CN103163011B - Vacuum liquid refrigeration sampling device - Google Patents
Vacuum liquid refrigeration sampling device Download PDFInfo
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- CN103163011B CN103163011B CN201110427065.0A CN201110427065A CN103163011B CN 103163011 B CN103163011 B CN 103163011B CN 201110427065 A CN201110427065 A CN 201110427065A CN 103163011 B CN103163011 B CN 103163011B
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- cold
- trap
- vacuum chamber
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Abstract
The invention discloses a vacuum liquid refrigeration sampling device. The device refrigerates liquid sprayed into a vacuum chamber through low temperature, and the situation that evaporation of the liquid breaks vacuum of the vacuum chamber is avoided. The device mainly comprises the vacuum chamber, a capillary pipe, an air exhaust system, a cold trap and a liquid analysis zone. After a liquid sample is sprayed into the vacuum chamber through the capillary pipe, the liquid sample moves downward to penetrate through a small hole in an upper cover of the cold trap and then enters a refrigerating chamber to be refrigerated. The vacuum liquid refrigeration sampling device has the advantages that under the vacuum condition, liquid jets can be directly analyzed. Meanwhile, the vacuum can be maintained 1*10-5Pa-1*10-2Pa, the cost is low and disassembly is convenient.
Description
Technical field
The present invention relates generally to technical field of vacuum, particularly needs liquid direct, the vacuum chamber higher to vacuum level requirements, and the direct research to liquid surface.
Background technology
Along with the development of vacuum technique, under vacuum, gas or solid sample analyzed and study more and more general.Time under atmospheric pressure environment to the research of liquid surface character, be always subject to the interference of air, only have under vacuo, could really liquid surface character be studied.But be but faced with a lot of challenges to the Direct Analysis of fluid sample, wherein, the maintenance of chamber pressure is a difficult problem always.When analyzing gaseous sample and solid sample, the sample size of gas is less, little on the pressure impact in vacuum chamber; The vapour pressure of solid sample is less, also very little on the pressure impact in vacuum chamber.When liquid enters vacuum chamber, first liquid gasify as gas, because the volume after the liquid gasification of 1mL is by expansion about 1000 times, causes great destruction to the vacuum tightness of whole vacuum chamber.Fluid sample Direct Analysis in a vacuum mainly contains two kinds of approach, and a kind of is adopt the number increasing high molecular pump, improves molecular pump pumping speed.Adopt differential technique, gas (becoming after liquid gasification) is directly extracted into outside vacuum chamber.Another kind utilizes cold-trap by the liquid freezing of vacuum chamber, and the liquid after freezing is because gasification is not little on pressure in vacuum tank impact.Although the former is feasible, the pump that this method needs is many, with high costs, and the general cold-trap that adopts freezing by liquid beam more.
But carry out freezing to fluid sample due to needs, the temperature of cold-trap is at-20 ~-100 degrees Celsius, and the sealing effectiveness that can enclose the seal member O of vacuum chamber produces and destroys greatly.If be directly welded on the cavity of vacuum chamber by cold-trap, although can solve the impact of cold-trap low temperature on sealing, processing technology is complicated, and disassembly, cleaning are very inconvenient.
According to above shortcoming, we devise a kind of vacuum liquid refrigeration device, for the direct injected of liquid under time limit vacuum condition.In order to overcome the impact of cold-trap low temperature on the sealing of O circle, we have employed the distance of roundabout folding structure to prolong liquid freezing room and O circle, with the addition of cold scattering piece simultaneously.Reduce the impact of liquid freezing room low temperature on the sealing of O circle.
Summary of the invention
The object of the present invention is to provide a kind of vacuum liquid refrigeration device, its effect is the vacuum direct injected realizing liquid, and utilize cold-trap by directly freezing for the fluid sample entered in vacuum, the pressure of vacuum chamber maintains 1 × 10
-5pa ~ 1 × 10
-2pa.
For achieving the above object, the technical solution used in the present invention is:
A kind of vacuum liquid refrigeration sampling device, comprises vacuum chamber, kapillary, exhaust system, cold-trap and fluid analysis district;
Described kapillary one end is connected with extraneous liquid source, and the other end stretches in vacuum chamber, and the capillary outlet stretched in vacuum chamber is placed in directly over cold-trap; The wall of vacuum chamber (1) is provided with the exhausr port be connected with molecular pump.
