CN204882380U - Based on relevant tomoscan freeze -drying microscope of optics - Google Patents

Based on relevant tomoscan freeze -drying microscope of optics Download PDF

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Publication number
CN204882380U
CN204882380U CN201520502789.0U CN201520502789U CN204882380U CN 204882380 U CN204882380 U CN 204882380U CN 201520502789 U CN201520502789 U CN 201520502789U CN 204882380 U CN204882380 U CN 204882380U
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China
Prior art keywords
freeze
drying
optical coherence
coherence tomography
water condenser
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Expired - Fee Related
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CN201520502789.0U
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Chinese (zh)
Inventor
于颖
刘代春
何小荣
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China Pharmaceutical University
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China Pharmaceutical University
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Abstract

The utility model discloses a based on relevant tomoscan freeze -drying microscope of optics, including experiment type freeze dryer and the relevant tomoscan imaging system of optics, experiment type freeze dryer includes the freeze -drying case and catches water condenser, its characterized in that: the freeze -drying case with catch water condenser for split type, the freeze -drying case with catch water condenser and pass through electric butterfly valve and be connected, an observation window is offered to a freeze -drying case side, the relevant tomoscan imaging system of optics has been installed outward to the observation window of freeze -drying case. The utility model relates to a laboratory research freeze -drying mechanism and on -line monitoring's a master tool is controlled portably.

Description

Based on optical coherence tomography freeze-drying microscope
Technical field
The utility model relates generally to biology, medicine and optical field, particularly relates to a kind of freeze-drying microscope.
Background technology
In the vacuum freeze drying process of medicine, food and microorganism, the Measurement accuracy of temperature and pressure is most crucial to guarantee quality of item.Eutectic temperature, eutectic temperature, collapse temperature and glass transition temperature are the key temperatures parameter in freeze-drying process.Wherein, eutectic temperature, eutectic temperature and glass transition temperature mainly adopt differential scanning calorimeter (DSC) to measure.In the past, assessing collapse temperature by the glass transition temperature of dsc measurement goods, often there is certain error in this, especially when in goods, protein content is higher.At present, collapse temperature generally adopts freeze-drying measurement microscope.Freeze-drying microscope, as a laboratory tool of observing article construction change in freeze-drying process in microcosmic point, can be followed the tracks of distillation interface and do to observe for a long time, present widespread use be Transmission light type freeze-drying microscope.But because the goods of its observation are placed between two pieces of microslides, and be micro-, so there is notable difference with goods status in medicine bottle in suitability for industrialized production.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-(being generally 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 in the cryodesiccation chamber of objective table, and difficulty of processing greatly, keeps in repair inconvenience.
Utility model content
The technical problems to be solved in the utility model is: for the deficiencies in the prior art, there is provided 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 utility model by the following technical solutions:
A kind of based on optical coherence tomography freeze-drying microscope, comprise test-type freeze dryer and Optical coherence tomography system, described test-type freeze dryer comprises freeze drying box and catches water condenser, it is characterized in that: described freeze drying box is split type with catching water condenser, shelf (5-1) is provided with in described freeze drying box, described freeze drying box with catch water condenser and be connected by electric butterfly valve, described shelf adopts Resistant heating, a fan view window is offered in described freeze drying box one side, is equiped with Optical coherence tomography system outside the view window of described freeze drying box.
Further improvement as technique scheme:
Described freeze drying box is positioned at catches below water condenser, and described freeze drying box is connected support by corrosion resistant plate outside water condenser and becomes one overall with catching.
Described the superiors shelf is thermal compensation plate, described thermal compensation plate is equiped with tamponade screw rod, and adopts sylphon seal.
Described shelf laid inside has folding refrigeration piping, and in described refrigeration piping, flowing is liquid nitrogen.In described shelf, the outer both sides of refrigeration piping wall are all welded with resistive heater.In described shelf, refrigeration piping is imported and exported section and is equipped with temp probe, is equiped with the temp probe for measuring products temperature in vial in described freeze drying box.
Describedly catch in water condenser the refrigeration piping being equiped with and spiraling, in described refrigeration piping, flowing is liquid nitrogen.Describedly catch refrigeration coil inflow point in water condenser and be equiped with temp probe.Described freeze drying box is all equiped with vacuum gauge with catching in water condenser.
Described view window is opened in the adjacent side of freeze-drying chamber door, and described Optical coherence tomography system is arranged on outside described view window.
The sample handel of described Optical coherence tomography system is pressed close at view window outside surface, and adjustable height.
Described view window oil surface antireflecting coating.
Described shelf with catch water condenser inner refrigerant pipe outlet and be connected a pipeline and lead to view window outside surface, prevent view window outside surface from hazing and affecting observation.
Described optical coherence tomography system can monitor the freeze-drying of goods in one or more normal glass bottle.
Compared with prior art, the utility model has the advantage of:
1, of the present utility model based on optical coherence tomography freeze-drying microscope adopt liquid nitrogen directly freeze, environmentally safe, without the need to chilled water, and can obtain lower minimum temperature, and shorter lyophilization cycle.
2, of the present utility model 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 utility model 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 one-piece construction schematic diagram of the present utility model.
Fig. 2 is shelf partial enlarged drawing of the present utility model
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail.
As shown in Figure 1, of the present utility model based on optical coherence tomography freeze-drying microscope, freeze drying box (5) top is equiped with the tamponade screw rod (5-3) for driving shelf (5-1) and thermal compensation plate (5-2) to be elevated, and tamponade screw rod (5-3) adopts corrugated stainless steel tubing to seal.After freeze-drying terminates, vial (5-11) in false add plug-like state is on shelf (5-1), make shelf (5-1) and thermal compensation plate (5-2) carry out tamponade under the drive of guide pole (5-13), bolt (5-12) by rotating tamponade screw rod (5-3), bottle stopper is pressed in bottleneck completely.After tamponade completes, rotate tamponade screw rod (5-3) in the other direction and shelf (5-1) and thermal compensation plate (5-2) are set back.
The outer both sides of described shelf (5-1) interior refrigeration piping (3-1) wall are all welded with resistive heater (5-9), are close to shelf (5-1).
Described freeze drying box (5) and the liquid nitrogen import of catching water condenser (3) are connected to refrigeration piping (3-1 and 5-10) through expansion valve (3-3) respectively, the outlet of described liquid nitrogen container (1) is connected with expansion valve (3-3) through liquid nitrogen pump (2), the refrigeration piping (3-1 and 5-10) that liquid nitrogen directly flows through above-mentioned freeze drying box (5) and catches in water condenser (3) after expansion valve (3-3), controls cryogenic temperature by the rate of outflow controlling liquid nitrogen.
Described freeze drying box (5) and catch the low temperature nitrogen that water condenser (3) refrigeration piping (3-1 and 5-10) exports and lowered the temperature to view window (5-8) outside surface by connection one pipeline, is hazed or frosting to prevent its surface.
Described freeze drying box is connected with air strainer (5-6), aeration valve (5-4), micrometering valve (5-5) and vacuum gauge (3-4), described catching on water condenser (3) is connected with vacuum gauge (3-4), the import and export of described shelf (5-1) interior refrigeration piping (5-10) are equiped with temp probe (3-2) respectively, described water condenser (3) refrigeration coil (5-10) inflow point of catching is equiped with temp probe (3-2), multiple temp probe (3-2) is equiped with for measuring the temperature on vial (5-11) interior goods and shelf (5-1) surface in described freeze drying box.
Described outlet side of catching water condenser (3) connects vacuum pump (6) through small butterfly valve (6-1).
Described view window (5-8) adopts antireflection material to carry out coating, and for obtaining good scan depths and lateral resolution simultaneously, described optical coherence tomography system (7) adopts time domain type.
Described liquid nitrogen pump (2), vacuum pump (6), temp probe (3-2), vacuum gauge (3-4), in be connected with described PLC (10) respectively every valve (4), small butterfly valve (6-1), aeration valve (5-4), micrometering valve (5-5), expansion valve (3-3).
Described PLC (10) is connected through bidirectional transducer (9), address card (8) same to computing machine (11) with optical coherence tomography system (7).
The utility model freeze-drying monitoring facilities is:
1, the pre-freeze stage
Click on computers and open the utility model based on the microscopical supervisory system of optical coherence tomography freeze-drying, setting parameters of freeze-drying process, opens liquid nitrogen container, liquid nitrogen pump, expansion valve and optical coherence tomography system simultaneously.In goods pre-freeze process, the image generated by analyzing optical coherence tomography system 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 and the scope of catching water condenser design temperature, liquid nitrogen pump open and close manually or automatically can provide refrigerating capacity.
2, the lyophilization stage
When catching water condenser temperature and dropping to about-45 DEG C, open successively vacuum pump, small butterfly valve and in start to vacuumize every valve, the goods image generated by analyzing optical coherence tomography system determines its collapse temperature, guarantee that distillation heating-up temperature is lower than its collapse temperature, freeze drying box 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 needed, ensureing that goods are not burnt or suitably raise the temperature and pressure of freeze drying box under Denaturing, to make goods residual amount between 3% ~ 5%, carry out manual tamponade by tamponade screw rod.Then, close refrigeration system, vacuum system and imaging system successively, freeze-drying terminates.
The foregoing is only preferred embodiment of the present utility model, the change under concept of the present utility model, be all considered as protection category of the present utility model.

