CN106706817A - Capillary liquid chromatographic column temperature control device - Google Patents
Capillary liquid chromatographic column temperature control device Download PDFInfo
- Publication number
- CN106706817A CN106706817A CN201710153651.8A CN201710153651A CN106706817A CN 106706817 A CN106706817 A CN 106706817A CN 201710153651 A CN201710153651 A CN 201710153651A CN 106706817 A CN106706817 A CN 106706817A
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- CN
- China
- Prior art keywords
- capillary
- liquid chromatographic
- chromatographic column
- temperature
- capillary liquid
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Classifications
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
Abstract
The invention relates to a capillary liquid chromatographic column temperature control device, and relates to a capillary liquid chromatographic column. The capillary liquid chromatographic column temperature control device comprises a cooling fan, a hollow capillary column supporting tube, a capillary liquid chromatographic column, a temperature control device and a base, wherein the cooling fan is arranged at the top of the hollow capillary column supporting tube, and the periphery of the hollow capillary column supporting tube is covered with an electric heating coating layer; a threaded groove is engraved in the outside of the hollow capillary column supporting tube and is used for fixing the capillary liquid chromatographic column, and the capillary liquid chromatographic column is spirally wound on the surface of the hollow capillary column supporting tube; the periphery of the hollow capillary column supporting tube wound with the capillary liquid chromatographic column is covered with a temperature sensitive resistance layer, and the temperature control device is provided with a temperature sensor and a display device; the temperature sensor is used for detecting the temperature of the temperature sensitive resistance layer, and the temperature signal output terminal of the temperature sensor is connected with the display device; and the temperature signals of the temperature sensor are displayed by the display device, and the hollow capillary column supporting tube is arranged on the base.
Description
Technical field
The present invention relates to capillary liquid chromatographic column, more particularly, to capillary liquid chromatographic column temperature regulating device.
Background technology
Since the eighties in last century, with the development of chromatographic theory and correlation technique, people start gradually to recognize micro-
The advantage of piece-rate system, when the mobile phase flow rate that chromatographic run is used tends to micro updating or even nanoliter level, due to background solvent
Volume reduces, and can increase substantially detection sensitivity, so as to the analysis for being adaptive to micro-example is detected.Simultaneously as
Flow-reduction, organic solvent amount required in unit run time is reduced, so as to limit the consumption of toxic solvent and save operation
Cost.In addition, in Tandem analysis technology online using liquid chromatography-mass spectrography, relatively low flow velocity can improve electron spray
The nebulization efficiency of ion gun is so as to further improve mass spectrographic detection sensitivity, it is adaptable to qualitative and quantitative point of complex sample
Analysis.
The important parameter that temperature as liquid chromatogram separate, when directly affecting chromatogram separative efficiency and analysis operation
Between.By raising running temperature, mobile phase viscosity can be effectively reduced, so as under very fast flow conditions, system is still able to
Relatively low operating pressure is in, so as to largely improve chromatographic velocity.Exist additionally, rising high-temperature and can accelerate sample
Mass-transfer efficiency between mobile phase and fixing phase, is conducive to obtaining preferable separating effect.
Traditional chromatographic column incubator can only support the capillary column of 15cm or so length mostly, and often for protein and
For the complex sample of the large biological molecules such as polypeptide, column length needs to reach that 50cm is even longer could be allowed in single run
The resolution capability of people's satisfaction, this causes that traditional column oven cannot very well be applied to the research fields such as proteomics.Meanwhile, pass
The heating journey of system column oven is shorter, and mobile phase not fully reaches temperature equalization in column jecket, and influence separates reappearance, and these are not
Foot all governs the performance of traditional column oven function in actual use.
