CN108226364A - The constant temperature system and operating method of a kind of liquid chromatogram - Google Patents
The constant temperature system and operating method of a kind of liquid chromatogram Download PDFInfo
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- CN108226364A CN108226364A CN201611130323.8A CN201611130323A CN108226364A CN 108226364 A CN108226364 A CN 108226364A CN 201611130323 A CN201611130323 A CN 201611130323A CN 108226364 A CN108226364 A CN 108226364A
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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
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
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Abstract
The present invention provides a kind of constant temperature system of liquid chromatogram, component part includes heat-conducting block, temperature sensor, capillary tubing, sampling valve, quantitative loop, chromatographic column, pump and temperature adjustment pond.It, can be accurately by chromatographic column column temperature stabilization in set temperature value ± 0.5 degree Celsius using liquid as heat-conducting medium, by the preheating to mobile phase.The configuration of the present invention is simple, technology maturation improve the control accuracy of chromatographic column column temperature, can meet the requirement of liquid chromatogram rigorous analysis.
Description
Technical field
The invention belongs to analysis fields, relate generally to liquid-phase chromatographic analysis.
Background technology
Liquid chromatogram is a kind of important separate analytical technique, is had in fields such as food security, environmental monitoring, biological medicines
Extensive use.The column temperature control of liquid chromatogram has a major impact the precision and accuracy that improve sample analysis, column temperature control
System processed is the important component of most liquid chromatographs, and design and temperature control effect are to improving qualitative, quantitative result
Precision has a significant impact.
For this purpose, the present invention propose a kind of constant temperature system of liquid chromatogram, using liquid as heat-conducting medium, pass through convection current
The preheating of dynamic phase further improves the control accuracy of chromatographic column temperature.The constant temperature system can be accurately by column temperature stabilization in setting temperature
Angle value ± 0.5 degree Celsius, compared with wind-heat (air-cooled) constant temperature system that usual liquid chromatogram uses, the small energy consumption of the present apparatus
It is low, the requirement of liquid chromatogram rigorous analysis can be met.
Invention content
Technical problem solved by the invention is to provide a kind of constant temperature system of liquid chromatogram.The invention belongs to analyze neck
Domain relates generally to chromatography field.
A kind of constant temperature system of liquid chromatogram, which is characterized in that including heat-conducting block, temperature sensor, capillary tubing, sample introduction
Valve, quantitative loop, chromatographic column, pump and temperature adjustment pond；
Heat-conducting block carries the block of hollow airtight cavity for an inside, capillary tubing run through from heat-conducting block internal cavity and
It crosses；Liquid phase pump is connected through capillary tubing, sampling valve with chromatographic column one end, internal duct and cavity form the space of closing；Heat conduction
Block internal cavity connects inlet tube and outlet tube respectively, is connected inside outlet tube and temperature adjustment pond, and temperature adjustment pond is hollow closed for one
Cavity, temperature adjustment pond inside pass through pipeline connection with pump inlet；The outlet of pump is connected with the inlet tube of heat-conducting block；Liquid is in heat conduction
The flow path of closure is formed between block, pump and temperature adjustment pond.
Heat-conducting block is the part with closed cavity internal made of the intermetallic composite coatings such as aluminium alloy, copper, stainless steel；On heat-conducting block
Equipped with groove, chromatographic column can be easily placed and taken out, and chromatography outer surface of column mutually connects with groove when chromatographic column is put into groove
It touches.
Closed cavity is equipped in heat-conducting block, is communicated with cavity equipped with inlet opening, fluid hole, capillary tubing import and capillary steel
Pipe exports；Temperature sensor is equipped in heat-conducting block.
Two end interface of capillary tubing is connected respectively with liquid phase pump and sampling valve interface；Capillary tubing is from heat-conducting block inner chamber
Body passes through, and capillary tubing is in heat-conducting block inside cavity pitch of the laps or as S-shaped bends to increase contact area.
Temperature adjustment pond is by liquid storage tank of the inside with cavity, the heating element which is provided with and cooling module composition；In liquid storage tank
Portion is filled with the heat-conducting liquid of certain capacity, the one or two or more kinds in the liquid such as pure water, ethylene glycol solution, oil；
Ranging from -5~80 DEG C of set temperature, system measure actual temperature according to temperature sensor, control heating element or cooling module
Start, stop, adjusting the temperature of heat-conducting liquid in liquid storage tank.
