CN112362254A - Freeze dryer silicone oil leakage monitoring mass spectrometer system based on Internet of things and monitoring method - Google Patents
Freeze dryer silicone oil leakage monitoring mass spectrometer system based on Internet of things and monitoring method Download PDFInfo
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- CN112362254A CN112362254A CN202011241387.1A CN202011241387A CN112362254A CN 112362254 A CN112362254 A CN 112362254A CN 202011241387 A CN202011241387 A CN 202011241387A CN 112362254 A CN112362254 A CN 112362254A
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- silicone oil
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- 238000012544 monitoring process Methods 0.000 title claims abstract description 42
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 17
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 230000003993 interaction Effects 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 3
- 238000001514 detection method Methods 0.000 claims description 14
- 230000000007 visual effect Effects 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000013079 data visualisation Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 239000003921 oil Substances 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 6
- 235000013305 food Nutrition 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229940079593 drug Drugs 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000012792 lyophilization process Methods 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000825 pharmaceutical preparation Substances 0.000 description 2
- 229940127557 pharmaceutical product Drugs 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
- G01M3/202—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material using mass spectrometer detection systems
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
- G01M3/202—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material using mass spectrometer detection systems
- G01M3/205—Accessories or associated equipment; Pump constructions
Abstract
The invention provides a freeze dryer silicone oil leakage monitoring mass spectrometer system and a monitoring method based on the Internet of things, wherein the freeze dryer silicone oil leakage monitoring mass spectrometer system comprises a monitoring center, a mass spectrometer and a plurality of wireless transceivers; the mass spectrometer is connected with the wireless transceiver to form a monitoring end, and the monitoring end is connected with the control center through a network and performs information interaction with the control center through the network; the mass spectrometer comprises a quadrupole mass analyzer, an ionization source and a data acquisition system; the ionization source is for ionizing a leakage species into ions that are captured or transmitted by the quadrupolar mass analyzer; the data acquisition system is used to collect ion signals after processing by the quadrupole mass analyzer. The invention connects each monitoring mass spectrometer to the control center through the wireless network, so that an operator can check the states of all the devices in the monitoring center in real time, and when the devices are changed, the network wiring is not needed, thereby reducing the cost.
Description
Technical Field
The invention relates to the technical field of mass spectrum monitoring, in particular to a freeze dryer silicone oil leakage monitoring mass spectrometer system and a monitoring method based on the Internet of things.
Background
The vacuum freeze-drying technique (hereinafter referred to as freeze-drying technique) is a technique of freezing a water-containing material at a low temperature and then sublimating water in the water-containing material directly in a vacuum state without passing through a liquid state. The physical, chemical and form of the material dried by the technology are basically unchanged, the loss of effective components is small, the rehydration performance is good, and the sealing and storage period is long. The freeze-drying technology has wide application, and especially plays an important role in the field of biological pharmacy.
With the continuous improvement of living standard, the environmental protection consciousness and health consciousness of the social public are further enhanced, people put forward higher requirements on the quality of consumer products, and the requirements on various medicines, health care products and freeze-dried foods are increased. The increasing demand for preparing various medicines, biological health products, freeze-dried foods, solid micro-powder and the like can strongly promote the further development of the freeze-drying technology, so that the application scale of the freeze-drying technology is continuously enlarged and the application field is continuously expanded.
The apparatuses for implementing the lyophilization technique are called lyophilizers, and generally speaking, the lyophilizers are composed of a lyophilization chamber, a vacuum system, a refrigeration system and a control system. The freeze-drying box is the main part of freeze dryer, and the freezing and drying of material are accomplished in the freeze-drying box, if be mixed with impurity in the freeze-drying box, the quality of freeze-dried food or medicine will be influenced, therefore the clean degree of freeze-drying box directly influences the quality of material after the freeze-drying. Further, if the food or the pharmaceutical product is not found due to the inclusion of impurities during the lyophilization process, once the food or the pharmaceutical product is taken/eaten as a qualified product and enters the human body, the human health is likely to be affected unpredictably, and therefore, the detection of the impurities during the lyophilization process becomes a focus of attention. The leaked silicone oil in the freeze-drying box is a main source of impurities, so that the real-time online detection of the leaked silicone oil in the freeze-drying machine has important significance for ensuring the quality of freeze-dried products.