Chinese patent CN104034831A discloses a kind of overlength protein with temp auto-controlled, peptide separation capillary liquid phase color
Spectrum column system, support is fixed on the middle part of shell；Populated capillary liquid chromatographic column is coiled on support, its post two
End is stretched out from the reserved aperture in the edge of shell respectively；After capillary is installed, insulation is filled between capillary column and shell
Material；Control panel is fixed on the middle part of shell, and be placed in capillary column circle and near the thermocouple of post, be fixed on
Temperature control module in capillary column circle and the semiconductor thermoelectric refrigeration piece connection as a column system shell part.The invention is
Controlling makees simple, cheap.Overlength capillary column is combined with temperature-controlling system, column temperature is raised, mobile phase can be effectively reduced
Viscosity, reduces back-pressure, accelerates two alternate mass transfer rates, convenient, efficient to realize that sample is separated.
The content of the invention
It is an object of the invention to provide the accurate quick control that can be realized to random length, especially overlength capillary column
The capillary liquid chromatographic column temperature regulating device of temperature.
The present invention is provided with radiator fan, hollow type capillary column support tube, capillary liquid chromatographic column, temperature control equipment
And base, radiator fan installed in hollow type capillary column support tube top, cover by the hollow type capillary column support tube periphery
There is electric heating coating, thread groove is carved with outside hollow type capillary column support tube, the thread groove is used for fixed capillary liquid
Phase chromatographic column, the capillary liquid chromatographic column is with spiral wrap on hollow type capillary column support tube surface；It is being wound with
The hollow type capillary column support tube periphery cladding thermo-sensitive resistor layer of capillary liquid chromatographic column, the thermo-sensitive resistor layer is for examining
Survey real-time column temperature；The temperature control equipment is used to show real-time column temperature and controls heating hollow type capillary column support tube and dissipate
The opening and closing of Hot-air fan, the temperature control equipment is provided with temperature sensor, display, and the temperature sensor is used to examine
The temperature of the quick resistive layer of thermometric, the temperature signal output termination display of temperature sensor, by display displays temperature sensor
Temperature signal, hollow type capillary column support tube be arranged on base on.
The hollow type capillary column support tube by heat good conductor be made, it is described heat good conductor may be selected from gold, silver,
Metal or alloy such as copper, iron etc., the external diameter of hollow type capillary column support tube can be 3~5cm.The electric heating coating can be used
Semiconductor thermoelectric film, infrared electrothermal film, magnetic induction Electric radiant Heating Film or other kinds of electric heating material, the thickness of electric heating coating can
It is 0.1~5mm, it is described to be covered with electric heating coating, can be using methods such as spraying, stickup or evaporations.
The thermo-sensitive resistor layer can be using RTD layer；The thermo-sensitive resistor layer is outer can be cased with being incubated sleeve, for maintaining
Steady temperature, it is described to be covered with thermo-sensitive resistor layer, can use and miniature platinum thermal resistance sensing probe is welded on insulation sleeve lining；
The thickness for being incubated sleeve can be 0.5~10mm, and the insulation sleeve can be made up of resistant to elevated temperatures hot non-conductor, the high temperature resistant
Hot non-conductor one kind for may be selected from asbestos, polytetrafluoroethylene (PTFE), ceramic fiber cotton etc..
Populated capillary liquid chromatographic column is with spiral wrap on hollow type capillary column support tube surface.
Compared with the prior art, the present invention has following technique effect：
1) present invention using hollow type capillary column support tube as heating skeleton so that capillary liquid chromatographic column can be with
Take spiral wrap on hollow type capillary column support tube surface, significantly reduce the volume shared by the present invention, effectively solution
Determine the heating problems of long column and overlength post, while allow many capillary liquid-phase chromatographic columns to heat parallel simultaneously, can be used for simultaneously
In the chromatographic fractionation system of row multichannel.
2) the spiral wrap structure that the present invention is used can effectively expand heating journey so that capillary liquid chromatographic column exists
Can be with thermally equivalent in the range of full post.
3) radiator fan is arranged on hollow type capillary column support tube top by the present invention, using cross-ventilated mode reality
It is now quick to reduce temperature.
4) electric heating coating of the invention is close to capillary liquid chromatographic column, and it is capillary column to take contact heat transfer
Heating so that heat transfer efficiency is higher.
5) present invention uses platinum resistance temperature sensor, can precisely detect capillary liquid chromatographic column real time temperature, can
With precise control capillary liquid chromatography running temperature, and excellent thermal insulation performance.