Described cold-trap is arranged at below vacuum chamber, and cold-trap and vacuum chamber are enclosed by O and seal; Cold-trap comprises liquid nitrogen storage tank, the freezing axle of cylindrical metal and refrigerating chamber.Freezing axle is arranged at refrigerating chamber lower end, and its one end is amplexiformed mutually with refrigerating chamber lower surface, and the other end of freezing axle stretches in liquid nitrogen storage tank;
Described refrigerating chamber upper end open is connected by back taper aperture with vacuum chamber, and lower end is airtight to be threaded connection with the freezing axle of cylindrical metal.The upper end open place of refrigerating chamber is provided with cold-trap top cover, is provided with a back taper aperture in the middle part of cold-trap top cover; Capillary outlet is placed in directly over the back taper entrance of cold-trap top cover, leaves space between capillary outlet and back taper aperture, forms fluid analysis district;
The edge, upper end of described refrigerating chamber is outwards up and down reciprocatingly roundabout folding, formed coaxial with refrigerating chamber more than 1, ring cavity that the one end open other end is airtight; The outer wall of outermost layer ring cavity extends to form a flange, and flange is provided with annular recess, is provided with O circle in annular recess; Cold-trap is sealed with the cavity wall of vacuum chamber mutually by O circle.
The sidewall of described vacuum chamber is symmetrically arranged with two optical windows, two optical windows and fluid analysis district are on same axis; One optical window is as light source entrance, and another optical window is as the outlet of light source;
In described vacuum chamber, place of fluid analysis district is provided with photo-detector, photo-detector is connected with outside signal analyzer by wire; Or in vacuum chamber, place of fluid analysis district being provided with ion detector, ion detector is connected with outside signal analyzer by wire;
Described capillary outlet place is coaxial with the back taper entrance on cold-trap top cover.Liquid sprays from capillary outlet, enters in refrigerating chamber through back taper entrance.Cold-trap lid is connected by screw thread with refrigerating chamber.
Described liquid beam is directly injected to vacuum enclosure by kapillary, and capillary diameter is between 0.01 ~ 0.2mm, and the distance of capillary outlet distance cold-trap upper cover is 0.5 ~ 200mm.
The outer wall of the roundabout folding outermost layer ring cavity of described refrigerating chamber is provided with metal cold scattering piece.The outer wall of the roundabout folding outermost layer ring cavity of refrigerating chamber is provided with temperature sensor.Temperature sensor is connected with warning device by wire.
The described ring cavity opening part be connected with ambient atmosphere is provided with thermal insulation material.Enter in the ring cavity be connected with ambient atmosphere for stoping water vapor and condensation occurs.
Compared with prior art, the advantage had and the beneficial effect of generation are in the present invention:
1. liquid can direct injected, and chamber pressure easily controls 1 × 10
-5pa ~ 1 × 10
-2pa.
2. cold-trap head temperature-20 ~-150 degrees Celsius, can cool preferably to liquid beam.
3. convenient disassembly.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of vacuum liquid refrigeration device: 1-vacuum chamber; 2-kapillary; 3-exhaust system; 4-cold-trap; 5-fluid analysis district;
Fig. 2 is the schematic diagram of cold-trap: 6-cold-trap upper cover; 7-cold-trap aperture; 8-O encloses; 9-refrigerating chamber; 10-liquid nitrogen; 11-freezing axle; 12-temperature sensor; 13-warning device; 14-cold scattering piece; 15-flange; 16-ring cavity the opening that is connected with ambient atmosphere; 17-thermal insulation material.
Embodiment
The present invention is used for the direct vacuum sample introduction of fluid sample, and fluid sample sprays in vacuum chamber 1 through kapillary 2.The liquid part spraying into vacuum chamber 1 evaporates into gas, is discharged to outside vacuum chamber by the molecular pump of exhaust system 3, and most of liquid is entered in cold-trap by the back taper aperture 7 of cold-trap 4 upper end.Being in kapillary 2 region exported between cold-trap 4 upper end is fluid analysis district 5.