Spectroscopic, chromatographic, sensor and mass spectrometric methods can all be used for the detection of silicone oil leaks. The spectrum and the sensor are not high in specificity, only specific target substances can be detected, the detection limit is insufficient, and quantitative analysis cannot be carried out. The detection method of the chromatogram can carry out quantitative analysis on the substances to be detected, but the detection period is too long. The silicon oil in the freeze dryer is mainly used for heat conduction, and the time, content and position of the silicon oil leakage are random, so that the spectrum, sensor and chromatographic methods cannot meet the requirement of on-site real-time online detection of the silicon oil leakage in the freeze dryer.
The mass spectrometry is one of important methods in the detection field, can qualitatively and quantitatively analyze complex compounds, can realize in-situ second-level response detection, and becomes a novel method for detecting silicone oil leakage.
Because the freeze dryer is more in the factory building, and the volume is great, all disposes silicon oil leakage monitoring mass spectrograph on every freeze dryer, this leads to the operator to need constantly to patrol the mass spectrograph monitoring state in the factory building, consumes a large amount of physical power and energy. If a wired network is used, the wiring is complicated and costly, and the replacement and movement of the equipment increases the maintenance cost.
Patent document CN105784289A (application number: CN201610223705.9) discloses a method for judging silicone oil leakage in a freeze dryer and an end point of primary sublimation drying, wherein a mass spectrometer is used for online scanning of a freeze drying process, and if (C2H6SiO) n with a molecular weight of 73 is detected in a freeze drying chamber to obviously increase, the fact that the freeze dryer has silicone oil leakage can be judged; if the proportion of each component in the air in the freeze-drying room is equal to that in the no-load operation, judging that the primary sublimation drying is finished; and otherwise, continuing drying until the drying is equivalent to the idle time, and finishing primary drying.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a freeze dryer silicon oil leakage monitoring mass spectrometer system and a monitoring method based on the Internet of things.
The freeze dryer silicone oil leakage monitoring mass spectrometer system based on the Internet of things comprises a monitoring center, a mass spectrometer and a plurality of wireless transceivers;
the mass spectrometer is connected with the wireless transceiver to form a monitoring end, and the monitoring end is connected with the control center through a network and performs information interaction with the control center through the network;
the mass spectrometer comprises a quadrupole mass analyzer, an ionization source and a data acquisition system;
the ionization source is for ionizing a leakage species into ions that are captured or transmitted by the quadrupolar mass analyzer;
the data acquisition system is used to collect ion signals after processing by the quadrupole mass analyzer.
Preferably, the mass spectrometer further comprises a vacuum holding device and a vacuum detection device;
the quadrupole mass analyzer is positioned in the vacuum cavity of the mass spectrometer and is connected with the vacuum cavity;
the vacuum holding apparatus and vacuum detection apparatus are used to maintain the operating gas pressure of the quadrupole mass analyzer.
Preferably, the monitoring center comprises a computer system and an audible and visual alarm;
the computer system comprises a computer, a monitor, a keyboard and a mouse, a storage device and a network router;
the monitor is connected with the computer and used for providing data visualization and a human-computer interaction interface;
the keyboard and the mouse are connected with the computer and used for providing control instruction input;
the storage device is connected with the computer and used for storing and reading data;
the computer system is connected with the wireless transceiver through a network cable or a network router, and is connected with the audible and visual alarm through an 485/232 interface.
Preferably, the wireless transceiver is a zigbee wireless transceiver;
the wireless network is a zigbee network.
Preferably, the mass spectrometer is a silicon oil leakage monitoring sensor, and the sample injection part of the mass spectrometer is connected with the vacuum cavity of the freeze dryer.