Sampling valve is four tunnel more than sampling valves, has two interfaces to be connected with two end of quantitative loop thereon.
It is identical with conventional liquid phase chromatograph, when sampling valve is in flushing state：Mobile phase injects capillary tubing from liquid phase pump,
Chromatographic column is then flowed by sampling valve, by entering detector after chromatography post separation；
When sampling valve is in sample introduction state：Mobile phase injects capillary tubing from liquid phase pump, then by sampling valve into excessively fixed
Chromatographic column is flowed into after amount ring, by entering detector after chromatography post separation；The flowing that will be flowed through in capillary tubing by heat-conducting block
The mobile phase for flowing through chromatographic column or sample are maintained at the temperature of setting by phase pre-set temperature.
The beneficial effects of the invention are as follows：Pass through the accurate control and the preheating of mobile phase to liquid chromatogram column temperature, Ke Yixian
The precision for improving separating degree, retention time and peak area is write, is provided safeguard for accurate liquid chromatography qualitative quantitative analysis.
Description of the drawings
Fig. 1 is the connection diagram of the constant temperature system of the liquid chromatogram of the present invention.Wherein, 1 is heat-conducting block；2 pass for temperature
Sensor；3 it is capillary tubing, 4 is sampling valve, 5 is quantitative loop, 6 is chromatographic column, 7 is pump, and 8 be temperature adjustment pond, and 9 be detector, and 10 are
Liquid phase pump.
Fig. 2 is the connection diagram of the heat-conducting block of the constant temperature system of the liquid chromatogram of the present invention.Wherein, 1a for inlet opening,
1b is fluid hole, 1c is capillary tubing import；1d is exported for capillary tubing；2 be temperature sensor；3 be capillary tubing, 4 be into
Sample valve, 5 be quantitative loop, and 6 be chromatographic column, and 7 be pump, and 8 be temperature adjustment pond, and 8a is liquid storage tank, 8b is heating element, and 8c is refrigeration member
Part.
Specific embodiment
A kind of organic matter samples thermal decomposition product sampler proposed by the present invention, chief component include heat-conducting block 1,
Temperature sensor 2, capillary tubing 3, sampling valve 4, quantitative loop 5, chromatographic column 6, pump 7 and temperature adjustment pond 8 etc.；The capillary tubing
3rd, sampling valve 4, being sequentially connected of chromatographic column 6, internal duct and cavity form the space of closing；Capillary tubing 3 is out of heat-conducting block 1
Portion's cavity passes through；1 internal cavity of heat-conducting block connects inlet tube and outlet tube respectively, and outlet tube is connected with 8 inside of temperature adjustment pond
Logical, 8 inside of temperature adjustment pond passes through pipeline connection with pump 7；The outlet of pump 7 is connected with the inlet tube of heat-conducting block 1；Liquid is in heat-conducting block
1st, the flow path of closure is formed between pump 7 and temperature adjustment pond 8.
Heat-conducting block 1 is the part with closed cavity internal made of the intermetallic composite coatings such as aluminium alloy, copper, stainless steel；Heat-conducting block 1
Be equipped with semiclosed groove, chromatographic column 6 can easily be placed and taken out, when chromatographic column 6 is put into groove chromatography outer surface of column with
Groove contacts with each other.Closed cavity is equipped in heat-conducting block 1, communicated with cavity equipped with inlet opening 1a, fluid hole 1b, capillary tubing into
Mouth 1c and capillary tubing outlet 1d；Temperature sensor 2 is equipped in heat-conducting block 1.3 liang of end interfaces of capillary tubing respectively with liquid phase pump
10 are connected with 4 interface of sampling valve；Capillary tubing 3 is passed through from 1 internal cavity of heat-conducting block, and capillary tubing 3 is in heat-conducting block 1)
Inside cavity pitch of the laps or such as S-shaped bend to increase contact area.
Temperature adjustment pond 8 is made of liquid storage tank 8a of the inside with cavity, heating element 8b and cooling module 8c；Inside liquid storage tank 8a
It is filled with the heat-conducting liquid of certain capacity, the liquid such as pure water, ethylene glycol solution, oil；Set temperature ranging from -5~80
DEG C, system measures actual temperature according to temperature sensor 2, and heating element 8b or cooling module 8c is controlled to start, stop, adjusting storage
The temperature of heat-conducting liquid in liquid pool 8a.