As shown in Figure 1, one end of the freezing axle 11 of metal is directly inserted in liquid nitrogen 10, and the other end is connected by screw thread with liquid freezing room 9.The low temperature of liquid nitrogen is delivered to liquid freezing room 9 and cold-trap upper cover 6 by freezing axle 11.Cold-trap upper cover 6 is connected by screw thread with liquid freezing room 9.Whole cold-trap 4 is connected with vacuum chamber 1 and extrudes O by gib screw and enclose 8 and seal.
The edge, upper end of refrigerating chamber 9 is outwards up and down reciprocatingly roundabout folding, formed coaxial with refrigerating chamber 9 more than 1, ring cavity that the one end open other end is airtight; The outer wall of outermost layer ring cavity extends to form a flange 15, and on flange, 15 are provided with annular recess, is provided with O circle 8 in annular recess; Cold-trap is sealed with the cavity wall of vacuum chamber 1 mutually by O circle 8.
Liquid freezing room 9 apart between O circle 8 by up and down reciprocatingly roundabout foldable structure, effectively extend distance between the two, reduce the impacts of liquid freezing room 9 on O circle 8 sealing.Liquid freezing room 9 separates with a hole of vacuum chamber cold-trap top cover, and the size in hole is at 0.1 ~ 5cm.
Around cold-trap, with the addition of cold scattering piece 14, improve the temperature of cold-trap wall.Be added with thermal insulation material 17 around the ring cavity opening 16 be connected with ambient atmosphere, enter cooling on wall for stoping water vapor and freeze.
Liquid enters vacuum chamber 1 by kapillary 2, after moving downward the distance of 0.1 ~ 20cm, arrives liquid freezing room 9 by the aperture 7 of the upper end cover 6 of cold-trap 4 in vacuum chamber 1.The temperature of refrigerating chamber 9 reaches-20 ~-150 degrees Celsius, by the liquid quick freeze entered, thus prevents liquid gasification from causing pressure in vacuum tank to raise.
In practical operation, first, under atmospheric pressure, carry out liquid beam sample introduction, guarantee calm upper cover 6 aperture 7 be positioned at immediately below kapillary 2, liquid beam can be entered in cold-trap 4 by the aperture 7 of top cover upper end.Then, stop kapillary 2 sample introduction, open exhaust system 3.Finally, when vacuum tightness reaches requirement of experiment, add liquid nitrogen, carry out capillary liquid direct injected.When closing instrument, first stop kapillary 2 sample introduction, then close vacuum system.Finally remove cold-trap 4, freezing liquid takes out by dismounting cold-trap.
Claims (7)
1. a vacuum liquid refrigeration sampling device, is characterized in that comprising: vacuum chamber (1), kapillary (2), exhaust system (3), cold-trap (4) and fluid analysis district (5);
Kapillary (2) one end is connected with extraneous liquid source, and the other end stretches in vacuum chamber (1), and kapillary (2) outlet stretched in vacuum chamber (1) is placed in directly over cold-trap (4);
Cold-trap (4) is arranged at vacuum chamber (1) below, and cold-trap (4) and vacuum chamber (1) enclose (8) by O and seal; Cold-trap (4) comprises liquid nitrogen storage tank (10), the freezing axle of cylindrical metal (11) and refrigerating chamber (9); Freezing axle (11) is arranged at refrigerating chamber (9) lower end, and its one end is amplexiformed mutually with refrigerating chamber (9) lower surface, and the other end of freezing axle (11) stretches in liquid nitrogen (10) storage tank;
Refrigerating chamber (9) upper end open is connected by back taper aperture (7) with vacuum chamber (1), and lower end is airtight to be threaded connection with the freezing axle of cylindrical metal (11);
The upper end open place of refrigerating chamber (9) is provided with cold-trap top cover (6), and cold-trap top cover (6) middle part is provided with a back taper aperture (7); Kapillary (2) outlet is placed in directly over the back taper entrance of cold-trap top cover (6), leaves space, form fluid analysis district (5) between kapillary (2) outlet and back taper aperture (7);
The edge, upper end of refrigerating chamber (9) is outwards up and down reciprocatingly roundabout folding, formed coaxial with refrigerating chamber (9) more than 1, ring cavity that the one end open other end is airtight; The outer wall of outermost layer ring cavity extends to form a flange (15), and flange (15) is provided with annular recess, is provided with O circle (8) in annular recess; Cold-trap (4) is sealed with the cavity wall of vacuum chamber (1) mutually by O circle;
The wall of vacuum chamber (1) is provided with the exhausr port be connected with molecular pump (3);
The outer wall of the roundabout folding outermost layer ring cavity of refrigerating chamber (9) is provided with metal cold scattering piece (14).
