CN104931503A - Freeze-drying microscope based on optical coherence tomography - Google Patents
Freeze-drying microscope based on optical coherence tomography Download PDFInfo
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- CN104931503A CN104931503A CN201510408046.1A CN201510408046A CN104931503A CN 104931503 A CN104931503 A CN 104931503A CN 201510408046 A CN201510408046 A CN 201510408046A CN 104931503 A CN104931503 A CN 104931503A
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- freeze
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Abstract
The invention discloses a freeze-drying microscope based on optical coherence tomography. The freeze-drying microscope based on the optical coherence tomography comprises an experimental type freeze-drying machine, an optical coherence tomography imaging system and a control system. The experimental type freeze-drying machine comprises a freeze-drying box, a water catching condenser and a liquid nitrogen container, wherein carrying plates used for carrying products are arranged in the freeze-drying box. The freeze-drying microscope is characterized in that the freeze-drying box is connected with the water catching condenser through an electric butterfly valve, the carrying plates are heated through resistance wires, guide rods and bolts are installed on the side faces of the carrying plates, an observation window is formed in one side face of the freeze-drying box, and the optical coherence tomography imaging system is arranged outside the observation window of the freeze-drying box. According to the freeze-drying microscope, the key temperature parameters of the products in small glass bottles are determined by generating 3D images of the freeze-dried products, and the freeze-drying microscope serves as a basic tool for researching the freeze-drying mechanism and carrying out online monitoring in a laboratory and is easy and convenient to control.
Description
Technical field
The present invention relates generally to a kind of based on optical coherence tomography freeze-drying microscope, is especially applied to medicine in vacuum freeze drying process, the 3D imaging of food and microorganism and key temperatures, pressure parameter and measures.
Background technology
In the vacuum freeze drying process of medicine, food profit microorganism, the Measurement accuracy of temperature and pressure is very crucial to guarantee quality of item.In the pre-freeze stage, the chilling temperature of goods need lower than its eutectic temperature T
eut; In the lyophilization stage, the heating-up temperature of goods need lower than its collapse temperature T
cor glass transition temperature T
g.These temperature are the key temperatures parameter in freeze-drying process.Wherein, eutectic temperature T
eutwith glass transition temperature T
gmain employing differential scanning calorimeter (DSC) and electric-resistivity method are measured, and collapse temperature T
cgeneral employing freeze-drying measurement microscope.The freeze-drying microscope generally applied at present is Transmission light type freeze-drying microscope, its imaging system is primarily of the optics of director's operating distance or the high-resolution video camera composition of electron microscope profit, testing sample two slides carry out film-making, then place in freeze-drying platform and carry out freeze drying.In whole freeze-drying process, the structure of goods changes camera being shot and records, for analyzing its key temperatures.The microscopical shortcoming of this freeze-drying is: 1, testing sample is placed between two slides, can not be used for the freeze-drying measuring goods in vial.2, testing sample is micro-(1 ~ 2 μ L), records the collapse temperature T of some goods
cwith T actual in vial
cthere is different.3, refrigeration is with heating module, liquid nitrogen are imported and exported, temperature and pressure transducer and vacuum orifice are installed on freeze-drying platform, and difficulty of processing greatly, keeps in repair inconvenience.
Summary of the invention
The technical problem to be solved in the present invention is: for the deficiencies in the prior art, provides one can follow the tracks of distillation interface, observe goods inner structure and generate 3D rendering and measure goods key temperatures parameter based on optical coherence tomography freeze-drying microscope.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of based on optical coherence tomography freeze-drying microscope, comprise test-type freeze dryer, Optical coherence tomography system and control system, described test-type freeze dryer comprises freeze drying box, catch water condenser and liquid nitrogen container, the shelf for placing goods is equiped with in described freeze drying box, it is characterized in that: described freeze drying box with catch water condenser and be connected by electric butterfly valve, described shelf adopts Resistant heating, described shelf side is equiped with guide pole profit bolt, a fan view window is offered in described freeze drying box one side, Optical coherence tomography system is equiped with outside the view window of described freeze drying box.