The constant temperature system of the liquid chromatogram is identical with conventional liquid phase chromatograph, when sampling valve is in flushing state：Mobile phase
Capillary tubing 3 is injected from liquid phase pump 10, chromatographic column 6 is then flowed by sampling valve 4, enters detection after being detached by chromatographic column 6
Device 9；When sampling valve 4 is in sample introduction state：Mobile phase injects capillary tubing 3 from liquid phase pump 10, then by sampling valve 4 into excessively fixed
Chromatographic column 6 is flowed into after measuring ring 5, enters detector 9 after being detached by chromatographic column 6.It will be flowed through in capillary tubing 3 by heat-conducting block 1
Mobile phase pre-set temperature, the mobile phase for flowing through chromatographic column 6 or sample are maintained to the temperature of setting.
Claims (7)
1. a kind of constant temperature system of liquid chromatogram, which is characterized in that including heat-conducting block (1), temperature sensor (2), capillary tubing
(3), sampling valve (4), quantitative loop (5), chromatographic column (6), pump (7) and temperature adjustment pond (8)；
Heat-conducting block (1) carries the block of hollow airtight cavity for an inside, and capillary tubing (3) is passed through from heat-conducting block (1) internal cavity
It wears and mistake；Liquid phase pump (10) is connected through capillary tubing (3), sampling valve (4) with chromatographic column (6) one end, internal duct and cavity shape
Into the space of closing；Heat-conducting block (1) internal cavity connects inlet tube and outlet tube, outlet tube and temperature adjustment pond (8) internal phase respectively
Connection, temperature adjustment pond (8) are a hollow airtight cavity, and temperature adjustment pond (8) are internal to pass through pipeline connection with pump (7) import；Pump (7) goes out
Mouth is connected with the inlet tube of heat-conducting block (1)；Liquid forms the stream of closure between heat-conducting block (1), pump (7) and temperature adjustment pond (8)
Road.
2. the constant temperature system of liquid chromatogram as described in claim 1, which is characterized in that heat-conducting block (1) is aluminium alloy, copper, no
Become rusty the internal part with closed cavity made of the intermetallic composite coatings such as steel；Heat-conducting block (1) is equipped with groove, and chromatographic column (6) can be square
Being placed and taken out just, chromatography outer surface of column is contacted with each other with groove when chromatographic column (6) is put into groove.
3. the constant temperature system of liquid chromatogram as described in claim 1, which is characterized in that closed cavity is equipped in heat-conducting block (1),
It is communicated with cavity and exports (1d) equipped with inlet opening (1a), fluid hole (1b), capillary tubing import (1c) and capillary tubing；In heat conduction
Block (1) is equipped with temperature sensor (2).
4. the constant temperature system of liquid chromatogram as described in claim 1, which is characterized in that (3) two end interface of capillary tubing is distinguished
It is connected with liquid phase pump (10) and sampling valve (4) interface；Capillary tubing (3) is passed through from heat-conducting block (1) internal cavity, capillary
Steel pipe (3) is in heat-conducting block (1) inside cavity pitch of the laps or as S-shaped bends to increase contact area.
5. the constant temperature system of liquid chromatogram as described in claim 1, which is characterized in that temperature adjustment pond (8) are by inside with cavity
Liquid storage tank (8a), the heating element which is provided with (8b) and cooling module (8c) composition；It is filled with inside liquid storage tank (8a) certain
The heat-conducting liquid of capacity, the one or two or more kinds in the liquid such as pure water, ethylene glycol solution, oil；Set temperature range
It it is -5~80 DEG C, system measures actual temperature according to temperature sensor (2), and control heating element (8b) or cooling module (8c) open
Dynamic, stopping adjusts the temperature of liquid storage tank (8a) interior heat-conducting liquid.
6. the constant temperature system of liquid chromatogram as described in claim 1, which is characterized in that sampling valve (4) is four tunnel more than sample introductions
Valve (4) has two interfaces to be connected with (5) two end of quantitative loop thereon.