The freeze dryer silicone oil leakage monitoring method based on the Internet of things comprises the following steps:
step 1: running an application program deployed on a computer of a monitoring center, connecting to a wireless network through a wireless transceiver, and acquiring the states of other wireless transceivers on the wireless network;
step 2: starting a mass spectrometer connected to the freeze dryer, and connecting a mass spectrometer control program to a wireless network through a wireless transceiver;
and step 3: setting parameters of a target mass spectrometer and starting monitoring through an application program deployed on a computer in a monitoring center;
and 4, step 4: an application program on a computer of the monitoring center inquires the running state of the mass spectrometer in a zigbee network through a wireless transceiver installed on the mass spectrometer;
and 5: when the mass spectrometer detects that the silicone oil leaks, setting the self state as an alarm state;
step 6: and when monitoring the alarm state of the mass spectrometer in the zigbee network, an application program on the computer of the monitoring center identifies an alarm on the monitor and starts an audible and visual alarm.
Compared with the prior art, the invention has the following beneficial effects: the invention connects each monitoring mass spectrometer to the control center through the wireless network, so that an operator can check the states of all the devices in the monitoring center in real time, and when the devices are changed, the network wiring is not needed, thereby reducing the cost.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic diagram of the system of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example (b):
referring to fig. 1, the present invention provides a technical solution: comprises a monitoring center, at least one mass spectrometer and a wireless transceiver.
Step 1, running an application program deployed on a computer of a monitoring center, connecting to a wireless network through a wireless transceiver, and acquiring states of other wireless transceivers on the wireless network.
Wherein, the monitoring center comprises a computer system, a wireless transceiver and an audible and visual alarm. The computer system may include a computer, a monitor, a keyboard, a storage device, a network router.
Wherein, the wireless transceiver is a zigbee wireless transceiver.
Wherein the wireless network is a zigbee network.
And 2, starting a mass spectrometer connected to the freeze dryer, and connecting a mass spectrometer control program to a wireless network through a wireless transceiver.
The mass spectrometer comprises a quadrupole mass analyzer, an ionization source, a vacuum holding device, a vacuum detection device, a solenoid valve and a data acquisition system.
The mass spectrometer is used as a silicon oil leakage monitoring sensor, and the sample injection part of the mass spectrometer is connected with the vacuum cavity of the freeze dryer.
Wherein, the wireless transceiver is a zigbee wireless transceiver.
Wherein the wireless network is a zigbee network.
And 3, setting parameters of the target mass spectrometer and starting monitoring by monitoring personnel in the monitoring center through an application program deployed on a computer, and also directly setting starting monitoring on the mass spectrometer.
And 4, continuously inquiring the running state of the mass spectrometer by the application program on the monitoring center computer through the wireless transceiver installed on the mass spectrometer in the zigbee network.
And 5, once the mass spectrometer detects the leakage of the silicon oil, setting the self state as an alarm state.
And 6, monitoring the alarm state of the mass spectrometer in the zigbee network by an application program on the computer of the monitoring center, identifying an alarm on the monitor and starting an audible and visual alarm.
Those skilled in the art will appreciate that, in addition to implementing the systems, apparatus, and various modules thereof provided by the present invention in purely computer readable program code, the same procedures can be implemented entirely by logically programming method steps such that the systems, apparatus, and various modules thereof are provided in the form of logic gates, switches, application specific integrated circuits, programmable logic controllers, embedded microcontrollers and the like. Therefore, the system, the device and the modules thereof provided by the present invention can be considered as a hardware component, and the modules included in the system, the device and the modules thereof for implementing various programs can also be considered as structures in the hardware component; modules for performing various functions may also be considered to be both software programs for performing the methods and structures within hardware components.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (6)
1. A freeze dryer silicone oil leakage monitoring mass spectrometer system based on the Internet of things is characterized by comprising a monitoring center, a mass spectrometer and a plurality of wireless transceivers;
the mass spectrometer is connected with the wireless transceiver to form a monitoring end, and the monitoring end is connected with the control center through a network and performs information interaction with the control center through the network;
the mass spectrometer comprises a quadrupole mass analyzer, an ionization source and a data acquisition system;
the ionization source is for ionizing a leakage species into ions that are captured or transmitted by the quadrupolar mass analyzer;
the data acquisition system is used to collect ion signals after processing by the quadrupole mass analyzer.
2. The Internet of things-based lyophilizer silicone oil leakage monitoring mass spectrometer system of claim 1, characterized in that said mass spectrometer further comprises a vacuum holding device and a vacuum detection device;
the quadrupole mass analyzer is positioned in the vacuum cavity of the mass spectrometer and is connected with the vacuum cavity;
the vacuum holding apparatus and vacuum detection apparatus are used to maintain the operating gas pressure of the quadrupole mass analyzer.