Claims (6)

1. one kind based on optical coherence tomography freeze-drying microscope, comprise test-type freeze dryer and Optical coherence tomography system (7), described test-type freeze dryer comprises freeze drying box (5) and catches water condenser (3), it is characterized in that: described freeze drying box (5) with catch water condenser (3) for split type, shelf (5-1) is provided with in described freeze drying box, described freeze drying box (5) with catch water condenser (3) and be connected by electric butterfly valve (4), a fan view window (5-8) is offered in described freeze drying box one side, Optical coherence tomography system (7) is equiped with outside the view window (5-8) 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 (5-10 and 3-1).
3. according to claim 2 based on optical coherence tomography freeze-drying microscope, it is characterized in that: in described refrigeration piping (5-10 and 3-1), flowing is liquid nitrogen.
4. according to claim 1 and 2 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described shelf (5-1) interior refrigeration piping (5-10) both sides are all welded with resistive heater (5-3).
5. according to claim 1 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 (5-10 with 3-1) endpiece and be connected a pipeline and lead to view window (5-8) outside surface.
6. according to claim 1 based on optical coherence tomography freeze-drying microscope, it is characterized in that: described view window (5-8) is opened in the adjacent side of freeze-drying chamber door, described Optical coherence tomography system (7) presses close to view window (5-8) outside.
CN201520502789.0U 2015-07-08 2015-07-08 Based on relevant tomoscan freeze -drying microscope of optics Expired - Fee Related CN204882380U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104931503A (en) * 2015-07-08 2015-09-23 中国药科大学 Freeze-drying microscope based on optical coherence tomography

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104931503A (en) * 2015-07-08 2015-09-23 中国药科大学 Freeze-drying microscope based on optical coherence tomography
CN104931503B (en) * 2015-07-08 2018-06-05 中国药科大学 Microscope is freezed based on optical coherence tomography

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Addressee: Yu Ying

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