CN102879483A - Supercutical fluid chromatograph (SFC) instrument and CO2 constant temperature apparatus used therein - Google Patents
Supercutical fluid chromatograph (SFC) instrument and CO2 constant temperature apparatus used therein Download PDFInfo
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- CN102879483A CN102879483A CN201110194677XA CN201110194677A CN102879483A CN 102879483 A CN102879483 A CN 102879483A CN 201110194677X A CN201110194677X A CN 201110194677XA CN 201110194677 A CN201110194677 A CN 201110194677A CN 102879483 A CN102879483 A CN 102879483A
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Abstract
The invention relates to a supercutical fluid chromatograph instrument which is composed of a liquefaction fluid tank, corrugated plate heat exchanger, a liquid CO2 delivery pump, a modifier delivery pump, a mixer, an automatic sample injector, a detector, an automatic back pressure regulator, a pressure sensor, a component collector, etc. When the instrument is at work, liquid fluid is guided into the liquid CO2 delivery pump through the corrugated plate heat exchanger, is mixed with the modifier outputted from the mixer and the modifier delivery pump, passes through the automatic sample injector and enters a chromatographic column for eluting the samples; each component of the samples is collected after being detected by the detector; and the critical state pressure of the supercutical fluid is controlled by the back pressure controller. Besides, the invention provides a liquid CO2 delivery pump head constant temperature tank which is used for a constant temperature cooling system (i.e. the corrugated plate heat exchanger) and is manufactured by semiconductor sheets.
Description
Technical field
The invention belongs to the preparation field of the products such as analytical instrument and biochemistry, medicine, is a kind of supercritical fluid high performance liquid chromatography tripping device.
Background technology
Supercritical fluid chromatography (SFC) is the chromatography take supercritical fluid as mobile phase.Supercritical fluid had both had near the viscosity of gas and high coefficient of diffusion, be about 10～100 times of liquid, have again high density and strong dissolving power near liquid, so SFC has both gas chromatography (GC) and both advantages of high performance liquid chromatography (HPLC).The used chromatographic stationary phases of SFC and liquid chromatography are similar, and mobile phase is generally the potpourri of carbon dioxide and organic solvent (methyl alcohol etc.).It not only can separate the difficult thermally labile that separates of GC, high molecular weight, strong polarity or non-volatile compounds, and can separate the high molecular weight compound that HPLC is difficult to separate.Supercritical fluid chromatography has that rate of propagation is faster, linear velocity is higher, multiple equilibria speed is faster, higher flux, viscosity are lower, Pressure Drop is little, flow velocity is high, can realize the advantages such as multicolumn sequence separation and can use widely in addition, especially its used supercritical fluid is generally carbon dioxide, compare with traditional liquid phase, the Discarded organic solvent that produces is few, pollute little, so this instrument has broad application prospects.
Supercritical fluid chromatograph is in fluid delivery process, and the state of fluid has some variations.Be CO such as fluid
2The time, CO
2Output will be lower than the pressure in the fluid reservoir, CO under the room temperature
2Can gasification, like this high pressure CO
2Flow velocity can be unstable when transfusion for ram pump.Because CO
2Critical point temperature be 30.98 ℃, the pressure of critical point is 7.377MPa, CO
2Out the pressure by reduction valve generally is set as 5MPA from fluid reservoir, and carbon dioxide will maintain liquid state, and its temperature then must maintain 5 ℃ of constant temperature, and temperature is excessive, CO
2Just gasification can affect the flow velocity of pump and the stability that system detects.
Therefore how with CO
2Temperature before the pump maintains 5 ℃ of constant temperature, makes CO
2Remaining on liquid state, is the difficult problem that equipment will solve.And existing thermostat adopts tube shell type structure, and its heat transfer efficiency is low, and the temperature difference of generation is large, makes the flow velocity of pump unstable.
Plate type heat exchanger is the ideal equipment that liquid-liquid, liquid-vapour carry out heat interchange.It has that heat exchange efficiency height, thermal loss are little, advantages of compact and light structure, installation easy to clean, be widely used, the characteristics such as long service life.Conductor refrigeration is a subject between Refrigeration Technique and semiconductor technology edge that grows up from the fifties, the P-N knot that it utilizes extraordinary semiconductor material to consist of, form thermopair pair, produce peltier effect, be i.e. a kind of New Refrigerating mode by the direct current refrigeration.Plate type heat exchanger and semiconductor refrigerating are widely used in having significant using value in the devices such as various refrigeration and heating at present.The present invention utilizes the advantage of the two, is applied in the supercritical fluid chromatograph, has successfully solved the constant problem of fluid temperature (F.T.) of keeping.
Summary of the invention
The purpose of this invention is to provide a kind of supercritical fluid chromatograph, utilize this chromatograph can be widely used in the biochemical separation and purification that waits material, and be used for this instrument at liquid CO
2A plate type heat exchanger and liquid CO between discharge pump and the fluid reservoir
2Carry the constant temperature oven by the semiconductor chip making of installing on the pump head.