Further improvement as technique scheme:
Described test-type freeze dryer belongs to split type, described in catch water condenser and be positioned at below described freeze drying box, described freeze drying box is connected support by corrosion resistant plate outside water condenser and becomes one overall with catching.
Be provided with one block of thermal compensation plate above described shelf, described thermal compensation plate be equiped with tamponade screw rod, and adopt sylphon seal.
Be equiped with refrigerant tubing and resistive heater in described shelf, described shelf cold-producing medium entrance end is equiped with temp probe, is equiped with the temp probe for measuring products temperature in vial in described freeze drying box.
Described water condenser of catching is equiped with liquid nitrogen refrigerating coil pipe, and described liquid nitrogen refrigerating coil pipe inflow point is equiped with temp probe.
Described freeze drying box profit is caught in water condenser and is all equiped with vacuum gauge.
Described sample handel is arranged on outside view window, and described 3D rendering comprises structure and the ice-nucleus effect of pre-freeze stage articles, and the distillation of sublimation stage solvent is collapsed with the micro-of goods or subsided completely.
Described view window oil surface antireflecting coating.
Described optical coherence tomography system can monitor the freeze-drying of goods in one or more normal glass bottle, also can monitor the freeze-drying of goods between slide.
Compared with prior art, the invention has the advantages that:
1, of the present inventionly adopt liquid nitrogen directly to freeze based on optical coherence tomography freeze-drying microscope, lower minimum temperature can be obtained, and better refrigeration.
2, of the present invention is Noninvasive, undamaged monitoring means based on optical coherence tomography freeze-drying microscope, can monitor in vial or the freeze-drying process of goods between slide, generate 2D or the 3D rendering of goods, resolution is high, can measure the key temperatures parameter of freeze-drying process more accurately.
3, of the present invention based on the maintenance of optical coherence tomography freeze-drying microscope or to change component convenient, manipulation is simple.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention process chart.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
As shown in Figure 1, of the present invention based on optical coherence tomography freeze-drying microscope, in freeze drying box, shelf (5-1) has one or more layers, freeze drying box (5) top is equiped with the tamponade screw rod (5-5) for driving shelf (5-1) and thermal compensation plate (5-4) to be elevated, and tamponade screw rod (5-5) adopts corrugated stainless steel tubing to seal.After freeze-drying terminates, vial in false add plug-like state is on shelf (5-1), make shelf (5-1) and thermal compensation plate (5-4) carry out tamponade under the drive of guide pole, bolt by rotating tamponade screw rod (5-5), bottle stopper is pressed in bottleneck completely.After tamponade completes, rotate tamponade screw rod (5-5) in the other direction and shelf (5-1) and thermal compensation plate (5-4) are set back.
Resistance wire (5-3) in described shelf (5-1) is welded on inside shelf.
Described freeze drying box (5) and catch water condenser (3) share a set of refrigeration system, described freeze drying box (5) and the liquid nitrogen import of catching water condenser (3) are connected to refrigeration piping (5-2,3-4) through expansion valve (3-2) respectively, the outlet of described liquid nitrogen container (1) is connected with expansion valve (3-2) through liquid nitrogen pump (2), the refrigeration piping (5-2,3-4) that liquid nitrogen directly flows through above-mentioned freeze drying box (5) and catches in water condenser (3) after expansion valve (3-2), controls cryogenic temperature by the rate of outflow controlling liquid nitrogen.
The low temperature nitrogen that described freeze drying box (5) and the refrigeration piping (5-2,3-4) of catching water condenser (3) export lowers the temperature to prevent from hazing to view window (5-10) outside surface by connection one pipeline.
Described freeze drying box is connected with air strainer (5-8), aeration valve (5-6), micrometering valve (5-7) and vacuum gauge (3-3), described catching on water condenser (3) is connected with vacuum gauge (3-3), the import and export of described shelf (5-1) interior refrigeration piping (5-2) is equiped with temp probe (3-1) respectively, described water condenser (3) interior refrigeration piping (3-4) inflow point of catching is equiped with temp probe (3-1), 4 ~ 6 temp probes (3-1) are equiped with for measuring the temperature on goods and shelf (5-1) surface in vial in described freeze drying box (5).
Described outlet side of catching water condenser (3) connects vacuum pump (6) through small butterfly valve (6-1).
Described view window (5-10) adopts antireflection material to carry out coating, and described wideband light source (7-1) selects super-radiance light emitting diode.
Described liquid nitrogen pump (2), vacuum pump (6), temp probe (3-1), vacuum gauge (3-3), in be connected with described PLC (10) respectively every valve (4), small butterfly valve (6-1), aeration valve (5-6), micrometering valve (5-7), expansion valve (3-2).
Described PLC (10) sharp digital signal processing is connected through bidirectional transducer (9), address card (8) same to computing machine (11) with image reconstructor (7-12).
Freeze-drying monitoring facilities of the present invention is:
1, the pre-freeze stage
Click to open on computers and the present invention is based on the microscopical supervisory system of optical coherence tomography freeze-drying, setting parameters of freeze-drying process, opens liquid nitrogen container (1), liquid nitrogen pump (2), expansion valve (3-2) and optical coherence tomography system (7) simultaneously.The Solutions in Freeze-drying configured or suspension, according to its freeze-drying Property requirements, both first can put into freeze drying box (5) freezing again, put into freezing after lowering the temperature also can first to freeze drying box (5) again.In goods pre-freeze process, the image generated by analyzing optical coherence tomography system (7) determines its eutectic point (eutectic point) or glass transition temperature, after products temperature is lower than its eutectic point or eutectic point 10 ~ 20K, maintains 1 ~ 2h, then enters lyophilization.At whole freeze-drying process, according to freeze drying box (5) with catch the temperature range that water condenser (3) sets, liquid nitrogen pump open and close manually or automatically can provide refrigerating capacity.
2, the lyophilization stage
When catching water condenser (3) temperature and dropping to about-45 DEG C, open successively vacuum pump (6), small butterfly valve (6-1) and in start to vacuumize every valve (4), the goods image generated by analyzing Optical coherence tomography system (7) determines its collapse temperature, guarantee that distillation heating-up temperature is lower than its collapse temperature, freeze drying box (5) vacuumizes resulting pressure lower than water saturation vapour pressure at this temperature, judges when terminate lyophilization to enter parsing-desiccation by observation distillation interface or voltage rise test.
3, the parsing-desiccation stage
The free water of more than 90% was removed in the lyophilization stage, now need ensureing that goods are not burnt or suitably raise the temperature and pressure of freeze drying box under Denaturing, make goods residual amount between 3% ~ 5%, carry out manual tamponade by tamponade screw rod (5-5).Then, close liquid nitrogen pump (2), liquid nitrogen container (1), small butterfly valve (6-1), vacuum pump (6) and Optical coherence tomography system (7) successively, open aeration valve (5-6) to make freeze drying box (5) and catch water condenser (3) to recover atmospheric pressure, freeze-drying terminates.
The foregoing is only the preferred embodiments of the present invention, structure change under the principles of the present invention and modification, all should belong to protection category of the present invention.
Claims (8)
1. one kind based on optical coherence tomography freeze-drying microscope, comprise test-type freeze dryer, Optical coherence tomography system (7) and control system, described test-type freeze dryer comprises freeze drying box (5), catch water condenser (3) and liquid nitrogen container (1), the shelf (5-1) for placing goods is provided with in described freeze drying box, it is characterized in that: described freeze drying box (5) with catch water condenser (3) and be connected by electric butterfly valve (4), described shelf (5-1) adopts resistance wire (5-3) to heat, described shelf (5-1) side is provided with guide pole and bolt, a fan view window (5-10) is offered in described freeze drying box one side, Optical coherence tomography system (7) is equiped with outside the view window (5-10) of described freeze drying box (5).
2. according to claim 1 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described shelf (5-1) and catch in water condenser (3) and be equiped with refrigeration piping.
3. according to claim 2 based on optical coherence tomography freeze-drying microscope, it is characterized in that: the interior refrigeration piping both sides of described shelf (5-1) are equiped with resistive heater (5-3), described shelf (5-1) with catch water condenser (3) interior refrigeration piping (5-2,3-4) entrance point and be connected with liquid nitrogen pump (2) endpiece through expansion valve (3-2).
4. according to claim 1 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described shelf (5-1) side is provided with guide pole and bolt and is connected by each shelf (5-1,5-4) and is elevated.
5. according to claim 1 and 2 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described shelf (5-1) with catch water condenser (3) interior refrigeration piping (5-2,3-4) endpiece and be connected a pipeline and lead to view window (5-10) outside surface.
6. according to claim 3 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described liquid nitrogen pump (2) entrance point connects liquid nitrogen container (1).
7. according to claim 1 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described Optical coherence tomography system (7) comprises wideband light source (7-1), sample handel (7-4), with reference to handel (7-3), spectroscope (7-5), collimation lens (7-2), light beam speed reduction unit (7-6), photodetector (7-7), signal amplifier (7-8), bandpass filtering (7-9), detuner (7-10), A/D modular converter (7-11), digital signal processing and image reconstructor (7-12).
8. according to claim 1 or 7 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described view window (5-10) is opened in the adjacent side of freeze-drying chamber door, described sample handel (7-4) presses close to view window (5-10) outside.
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| CN201510408046.1A CN104931503B (en) | 2015-07-08 | 2015-07-08 | Microscope is freezed based on optical coherence tomography |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109490243A (en) * | 2018-12-29 | 2019-03-19 | 深圳职业技术学院 | The system and monitoring method of material appearance during on-line monitoring microwave freeze-drying |
| CN112419395A (en) * | 2020-11-24 | 2021-02-26 | 上海理工大学 | Method for determining collapse temperature of freeze-dried material by using image processing technology |
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| DE19504392A1 (en) * | 1994-03-08 | 1996-01-04 | Wurzer Harald | In situ microscope observation of water samples |
| CN1731159A (en) * | 2005-08-02 | 2006-02-08 | 中国海洋大学 | Device for performing visualized real-time monitoring on chemical liquid under high-temperature and high-voltage environment |
| US20150063406A1 (en) * | 2011-05-17 | 2015-03-05 | Physical Sciences, Inc. | Optical Coherence Tomography (OCT) Freeze Drying Microscopy |
| CN204882380U (en) * | 2015-07-08 | 2015-12-16 | 中国药科大学 | Based on relevant tomoscan freeze -drying microscope of optics |
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2015
- 2015-07-08 CN CN201510408046.1A patent/CN104931503B/en not_active Expired - Fee Related
Patent Citations (4)
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| DE19504392A1 (en) * | 1994-03-08 | 1996-01-04 | Wurzer Harald | In situ microscope observation of water samples |
| CN1731159A (en) * | 2005-08-02 | 2006-02-08 | 中国海洋大学 | Device for performing visualized real-time monitoring on chemical liquid under high-temperature and high-voltage environment |
| US20150063406A1 (en) * | 2011-05-17 | 2015-03-05 | Physical Sciences, Inc. | Optical Coherence Tomography (OCT) Freeze Drying Microscopy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109490243A (en) * | 2018-12-29 | 2019-03-19 | 深圳职业技术学院 | The system and monitoring method of material appearance during on-line monitoring microwave freeze-drying |
| CN112419395A (en) * | 2020-11-24 | 2021-02-26 | 上海理工大学 | Method for determining collapse temperature of freeze-dried material by using image processing technology |
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| CN104931503B (en) | 2018-06-05 |
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