂 | It is a kind of can online CIP/SIP thimerosal filtration sterilization and cleaning system |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4701861A (en) * | 1985-05-31 | 1987-10-20 | Pall Corporation | Filter test device |
CN201732014U (en) * | 2010-08-20 | 2011-02-02 | 伊马莱富(北京)制药系统有限公司 | Online integrity test system of sterile filter |
CN102235963A (en) * | 2010-04-26 | 2011-11-09 | 上海威滤净化设备有限公司 | Full-automatic filter element integrity tester |
CN102435224A (en) * | 2011-11-08 | 2012-05-02 | 上海东富龙科技股份有限公司 | On-line integrity test method of filter |
CN104048839A (en) * | 2014-05-26 | 2014-09-17 | 上海东富龙拓溥科技有限公司 | On-line integrity detecting device and method used after fully-automatic sterilization |
EP2840379A1 (en) * | 2013-08-13 | 2015-02-25 | Institute of Nuclear Energy Research, Atomic | An automated test apparatus for testing risk and integrity of pharmaceutical filtration membranes and method thereof |
CN204988705U (en) * | 2015-09-11 | 2016-01-20 | 上海东富龙拓溥科技有限公司 | That uses isolation tank joins in marriage online integrality test system of liquid system filter core |
-
2015
- 2015-09-11 CN CN201510578250.8A patent/CN105092234B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4701861A (en) * | 1985-05-31 | 1987-10-20 | Pall Corporation | Filter test device |
CN102235963A (en) * | 2010-04-26 | 2011-11-09 | 上海威滤净化设备有限公司 | Full-automatic filter element integrity tester |
CN201732014U (en) * | 2010-08-20 | 2011-02-02 | 伊马莱富(北京)制药系统有限公司 | Online integrity test system of sterile filter |
CN102435224A (en) * | 2011-11-08 | 2012-05-02 | 上海东富龙科技股份有限公司 | On-line integrity test method of filter |
EP2840379A1 (en) * | 2013-08-13 | 2015-02-25 | Institute of Nuclear Energy Research, Atomic | An automated test apparatus for testing risk and integrity of pharmaceutical filtration membranes and method thereof |
CN104048839A (en) * | 2014-05-26 | 2014-09-17 | 上海东富龙拓溥科技有限公司 | On-line integrity detecting device and method used after fully-automatic sterilization |
CN204988705U (en) * | 2015-09-11 | 2016-01-20 | 上海东富龙拓溥科技有限公司 | That uses isolation tank joins in marriage online integrality test system of liquid system filter core |
Non-Patent Citations (1)
Title |
---|
张金 等: "除菌过滤系统完整性检测在生物制药行业生产中的应用", 《现代检验医学杂志》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108613776A (en) * | 2018-07-16 | 2018-10-02 | 纳盛洁净技术(苏州)有限公司 | A kind of hydrophobic filter integrity test device |
CN109364279A (en) * | 2018-09-06 | 2019-02-22 | 丽珠集团利民制药厂 | It is a kind of can online CIP/SIP thimerosal filtration sterilization and cleaning system |
Also Published As
Publication number | Publication date |
---|---|
CN105092234B (en) | 2017-11-03 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104048839A (en) | On-line integrity detecting device and method used after fully-automatic sterilization | |
CN204988705U (en) | That uses isolation tank joins in marriage online integrality test system of liquid system filter core | |
CN103698265B (en) | A kind of engine coolant cooling water tank Internal corrosion tests platform | |
CN203101036U (en) | Verification apparatus for steam verification of safety valve | |
US20090114035A1 (en) | Testing Device for High Pressure Injectors of a Common Rail Injection System, and Method for Testing High Pressure Injectors | |
CN105092234A (en) | System and method applying isolation tank for liquid dosing system filter core on-line integrity tests | |
CN102229888A (en) | Feedback-type pneumatic-control pressure stress cell culture device | |
CN103335938A (en) | Pipe conveying medium multi-flow-velocity corrosion determination apparatus and determination method thereof | |
CN102313691A (en) | Tester and test method for reverse bubble point of single filter core | |
CN202710266U (en) | Gas cylinder gas tightness detecting device | |
CN102535071A (en) | Online detection method for dye liquor components of bundle type dye machine on basis of programmable logic controller (PLC) | |
CN106969793A (en) | A kind of Batch Transportation contaminated product tests circuit platform | |
CN104075946B (en) | A kind of overpotential test device for testing anti-explosion product | |
CN102445355A (en) | System and method for testing micro-flow thermal throttling device for ionic electric propulsion | |
CN111175052A (en) | Engine gas distribution system fault testing system for engine cold test | |
CN104502039A (en) | Gas tightness detecting method for fuel gas meter | |
CN207894599U (en) | A kind of discharge coefficient test gas circuit | |
CN211504658U (en) | Safety valve service life testing device | |
CN105203277A (en) | Water injection replacement and pressure maintenance test method for hydrogen storage tank of nuclear power station | |
CN203365409U (en) | Multi-flow-velocity corrosion measurement device of pipe conveyed medium | |
CN207586103U (en) | A kind of salt mist tester with salt fog processing function | |
CN110967259A (en) | High-flux external extrusion damage test device and method for metal pipe with defects | |
CN112710441B (en) | Ball valve air tightness anhydrous detection system and method | |
CN205449392U (en) | Sealed detection mechanism of ball valve that lead to more | |
CN110187067A (en) | A kind of water oxygen particle automatic analysis system and its analysis method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |