CN105866305A - Gas chromatography sample injecting system visualization device - Google Patents
Gas chromatography sample injecting system visualization device Download PDFInfo
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- CN105866305A CN105866305A CN201610441505.0A CN201610441505A CN105866305A CN 105866305 A CN105866305 A CN 105866305A CN 201610441505 A CN201610441505 A CN 201610441505A CN 105866305 A CN105866305 A CN 105866305A
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- China
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- main body
- camera bellows
- visualization device
- vaporizer
- constant temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
Abstract
The invention discloses a gas chromatography sample injecting system visualization device. The gas chromatography sample injecting system visualization device comprises a hidden box main body with a carrier gas hole and an observation window, wherein a light source system, a temperature control system and a vaporizing chamber system are arranged in a front chamber of the hidden box main body, and a circuit is arranged in a rear chamber; the light source system comprises a fluorescent tube and an ultraviolet light; the temperature control system comprises a constant temperature magnetic stirrer arranged at the center of the front chamber and an exhaust fan arranged on the wall of the hidden box main body, a marker post and a thermometer of the constant temperature magnetic stirrer respectively penetrate out the hidden box main body from a maker post hole and a thermometer hole in the surface of the hidden box main body; the vaporizing chamber system comprises a quartz square cylinder which is arranged on the constant temperature magnetic stirrer and is filled with silicone oil, a sample injecting hole simulator immersing the silicone oil and a vaporizing chamber; the sample injecting hole simulator is a snake-shaped U-shaped pipe connected by virtue of a three-way joint and a U-shaped pipe internally provided with a vaporizing chamber; a screw thread matched with a hollow nut is formed at the other port of the three-way joint, and the port is arranged below a sample injecting hole of the hidden box main body. The gas chromatography sample injecting system visualization device is simple in structure.
Description
Technical field
The present invention relates to a kind of gas chromatographic sample introduction system visualization device, belong to gas chromatographic sample introduction system visual analyzing field.
Background technology
The air-channel system strict seal of gas chromatograph, will not cause gas leakage for sample is sent into chromatographic system, it is necessary to arrange special device injection port.Owing to general sample is in a liquid state, needing to be gasified totally before entering chromatographic column, therefore injection port is also known as vaporizer.The first step of gas chromatographic analysis i.e. introduces the sample into vaporizer and wherein by thermal evaporation, the most quantitatively proceed to chromatographic column [Liu Huwei, gas chromatography and application, Chemical Industry Press: Beijing, 2007; p5].Under normal circumstances, according to chromatographic process data-optimized injection port condition, including vaporizer temperature, input mode, vaporizer type and the kind of implant and mounting condition.But chromatographic process evaluation means is difficult to provide the integrated information that sample gasifies in vaporizer, and the athletic meeting of sample gasification Indoor Air process affects gasification efficiency, produce gasification postpone and form spraying, i.e. Leiden spraying effect (Leiden frost phenomenon) [Journal of High
Resolution Chromatography 1995, 18 (9), 573-578].Therefore, for system evaluation gas chromatographic sample introduction system, the present invention designs a kind of visualization device, uses fluorescent agent perylene to observe liquid gasification in vaporizer, and by digital camera shooting record gasification.
Summary of the invention
It is an object of the invention to provide a kind of gas chromatographic sample introduction system visualization device.
Device of the present invention can simulate thermal shunt/Splitless injecting samples process, by the camera record liquor sample concrete gasification in vaporizer, to realize the optimization of injection port condition.This device has simple in construction, invests the advantages such as little, can accelerate experiment progress and expand new analysis method simultaneously.
A kind of gas chromatographic sample introduction system visualization device, it is characterized in that including which is provided with the camera bellows main body of watch window, this camera bellows main body is classified as forward and backward room, being provided with light-source system, temperature control system and vaporizer system in described cup by its internal set dividing plate；Described light-source system includes that fluorescent tube and λ are 365 nm or the uviol lamp of 254 nm；Described temperature control system includes the constant temperature blender with magnetic force being positioned at cup central authorities and the exhaust fan being placed on described camera bellows main wall, and the mark post of described constant temperature blender with magnetic force and thermometer pass camera bellows main body from the table bar mouth of camera bellows body surfaces and thermometer mouth respectively；Described vaporizer system includes being placed in described constant temperature blender with magnetic force and it is built with the square quartz cylinder of silicone oil, the injection port analog immersed in silicone oil and vaporizer；Described injection port analog is two U-tube connected by threeway, and one of them U-tube is snakelike pipeline, and another U-tube is provided with vaporizer in the pipe of threeway；The port not being connected with U-tube in described threeway is provided with the screw thread matched with hollow nut, and this port is positioned at the lower section of injection port set by camera bellows main body；Carrier gas carrier gas port in camera bellows main body is passed through from snakelike pipeline；The rear chamber of described camera bellows main body installs circuit.
The two ends of described square quartz cylinder are provided with groove.
It is provided with sample introduction dottle pin in described hollow nut.
Described camera bellows main body is used for isolating external light source, disposing internal light source system, heating system and interlock circuit；Described camera bellows body surfaces is provided with the circular hole of different pore size, including: watch window, it is used for observing and shoot liquid gasification process；Thermometer mouth, is used for assigning mercurial thermometer, simulates the hot sample introduction of gas chromatogram；Table bar mouth, for assigning the table bar of magnetic stirring apparatus, with fixing mercurial thermometer；Carrier gas port, is used for assigning gas-carrier pipeline and electric wire；Injection port, for syringe sampling；Described dividing plate can isolate the hot environment of cup, it is ensured that the safety of rear interior circuit；Described light-source system provides light source to realize the visual observation of liquor sample gasification, wherein λ is the uviol lamp colour developing for fluorescent agent perylene of 365 nm, λ is the uviol lamp colour developing for other fluorescent agents of 254 nm, and daylight lamp is convenient tests the observation of each device in gap realizes camera bellows main body；Described constant temperature blender with magnetic force, distribution contact mercurial thermometer can automatically control oil bath heating-up temperature；Described exhaust fan can realize the fast cooling of camera bellows cup；Described square quartz cylinder uses squared design can reduce the luminous reflectance impact on pickup quality.
Visualization device of the present invention introduces camera bellows, it is to avoid external light source interference, and experiment condition is easily achieved；Introduce exhaust fan, it is easy to cooling, shorten the sample introduction cycle；Carrier gas realizes preheating by snakelike pipeline, preferably simulates injector temperature condition；And there is simple in construction, invest little, safe advantage.
Accompanying drawing explanation
Fig. 1 is the structural representation (perspective view) of the present invention.
Fig. 2 is the structural front view of the present invention.
Fig. 3 is the structural side view of the present invention.
Fig. 4 is the structure top view of the present invention.
Fig. 5 is the structural representation of injection port analog of the present invention.
Fig. 6 is the structural representation of square quartz cylinder of the present invention.
Fig. 7 is sample view data of gasification in empty straight vaporizer.
Fig. 8 is sample view data of gasification in the vaporizer containing glass cotton.
Fig. 9 is sample view data of gasification in glass cup vaporizer.
Figure 10 is sample view data of gasification in baffle plate vaporizer.
In figure: 1-λ is the uviol lamp of 365 nm；2-λ is the uviol lamp of 254 nm；3-fluorescent tube；4-exhaust fan；1 '-uviol lamp (λ=365 nm) switchs；2 '-uviol lamp (λ=254 nm) switchs；3 '-switch for fluorescent lamp；4 '-fan switches；5-watch window；6-thermometer mouth；7-table bar mouth；8-carrier gas port；9-injection port.
Detailed description of the invention
1-4 referring to the drawings, a kind of gas chromatographic sample introduction system visualization device, including which is provided with the camera bellows main body of watch window 5, this camera bellows main body is classified as forward and backward room by its internal set dividing plate, is provided with light-source system, temperature control system and vaporizer system in cup；Light-source system includes the uviol lamp 1,2 that fluorescent tube 3 and λ is 365 nm or 254 nm；Temperature control system includes the constant temperature blender with magnetic force being positioned at cup central authorities and the exhaust fan 4 being placed on camera bellows main wall, and the mark post of constant temperature blender with magnetic force and thermometer pass camera bellows main body from the table bar mouth 7 of camera bellows body surfaces and thermometer mouth 6 respectively；Vaporizer system includes being placed in described constant temperature blender with magnetic force and it is built with the square quartz cylinder of silicone oil, the injection port analog immersed in silicone oil and vaporizer；Injection port analog is two U-tube connected by threeway, and one of them U-tube is snakelike pipeline, and another U-tube is provided with vaporizer in the pipe of threeway；The port not being connected with U-tube in threeway is provided with the screw thread matched with hollow nut, and this port is positioned at the lower section of injection port 9 set by camera bellows main body；Carrier gas carrier gas port 8 in camera bellows main body is passed through from snakelike pipeline；The rear chamber of camera bellows main body installs circuit.