6) present invention can be integrated in miniaturization chromatographic system in, due to capillary column with spiral wrap on support tube,
Therefore random length capillary chromatographic column is supported, especially the temperature control of overlength capillary chromatographic column (being more than 50cm).
Brief description of the drawings
Fig. 1 is the structure composition schematic diagram of the embodiment of the present invention.
Specific embodiment
Following examples will the present invention is further illustrated with reference to accompanying drawing.
Referring to Fig. 1, the embodiment of the present invention is provided with radiator fan 1, hollow type capillary column support tube 2, capillary liquid phase color
Spectrum post 5, temperature control equipment 7 and base 6, radiator fan 1 are arranged on the top of hollow type capillary column support tube 2, described hollow
The periphery of formula capillary column support tube 2 is coated with electric heating coating, and thread groove is carved with outside hollow type capillary column support tube 2,
The thread groove is used for fixed capillary liquid-phase chromatographic column 5, and the capillary liquid chromatographic column 5 is with spiral wrap in hollow type
The surface of capillary column support tube 2；It is covered with the periphery of hollow type capillary column support tube 2 for being wound with capillary liquid chromatographic column 5
Thermo-sensitive resistor layer 3, the thermo-sensitive resistor layer 3 is used to detect real-time column temperature；The temperature control equipment 7 is used to show real-time column temperature
And control to heat the opening and closing of hollow type capillary column support tube 2 and radiator fan 1, the temperature control equipment 7 is provided with
Temperature sensor, display, the temperature sensor are used to detect the temperature of thermo-sensitive resistor layer 3, the temperature letter of temperature sensor
Number output termination display, by the temperature signal of display displays temperature sensor, hollow type capillary column support tube 2 is arranged on
On base 6.
The hollow type capillary column support tube 2 by heat good conductor be made, it is described heat good conductor may be selected from gold, silver,
Metal or alloy such as copper, iron etc., the external diameter of hollow type capillary column support tube 2 can be 3~5cm.The electric heating coating can be adopted
With semiconductor thermoelectric film, infrared electrothermal film, magnetic induction Electric radiant Heating Film or other kinds of electric heating material, the thickness of electric heating coating
Can be 0.1~5mm, it is described to be covered with electric heating coating, can be using methods such as spraying, stickup or evaporations.
The thermo-sensitive resistor layer 3 can be using RTD layer；Can be cased with being incubated sleeve 4 outside the thermo-sensitive resistor layer 3, for tieing up
Steady temperature is held, it is described to be covered with thermo-sensitive resistor layer 3, can use and miniature platinum thermal resistance sensing probe is welded on insulation sleeve 4
Inwall；The thickness for being incubated sleeve 4 can be 0.5~10mm, and the insulation sleeve 4 can be made up of resistant to elevated temperatures hot non-conductor, institute
State one kind that resistant to elevated temperatures hot non-conductor may be selected from asbestos, polytetrafluoroethylene (PTFE), ceramic fiber cotton etc..
Populated capillary liquid chromatographic column is with spiral wrap on hollow type capillary column support tube surface.
Specific embodiment given below.
An external diameter 50mm, the copper hollow cylinder of thickness 3mm, 150mm high are processed, surface goes out to be used to solid using lathe process
Determine the screw thread of capillary liquid chromatographic column.A length is taken for 1m, 365 μm of external diameter, the capillary liquid chromatographic column that 100 μm of internal diameter
Support tube surface is wrapped in by threaded line.
It is the semiconductor thermoelectric film of 0.5mm in support tube plated surface last layer thickness to use vapour deposition process, and in support
Cylinder upper and lower ends pick out wire respectively.
It is 50.3mm to make an internal diameter with the ceramic fiber cotton that thickness is 3mm, the insulation sleeve of 120mm high, in sleeve
Wall is pasted with metal platinum sensor probe, and picks out respective wire.By the above-mentioned support tube for being tied with capillary column through guarantor
It is fixed on base after warm sleeve, capillary column is imported and exported and is stretched out from sleeve upper and lower ends respectively.