To achieve these goals, the invention provides a kind of instrument for separation of products such as biochemistry, fluid through plate type heat exchanger, imports liquid CO by hold-up vessel during work
2In the discharge pump, after modifier mixed, the automatic sampler of flowing through after sample injects chromatographic column by injector, entered analytic sample in the chromatographic column, collects each component in the sample after device detects after testing.Wherein the back pressure controller is controlled the pressure of whole system.
The present invention relates to a kind of temperature controller---plate type heat exchanger is controlled fluid and is entered liquid CO
2Temperature before the discharge pump.Corrugated cardboard sheet heat interchanger of the present invention comprises: O-ring seal, overhead gage, lower baffle plate and be clipped in wherein heat exchange plate; Heat exchange plate is rearranged by a plurality of, is distributed with the convex ripple on it, and forms heat exchanger channels between adjacent heat exchange plate, guarantees high pressure-bearing and high heat exchange efficiency.For increasing log-mean temperature difference and heat transfer coefficient, adopt hot and cold matchmaker's counter-flow arrangement.Thermal medium enters heat exchanger plates uniformly, flows therein and heat exchange.Cold media enters in the rear heat exchanger plates that is assigned to uniformly between each heat exchanger plates that contains thermal medium, carries out heat exchange with heating agent, and outflow equipment.
The present invention relates in addition a kind of constant temperature oven, this constant temperature oven is comprised of semiconductor chilling plate and heating radiator, when flow through liquid CO
2During the discharge pump pump head, utilize the thermolysis of semi-conductive refrigeration and heating radiator to keep the constant of temperature.
Description of drawings
Fig. 1 is the structural representation of the integral body of supercritical fluid chromatography separation equipment among the present invention
As shown in the figure: 1, CO
2Storage tank 2, reduction valve 3, tensimeter 4, plate type heat exchanger 5, modifier pump 6, liquid CO
2Discharge pump 7, mixer 8, automatic sampler 9, chromatographic column and column oven 10, detecting device 11, back pressure device 12, gatherer.
Fig. 2 is liquid CO of the present invention
2The front elevation of discharge pump
As shown in the figure: 1, plate type heat exchanger 2, temperature controller 3, liquid CO
2Discharge pump control panel 4, liquid CO
2The discharge pump pump head
Fig. 3 is the structural drawing of plate type heat exchanger of the present invention
As shown in the figure: 1, O-ring seal 2, overhead gage 3, heat exchange plate 4, lower baffle plate
Fig. 4 is liquid CO among the present invention
2The Semi-conductive thermostat top plan view of discharge pump pump head
As shown in the figure: 5, high pressure CO
2Pump head constant temperature oven 6, semiconductor chilling plate 7, heating radiator
Fig. 5 is the structural drawing of semiconductor chilling plate
As shown in the figure: 1, cold junction 2, P-type semiconductor 3, N-type semiconductor 4, hot junction
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
1 embodiments of the present invention are described by reference to the accompanying drawings.At first, description of drawings be used for supercritical fluid chromatography equipment of the present invention.It mainly comprises: as the CO of feeder
2Storage tank 1; The reduction valve 2 of adjustments of gas pressure; Tensimeter 3; Be used for keeping CO
2The thermostat plate type heat exchanger 4 of temperature; Modifier pump 5 for delivery of organic solvent; Liquid CO for delivery of supercritical fluid
2Discharge pump 6; Be used for the mixer 7 with supercritical fluid and solvent; Be used for sample is injected the automatic sampler 8 that mobile phase is done; For separating of the chromatographic column and the column oven 9 that inject the sample desired substance; For detection of the detecting device 10 by the material in the mobile phase of chromatographic column; Back pressure device 11 as pressure adjustment assembly; Be used for storing the gatherer 12 of the liquid that separates through supercritical fluid.
Described CO
2Storage tank 1, reduction valve 2, tensimeter 3, plate type heat exchanger 4, liquid CO
2Discharge pump 6, mixer 7, automatic sampler 8, chromatographic column and constant temperature oven 9, detecting device 10 and back pressure device 11 are linked in sequence by pipeline.Modifier pump 5 is by pipeline and liquid CO
2Discharge pump 6 parallel connections.Still there are in this embodiment some external device should join the correct position of device, although it is not expressed.
CO
2From storage tank, discharge through reduction valve 2 and tensimeter 3 and arrive plate type heat exchanger 4, keep herein liquid condition, liquid CO
2Be connected with semiconductor chilling plate on the pump head of discharge pump 6, make CO
2Reach Supercritical Conditions, the organic solvent of carrying with modifier pump 5 is mixed into the supercritical fluid that mixes at mixer 7, the sample delivery that to inject from automatic sampler 8 and is separated the various materials in the sample on chromatographic column 9 according to its approach by chromatographic column.The material that has passed through in the movement mutually of chromatographic column is detected by detecting device 10, uses gatherer 12 to collect according to testing result.The movement of having passed through detecting device is transported to counterbalance valve 11 mutually, and is mobile mutually by its pressure decreased behind the counterbalance valve.