The two ends of square quartz cylinder are provided with groove.
Sample introduction dottle pin it is provided with in hollow nut.
Three light sources (1,2,3) can rely on visualization requirements to shift one's position.Place constant temperature blender with magnetic force, thermometer mouth 6 and table bar mouth 7 bottom camera bellows to regulate according to size and the riding position of magnetic stirring apparatus.
Referring to the drawings 5, it is shown that the structural representation of existing injection port analog, middle glass tubing is used for laying vaporizer, and the internal diameter of this glass tubing should be the least to prevent rocking of vaporizer.For carrier gas preheating is better achieved, devise snakelike pipeline.
Referring to the drawings 6, it is shown that the structural representation of the existing square quartz cylinder holding oil bath, its squared design is mainly for reducing the luminous reflectance impact on pickup quality, and the outer surface at rear portion can black coating color high-temperaure coating.For fixing injection port analog, it is carved with groove at the two ends of square quartz cylinder.
7-10 referring to the drawings, it is shown that liquor sample is the view data of gasification in different universal/tailored version vaporizers.
Embodiment 1
For shunting/Splitless injecting samples mouth, the hot pin sample introduction of general employing.When injector temperature is relatively low or sample size is bigger, produce zone sample introduction.Utilize the visualization device of design, analyze the gasification of empty straight type gasification indoor liquid: be first turned on constant temperature blender with magnetic force controlling injection port (oil bath) temperature is 100 DEG C, open the uviol lamp of λ=365 nm, syringe sampling 6 μ L(sample is the perylene-chloroformic solution of 0.1%), digital camera (camera bellows is outer) is used to pass through watch window recording liquid gasification in using empty straight type vaporizer, as shown in Figure 7.Visualization result shows, zone liquid passes rapidly through straight type vaporizer, is gathered in bottom vaporizer and gasifies, and gasification efficiency is relatively low, and with violent random motion, the accuracy of impact analysis result and repeatability.And the fluid sample of bottom may be directly entered chromatographic column and pollute.
Embodiment 2
When analyzing high boiling point, thermally labile or during trace components, owing to vaporizer temperature is relatively low, sample size is compared with big or that the boiling point of sample own is higher feature, it is difficult to realize spraying sample introduction, it is necessary in gasification indoor location implant.Utilize the visualization device of design, analyze the gasification containing glass cotton gasification indoor liquid: be first turned on constant temperature blender with magnetic force controlling injection port (oil bath) temperature is 100 DEG C, open the uviol lamp of λ=365 nm, syringe sampling 6 μ L(sample is the perylene-chloroformic solution of 0.1%), use digital camera (camera bellows is outer) by watch window recording liquid containing the gasification in glass cotton vaporizer.Visualized experiment shows, glass cotton (loadings 9 mg, filling height 5 mm) can trap zone liquid well until sample is gasified totally on its surface, as shown in Figure 8.
Embodiment 3
Utilize the visualization device of design, evaluate the impact on the gasification of liquor sample of the commercially available professional vaporizer: be first turned on constant temperature blender with magnetic force controlling injection port (oil bath) temperature is 100 ° of C, open the uviol lamp of λ=365 nm, syringe sampling 6 μ L(sample is the perylene-chloroformic solution of 0.1%), digital camera (camera bellows is outer) is used to pass through watch window recording liquid gasification in commercially available glass vaporizer, such as accompanying drawing 9.Visualization result shows, glass can well limit the motion of zone.
Embodiment 4
Utilize the visualization device of design, analyze fluid sample gasification in the commercially available vaporizer containing many baffle plates further: be first turned on constant temperature blender with magnetic force controlling injection port (oil bath) temperature is 100 ° of C, open the uviol lamp of λ=365 nm, syringe sampling 6 μ L(sample is the perylene-chloroformic solution of 0.1%), digital camera (camera bellows is outer) is used to pass through watch window recording liquid gasification in commercially available baffle plate vaporizer, such as accompanying drawing 10.Visualization result shows, baffle design can also effectively change speed and the flow direction of zone motion, and gasification efficiency is improved.