Radiator fan is installed with screw and bolt arrangement at the top of support tube, by its wire together with Electric radiant Heating Film wire, platinum electricity
Resistance sensor conductor is connected on the corresponding pin of temperature control equipment together.
Heater switch in opening temperature control equipment in chromatographic system equilibrium process starts to capillary liquid chromatography
Post is heated, while display screen is obtained on temperature control equipment can show real-time column temperature, heating is disconnected after being heated to assigned temperature
Switch enters insulating process, and fan swicth is opened when need to reduce temperature carries out forced convertion.
Claims (10)
1. capillary liquid chromatographic column temperature regulating device, it is characterised in that be provided with radiator fan, hollow type capillary column support tube, hair
Capillary liquid-phase chromatographic post, temperature control equipment and base, radiator fan are arranged on hollow type capillary column support tube top, described
Hollow type capillary column support tube periphery is covered with electric heating coating, and thread groove is carved with outside hollow type capillary column support tube,
The thread groove is used for fixed capillary liquid-phase chromatographic column, and the capillary liquid chromatographic column is with spiral wrap in hollow type hair
Capillary column support tube surface；Temperature sensitive electricity is coated in the hollow type capillary column support tube periphery for being wound with capillary liquid chromatographic column
Resistance layer, the thermo-sensitive resistor layer is for detecting real-time column temperature；The temperature control equipment is used to show real-time column temperature and controls to add
The opening and closing of hot hollow type capillary column support tube and radiator fan, the temperature control equipment be provided with temperature sensor,
Display, the temperature sensor is used to detect the temperature of thermo-sensitive resistor layer, and the temperature signal output termination of temperature sensor is aobvious
Show device, by the temperature signal of display displays temperature sensor, hollow type capillary column support tube is arranged on base.
2. capillary liquid chromatographic column temperature regulating device as claimed in claim 1, it is characterised in that the hollow type capillary column branch
Support cylinder is made up of the good conductor of heat.
3. capillary liquid chromatographic column temperature regulating device as claimed in claim 2, it is characterised in that the good conductor of the heat be selected from gold,
Silver, copper, iron or alloy.
4. capillary liquid chromatographic column temperature regulating device as claimed in claim 1, it is characterised in that hollow type capillary column support tube
External diameter be 3~5cm.
5. capillary liquid chromatographic column temperature regulating device as claimed in claim 1, it is characterised in that the electric heating coating is using half
Conductor electrothermal diaphragm, infrared electrothermal film, magnetic induction Electric radiant Heating Film or other kinds of electric heating material.
6. the capillary liquid chromatographic column temperature regulating device as described in claim 1 or 5, it is characterised in that the thickness of the electric heating coating
It is 0.1~5mm to spend.
7. capillary liquid chromatographic column temperature regulating device as claimed in claim 1, it is characterised in that described to be covered with electric heating coating, adopts
With spraying, paste or evaporation coating method.
8. capillary liquid chromatographic column temperature regulating device as claimed in claim 1, it is characterised in that the thermo-sensitive resistor layer uses platinum
Resistive layer.
9. capillary liquid chromatographic column temperature regulating device as claimed in claim 1, it is characterised in that the thermo-sensitive resistor layer is outer to be cased with
Insulation sleeve；The thickness for being incubated sleeve can be 0.5~10mm, and the insulation sleeve can be made up of resistant to elevated temperatures hot non-conductor,
The resistant to elevated temperatures hot non-conductor may be selected from the one kind in asbestos, polytetrafluoroethylene (PTFE), ceramic fiber cotton.