7. the operating method of the constant temperature system of the liquid chromatogram as described in claim 1-6 is any, which is characterized in that with conventional liquid
Chromatography is identical, when sampling valve (4) is in the state of flushing：Mobile phase is then led to from liquid phase pump (10) injection capillary tubing (3)
It crosses sampling valve (4) and flows into chromatographic column (6), enter detector (9) after being detached by chromatographic column (6)；
When sampling valve (4) is in sample introduction state：Mobile phase then passes through sampling valve from liquid phase pump (10) injection capillary tubing (3)
(4) into quantitative loop (5) inflow chromatographic column (6) afterwards is crossed, enter detector (9) after being detached by chromatographic column (6)；Pass through heat-conducting block
(1) the mobile phase pre-set temperature that will be flowed through in capillary tubing (3), setting is maintained at by the mobile phase for flowing through chromatographic column (6) or sample
Temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611130323.8A CN108226364B (en) | 2016-12-09 | 2016-12-09 | Constant temperature system of liquid chromatogram |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611130323.8A CN108226364B (en) | 2016-12-09 | 2016-12-09 | Constant temperature system of liquid chromatogram |
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| CN108226364A true CN108226364A (en) | 2018-06-29 |
| CN108226364B CN108226364B (en) | 2020-08-11 |
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| CN201611130323.8A Active CN108226364B (en) | 2016-12-09 | 2016-12-09 | Constant temperature system of liquid chromatogram |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113274764A (en) * | 2021-06-18 | 2021-08-20 | 中触媒新材料股份有限公司 | Liquid phase adsorption separation system and temperature control process method thereof |
| WO2022235752A1 (en) * | 2021-05-04 | 2022-11-10 | Waters Technologies Corporation | Compact liquid chromatography system providing thermal management and detection |
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| US20030061867A1 (en) * | 2001-09-28 | 2003-04-03 | Yuri Gerner | Apparatus for conducting high-temperature liquid chromotography analysis |
| CN202794124U (en) * | 2012-07-29 | 2013-03-13 | 安徽皖仪科技股份有限公司 | Ion chromatograph column heater |
| CN204065039U (en) * | 2014-04-28 | 2014-12-31 | 上海大学 | Liquid chromatograph mobile phase temperature regulating device |
| US20150135861A1 (en) * | 2012-03-08 | 2015-05-21 | Waters Technologies Corporation | Pre-column heating of mobile phase solvent in chromatography systems |
| CN204630991U (en) * | 2015-05-18 | 2015-09-09 | 深圳迈瑞生物医疗电子股份有限公司 | Temp. controlling box and use the liquid chromatography system of this temp. controlling box |
| CN205388592U (en) * | 2016-01-25 | 2016-07-20 | 北京博恩特药业有限公司 | Liquid accuse temperature high performance liquid chromatography column incubator |
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2016
- 2016-12-09 CN CN201611130323.8A patent/CN108226364B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030061867A1 (en) * | 2001-09-28 | 2003-04-03 | Yuri Gerner | Apparatus for conducting high-temperature liquid chromotography analysis |
| US20150135861A1 (en) * | 2012-03-08 | 2015-05-21 | Waters Technologies Corporation | Pre-column heating of mobile phase solvent in chromatography systems |
| CN202794124U (en) * | 2012-07-29 | 2013-03-13 | 安徽皖仪科技股份有限公司 | Ion chromatograph column heater |
| CN204065039U (en) * | 2014-04-28 | 2014-12-31 | 上海大学 | Liquid chromatograph mobile phase temperature regulating device |
| CN204630991U (en) * | 2015-05-18 | 2015-09-09 | 深圳迈瑞生物医疗电子股份有限公司 | Temp. controlling box and use the liquid chromatography system of this temp. controlling box |
| CN205388592U (en) * | 2016-01-25 | 2016-07-20 | 北京博恩特药业有限公司 | Liquid accuse temperature high performance liquid chromatography column incubator |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022235752A1 (en) * | 2021-05-04 | 2022-11-10 | Waters Technologies Corporation | Compact liquid chromatography system providing thermal management and detection |
| CN113274764A (en) * | 2021-06-18 | 2021-08-20 | 中触媒新材料股份有限公司 | Liquid phase adsorption separation system and temperature control process method thereof |
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| CN108226364B (en) | 2020-08-11 |
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