Claims (3)
1. a gas chromatographic sample introduction system visualization device, it is characterized in that the camera bellows main body including which is provided with watch window (5), this camera bellows main body is classified as forward and backward room, being provided with light-source system, temperature control system and vaporizer system in described cup by its internal set dividing plate；Described light-source system includes fluorescent tube (3) and the uviol lamp (1,2) that λ is 365 nm or 254 nm；Described temperature control system includes the constant temperature blender with magnetic force being positioned at cup central authorities and the exhaust fan (4) being placed on described camera bellows main wall, and the mark post of described constant temperature blender with magnetic force and thermometer pass camera bellows main body from table bar mouth (7) of camera bellows body surfaces and thermometer mouth (6) respectively；Described vaporizer system includes being placed in described constant temperature blender with magnetic force and it is built with the square quartz cylinder of silicone oil, the injection port analog immersed in silicone oil and vaporizer；Described injection port analog is two U-tube connected by threeway, and one of them U-tube is snakelike pipeline, and another U-tube is provided with vaporizer in the pipe of threeway；The port not being connected with U-tube in described threeway is provided with the screw thread matched with hollow nut, and this port is positioned at the lower section of injection port (9) set by camera bellows main body；Carrier gas carrier gas port (8) in camera bellows main body is passed through from snakelike pipeline；The rear chamber of described camera bellows main body installs circuit.
2. visualization device as claimed in claim 1, it is characterised in that the two ends of described square quartz cylinder are provided with groove.
3. visualization device as claimed in claim 1, it is characterised in that be provided with sample introduction dottle pin in described hollow nut.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610441505.0A CN105866305A (en) | 2016-06-20 | 2016-06-20 | Gas chromatography sample injecting system visualization device |
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| CN201610441505.0A CN105866305A (en) | 2016-06-20 | 2016-06-20 | Gas chromatography sample injecting system visualization device |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57182164A (en) * | 1981-05-06 | 1982-11-09 | Kotaki Seisakusho:Kk | Removal device for solvent |
| CN2080673U (en) * | 1990-11-09 | 1991-07-10 | 兰州大学 | Multipurpose sample injector for gas chromatograph or chromatograph-mass spectrometer |
| US6245298B1 (en) * | 1998-04-17 | 2001-06-12 | Gerstel Gmbh & Co., Kg | Sample application device for a gas chromatograph |
| CN101210912A (en) * | 2006-12-30 | 2008-07-02 | 中国石油化工股份有限公司 | Gas chromatographic analysis device |
| CN101300486A (en) * | 2005-09-02 | 2008-11-05 | Abb公司 | Modular gas chromatograph |
| CN102384952A (en) * | 2010-08-31 | 2012-03-21 | 株式会社岛津制作所 | Gas chromatograph |
| CN204575620U (en) * | 2015-04-22 | 2015-08-19 | 上海福劳斯检测技术有限公司 | A kind of gas on-line analyzer for the production of on-the site analysis |
| CN205879892U (en) * | 2016-06-20 | 2017-01-11 | 中国科学院兰州化学物理研究所 | Visual device of gas chromatography sampling system |
-
2016
- 2016-06-20 CN CN201610441505.0A patent/CN105866305A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57182164A (en) * | 1981-05-06 | 1982-11-09 | Kotaki Seisakusho:Kk | Removal device for solvent |
| CN2080673U (en) * | 1990-11-09 | 1991-07-10 | 兰州大学 | Multipurpose sample injector for gas chromatograph or chromatograph-mass spectrometer |
| US6245298B1 (en) * | 1998-04-17 | 2001-06-12 | Gerstel Gmbh & Co., Kg | Sample application device for a gas chromatograph |
| CN101300486A (en) * | 2005-09-02 | 2008-11-05 | Abb公司 | Modular gas chromatograph |
| CN101210912A (en) * | 2006-12-30 | 2008-07-02 | 中国石油化工股份有限公司 | Gas chromatographic analysis device |
| CN102384952A (en) * | 2010-08-31 | 2012-03-21 | 株式会社岛津制作所 | Gas chromatograph |
| CN204575620U (en) * | 2015-04-22 | 2015-08-19 | 上海福劳斯检测技术有限公司 | A kind of gas on-line analyzer for the production of on-the site analysis |
| CN205879892U (en) * | 2016-06-20 | 2017-01-11 | 中国科学院兰州化学物理研究所 | Visual device of gas chromatography sampling system |
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