In this embodiment, used plate heat exchanger device, having comprised: O-ring seal 1, overhead gage 2, lower baffle plate 4 and be clipped in wherein heat exchange plate 3; Heat exchange plate is rearranged by a plurality of, is distributed with the convex ripple on it, and forms heat exchanger channels between adjacent heat exchange plate, guarantees high pressure-bearing and high heat exchange efficiency.Adopt hot and cold matchmaker's counter-flow arrangement, cold and hot exchange is to advance by diagonally opposing corner, and diagonally opposing corner goes out.Thermal medium enters heat exchanger plates uniformly, flows therein and heat exchange.Cold media enters in the rear heat exchanger plates that is assigned to uniformly between each heat exchanger plates that contains thermal medium, carries out heat exchange with heating agent, and outflow equipment.Every layer of heat exchange plate has O-ring seal, has both guaranteed the medium of two kinds of temperature, can pass through in cross-stratum, has guaranteed again mutually dissolving of two media.
In addition, in this embodiment, used the semiconductor refrigerating sheet devices.N.P type semiconductor links by metal deflector, when electric current passes through P-type semiconductor 2 by N-type semiconductor 3, electric field makes electronics in the N-type semiconductor and the hole reversed flow in the P-type semiconductor, the energy that they produce is from the heat energy of lattice, so absorb heat at flow deflector (cold junction 1), and in the other end (hot junction 4) heat release, produce the temperature difference.Then the heat that is higher than chip in hot junction 4 dissipates by heat radiator.
Above-described embodiment is used for explaining the present invention, rather than limits the invention, and in spirit of the present invention and claim protection domain, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (3)
1. supercritical fluid chromatograph device is by liquefaction fluid tank, corrugated cardboard sheet heat interchanger, liquid CO
2The compositions such as discharge pump, modifier discharge pump, mixer, automatic sampler, detecting device, automatic back pressure regulator, pressure transducer, component gatherer.It is characterized in that: liquid CO
2Between discharge pump and the liquefaction fluid tank individual corrugated cardboard sheet heat interchanger is arranged, when its hold-up vessel is derived, be in critical temperature, simultaneously liquid CO to guarantee fluid liquid
2The discharge pump pump head is provided with constant temperature oven, guarantees equally the critical temperature of fluid, and this constant temperature oven is made by semiconductor chip.
2. method according to claim 1, wherein said liquid CO
2Between discharge pump and the fluid liquid tank individual heat interchanger is arranged, this heat interchanger is a kind of plate type heat exchanger.
3. method according to claim 1, wherein said liquid CO
2Carrying the pump head constant temperature oven is that semiconductor material is made.Formed by semiconductor chilling plate and heating radiator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110194677XA CN102879483A (en) | 2011-07-13 | 2011-07-13 | Supercutical fluid chromatograph (SFC) instrument and CO2 constant temperature apparatus used therein |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110194677XA CN102879483A (en) | 2011-07-13 | 2011-07-13 | Supercutical fluid chromatograph (SFC) instrument and CO2 constant temperature apparatus used therein |
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|---|---|
| CN102879483A true CN102879483A (en) | 2013-01-16 |
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| CN201110194677XA Pending CN102879483A (en) | 2011-07-13 | 2011-07-13 | Supercutical fluid chromatograph (SFC) instrument and CO2 constant temperature apparatus used therein |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105987968B (en) * | 2015-03-18 | 2018-10-26 | 株式会社岛津制作所 | Liquefied carbon dioxide liquid-feeding pump and the supercritical fluid chromatograph for having the pump |
| US10451049B2 (en) | 2015-03-18 | 2019-10-22 | Shimadzu Corporation | Liquid carbon dioxide delivery pump, and supercritical fluid chromatograph provided with the same |
| CN113549305A (en) * | 2021-06-04 | 2021-10-26 | 浙江工业大学 | Full-biodegradable modified PBAT foamed sheet and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105987968B (en) * | 2015-03-18 | 2018-10-26 | 株式会社岛津制作所 | Liquefied carbon dioxide liquid-feeding pump and the supercritical fluid chromatograph for having the pump |
| US10451049B2 (en) | 2015-03-18 | 2019-10-22 | Shimadzu Corporation | Liquid carbon dioxide delivery pump, and supercritical fluid chromatograph provided with the same |
| CN113549305A (en) * | 2021-06-04 | 2021-10-26 | 浙江工业大学 | Full-biodegradable modified PBAT foamed sheet and preparation method and application thereof |
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Application publication date: 20130116 |