2. device according to claim 1, is characterized in that:
The sidewall of vacuum chamber (1) is symmetrically arranged with two optical windows, two optical windows and fluid analysis district (5) are on same axis; One optical window is as light source entrance, and another optical window is as the outlet of light source.
3. device according to claim 2, is characterized in that:
In vacuum chamber (1), fluid analysis district (5) place is provided with photo-detector, photo-detector is connected with outside signal analyzer by wire; Or in vacuum chamber (1), fluid analysis district (5) place being provided with ion detector, ion detector is connected with outside signal analyzer by wire.
4. device according to claim 1, is characterized in that:
Kapillary (2) exit is coaxial with the back taper entrance (7) on cold-trap top cover (6); Liquid, from kapillary (2) outlet ejection, enters in refrigerating chamber (9) through back taper entrance (7); Cold-trap lid (6) is connected by screw thread with refrigerating chamber (9).
5. device according to claim 4, is characterized in that:
Liquid beam is directly injected to vacuum chamber (1) the inside by kapillary (2), and capillary diameter is between 0.01 ~ 0.2mm, and the distance of kapillary (2) outlet distance cold-trap upper cover (6) is 0.5 ~ 200mm.
6. device according to claim 1, is characterized in that:
The outer wall of the roundabout folding outermost layer ring cavity of refrigerating chamber (9) is provided with temperature sensor (12); Temperature sensor is connected with warning device (13) by wire.
7. device according to claim 1, is characterized in that:
Ring cavity opening (16) place be connected with ambient atmosphere is provided with thermal insulation material (17); Enter in the ring cavity be connected with ambient atmosphere for stoping water vapor and condensation occurs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110427065.0A CN103163011B (en) | 2011-12-19 | 2011-12-19 | Vacuum liquid refrigeration sampling device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110427065.0A CN103163011B (en) | 2011-12-19 | 2011-12-19 | Vacuum liquid refrigeration sampling device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103163011A CN103163011A (en) | 2013-06-19 |
| CN103163011B true CN103163011B (en) | 2015-06-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110427065.0A Expired - Fee Related CN103163011B (en) | 2011-12-19 | 2011-12-19 | Vacuum liquid refrigeration sampling device |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020005209A (en) * | 2000-06-27 | 2002-01-17 | 장근호 | Cold Trap for contamination protection during vacuum pump operation of thermal vacuum chamber |
| EP1696231A1 (en) * | 2005-02-25 | 2006-08-30 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | Gas chromatography apparatus |
| CN102023114A (en) * | 2009-09-22 | 2011-04-20 | 中国科学院理化技术研究所 | Experimental system for use with liquid helium cryogenic target |
| CN202442917U (en) * | 2011-12-19 | 2012-09-19 | 中国科学院大连化学物理研究所 | Vacuum liquid freezing and sampling device |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001015498A (en) * | 1999-06-28 | 2001-01-19 | Tokyo Electron Ltd | Heat treatment device |
| DE10242622A1 (en) * | 2002-09-13 | 2004-04-01 | MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. | Liquid trap for collecting liquids in a vacuum device |
-
2011
- 2011-12-19 CN CN201110427065.0A patent/CN103163011B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020005209A (en) * | 2000-06-27 | 2002-01-17 | 장근호 | Cold Trap for contamination protection during vacuum pump operation of thermal vacuum chamber |
| EP1696231A1 (en) * | 2005-02-25 | 2006-08-30 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | Gas chromatography apparatus |
| CN102023114A (en) * | 2009-09-22 | 2011-04-20 | 中国科学院理化技术研究所 | Experimental system for use with liquid helium cryogenic target |
| CN202442917U (en) * | 2011-12-19 | 2012-09-19 | 中国科学院大连化学物理研究所 | Vacuum liquid freezing and sampling device |
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|---|---|
| CN103163011A (en) | 2013-06-19 |
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Granted publication date: 20150617 Termination date: 20181219 |