10. capillary liquid chromatographic column temperature regulating device as claimed in claim 1, it is characterised in that described to be covered with thermo-sensitive resistor layer,
Insulation sleeve lining is welded on using by miniature platinum thermal resistance sensing probe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710153651.8A CN106706817A (en) | 2017-03-15 | 2017-03-15 | Capillary liquid chromatographic column temperature control device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710153651.8A CN106706817A (en) | 2017-03-15 | 2017-03-15 | Capillary liquid chromatographic column temperature control device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106706817A true CN106706817A (en) | 2017-05-24 |
Family
ID=58884742
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710153651.8A Pending CN106706817A (en) | 2017-03-15 | 2017-03-15 | Capillary liquid chromatographic column temperature control device |
Country Status (1)
| Country | Link |
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| CN (1) | CN106706817A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109082361A (en) * | 2017-06-13 | 2018-12-25 | 无锡源清天木生物科技有限公司 | A kind of capillary array device |
| CN109243962A (en) * | 2018-09-29 | 2019-01-18 | 厦门大学 | A kind of heating device of electrospray ionization mass spectrum transfer capillary |
| CN113916996A (en) * | 2020-07-10 | 2022-01-11 | 北京普析通用仪器有限责任公司 | Column oven for gas chromatograph and gas chromatograph |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4726822A (en) * | 1984-10-22 | 1988-02-23 | Honeywell Inc. | Fast response thermochromatographic capillary columns |
| EP1262772A2 (en) * | 2001-05-30 | 2002-12-04 | Gerstel Systemtechnik GmbH & Co. KG | Temperature-controlled injector for chemical analyser |
| CN2840033Y (en) * | 2005-06-06 | 2006-11-22 | 张西咸 | High precision temperature control micro-chromatographic column box |
| CN1877320A (en) * | 2005-06-06 | 2006-12-13 | 张西咸 | Minisize chromatographic column box with high precision temperature control system |
| CN1877319A (en) * | 2005-06-06 | 2006-12-13 | 张西咸 | Minisize chromatographic column box with high precision temperature control system |
| CN201903535U (en) * | 2010-11-30 | 2011-07-20 | 中国科学院大连化学物理研究所 | Chromatographic column rapid-heating device |
| CN104181262A (en) * | 2013-05-23 | 2014-12-03 | 中国科学院大连化学物理研究所 | Cold zone-free low-power dissipation miniature furnace case |
-
2017
- 2017-03-15 CN CN201710153651.8A patent/CN106706817A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4726822A (en) * | 1984-10-22 | 1988-02-23 | Honeywell Inc. | Fast response thermochromatographic capillary columns |
| EP1262772A2 (en) * | 2001-05-30 | 2002-12-04 | Gerstel Systemtechnik GmbH & Co. KG | Temperature-controlled injector for chemical analyser |
| CN2840033Y (en) * | 2005-06-06 | 2006-11-22 | 张西咸 | High precision temperature control micro-chromatographic column box |
| CN1877320A (en) * | 2005-06-06 | 2006-12-13 | 张西咸 | Minisize chromatographic column box with high precision temperature control system |
| CN1877319A (en) * | 2005-06-06 | 2006-12-13 | 张西咸 | Minisize chromatographic column box with high precision temperature control system |
| CN201903535U (en) * | 2010-11-30 | 2011-07-20 | 中国科学院大连化学物理研究所 | Chromatographic column rapid-heating device |
| CN104181262A (en) * | 2013-05-23 | 2014-12-03 | 中国科学院大连化学物理研究所 | Cold zone-free low-power dissipation miniature furnace case |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109082361A (en) * | 2017-06-13 | 2018-12-25 | 无锡源清天木生物科技有限公司 | A kind of capillary array device |
| CN109243962A (en) * | 2018-09-29 | 2019-01-18 | 厦门大学 | A kind of heating device of electrospray ionization mass spectrum transfer capillary |
| CN109243962B (en) * | 2018-09-29 | 2019-09-10 | 厦门大学 | A kind of heating device of electrospray ionization mass spectrum transfer capillary |
| CN113916996A (en) * | 2020-07-10 | 2022-01-11 | 北京普析通用仪器有限责任公司 | Column oven for gas chromatograph and gas chromatograph |
| CN113916996B (en) * | 2020-07-10 | 2023-12-15 | 北京普析通用仪器有限责任公司 | Column incubator for gas chromatograph and gas chromatograph |
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Legal Events
| Date | Code | Title | Description |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170524 |
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| RJ01 | Rejection of invention patent application after publication |