3. The Internet of things-based lyophilizer silicone oil leakage monitoring mass spectrometer system of claim 1, characterized in that said monitoring center comprises a computer system and an audible and visual alarm;
the computer system comprises a computer, a monitor, a keyboard and a mouse, a storage device and a network router;
the monitor is connected with the computer and used for providing data visualization and a human-computer interaction interface;
the keyboard and the mouse are connected with the computer and used for providing control instruction input;
the storage device is connected with the computer and used for storing and reading data;
the computer system is connected with the wireless transceiver through a network cable or a network router, and is connected with the audible and visual alarm through an 485/232 interface.
4. The Internet of things-based lyophilizer silicone oil leakage monitoring mass spectrometer system of claim 1, characterized in that said wireless transceiver is a zigbee wireless transceiver;
the wireless network is a zigbee network.
5. The Internet of things-based lyophilizer silicone oil leakage monitoring mass spectrometer system of claim 1, characterized in that, the mass spectrometer is a silicone oil leakage monitoring sensor, and the sample injection part of the mass spectrometer is connected with the lyophilizer vacuum cavity.
6. An internet of things-based lyophilizer silicone oil leakage monitoring method, characterized in that, the internet of things-based lyophilizer silicone oil leakage monitoring mass spectrometer system of any one or more of claims 1-5 is adopted, comprising:
step 1: running an application program deployed on a computer of a monitoring center, connecting to a wireless network through a wireless transceiver, and acquiring the states of other wireless transceivers on the wireless network;
step 2: starting a mass spectrometer connected to the freeze dryer, and connecting a mass spectrometer control program to a wireless network through a wireless transceiver;
and step 3: setting parameters of a target mass spectrometer and starting monitoring through an application program deployed on a computer in a monitoring center;
and 4, step 4: an application program on a computer of the monitoring center inquires the running state of the mass spectrometer in a zigbee network through a wireless transceiver installed on the mass spectrometer;
and 5: when the mass spectrometer detects that the silicone oil leaks, setting the self state as an alarm state;
step 6: and when monitoring the alarm state of the mass spectrometer in the zigbee network, an application program on the computer of the monitoring center identifies an alarm on the monitor and starts an audible and visual alarm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011241387.1A CN112362254A (en) | 2020-11-09 | 2020-11-09 | Freeze dryer silicone oil leakage monitoring mass spectrometer system based on Internet of things and monitoring method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011241387.1A CN112362254A (en) | 2020-11-09 | 2020-11-09 | Freeze dryer silicone oil leakage monitoring mass spectrometer system based on Internet of things and monitoring method |
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| CN112362254A true CN112362254A (en) | 2021-02-12 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011078835A1 (en) * | 2009-12-22 | 2011-06-30 | Ima Life North America Inc. | Monitoring freeze drying with gas measurement on vaccum pump exhaust |
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| CN105757465A (en) * | 2016-04-25 | 2016-07-13 | 华东交通大学 | Valve inner leakage wireless networking real-time detecting device |
| CN110648895A (en) * | 2019-08-16 | 2020-01-03 | 上海裕达实业有限公司 | Mass spectrum device and method for detecting silicone oil leakage in freeze-drying process |
-
2020
- 2020-11-09 CN CN202011241387.1A patent/CN112362254A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011078835A1 (en) * | 2009-12-22 | 2011-06-30 | Ima Life North America Inc. | Monitoring freeze drying with gas measurement on vaccum pump exhaust |
| CN202634488U (en) * | 2012-06-01 | 2012-12-26 | 广州市启铭星科技有限公司 | Gas leakage accident early-warning monitoring system based on internet of things |
| CN204536807U (en) * | 2015-03-17 | 2015-08-05 | 四川智联正邦信息技术有限公司 | Based on the gas numerical potential policing services plateform system of technology of Internet of things |
| CN105757465A (en) * | 2016-04-25 | 2016-07-13 | 华东交通大学 | Valve inner leakage wireless networking real-time detecting device |
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Non-Patent Citations (2)
| Title |
|---|
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Application publication date: 20210212 |