CN103376293A - Supercritical fluid chromatograph (SFC) and precise fluid divider applying same - Google Patents
Supercritical fluid chromatograph (SFC) and precise fluid divider applying same Download PDFInfo
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- CN103376293A CN103376293A CN2012101143573A CN201210114357A CN103376293A CN 103376293 A CN103376293 A CN 103376293A CN 2012101143573 A CN2012101143573 A CN 2012101143573A CN 201210114357 A CN201210114357 A CN 201210114357A CN 103376293 A CN103376293 A CN 103376293A
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Abstract
The invention discloses a semipreparation/preparation type supercritical fluid chromatograph. The semipreparation/preparation type supercritical fluid chromatograph comprises a liquifying fluid tank, a pressure reducing valve, a pressure meter, a plate type heat exchanger, a liquified CO2 conveying pump, a modifier conveying pump, a mixer, an automatic sampler, a precise fluid divider, a detector, an automatic back-pressure adjuster, a pressure sensor and a component collector. In an operation process of the instruments, large-flow fluid can enter detectors such as a variable-wavelength detector (VWD), a photoelectric diode array detector (DAD), a hydrogen flame ionization detector (FID), a nitrogen-phosphorus detector (NPD) and a mass spectrometer (MS) to carry out subsequent detecting procedure after precise fluid division is carried out. At the present, companies such as Water and jasco adopt manual fluid dividing devices with fussy operation and difficult control. The semipreparation/preparation type supercritical fluid chromatograph disclosed by the invention has the advantages that a self-developed precise fluid divider is adopted, a stepping motor drives a metering rod to move up and down, and the metering rod can be in transitional matching with an adjustable rod bushing in a moving process to change the resistance of flow channels, so that the flow percent of fluids in two flow channels is controlled and the precise fluid dividing ratio is achieved.
Description
Technical field
The invention belongs to the scientific instruments equipment field of the preparation product such as biochemical, medical, particularly is a kind of accurate part flow arrangement for supercritical fluid chromatography.
Background technology
Supercritical fluid chromatography (supercritical fluid chromatography, be called for short SFC) be with supercritical fluid (a kind of state of material when being higher than emergent pressure and critical temperature, it have gas low viscosity, liquid high density and between gas, liquid higher features such as coefficient of diffusion) be mobile phase, take solid adsorbent or be bonded to superpolymer on the carrier as the fixing chromatogram of phase.SFC is the important supplement of gas chromatography (GC) and liquid chromatography (LC), have efficient, fast, the characteristics such as environmental protection.
Supercritical fluid chromatography adopts CO
2As mobile phase, in separating preparation process, can keep well the activity of target compound, in the separation such as the homolog of chipal compounds, structural similarity and isomeride, low pole compound, have unrivaled advantage than other method.Supercritical fluid chromatograph (SFC) can be widely used in analysis, the separation and purification of the aspects such as biological medicine, environmental protection, petrochemical complex, high molecular polymer, Coal Chemical Industry, dyestuff and agricultural chemicals, except fraction material (material, inorganic salts and molecular weight can only be water-soluble or that need the dissolving of buffer solution or water-soluble Ion reagent greater than 15000 material) is not suitable for the supercritical fluid chromatography, other materials are all available.
SFC can be divided into analysis SFC and preparation type SFC.Analytic type SFC, because the flow of fluid is little, and supercritical CO
2Behind counterbalance valve, be gasificated into gaseous state, can be directly and variable-wavelenght detector (VWD), photodiode array detector (DAD), flame ionization ditector (FID), nitrogen phosphorous detector (NPD), the connections such as mass spectrum (MS), but for half preparation, preparation type SFC, the flow of fluid is larger, can not directly link to each other with above-mentioned detecting device, after flow goes out chromatographic column, must carry out accurate shunting to it, the above-mentioned detecting device of being allowed for access carries out testing.CO after the shunting
2Gasify through behind the automatic counterbalance valve, be directly connected to the detecting devices such as ELSD, MS, FID, NPD.Therefore, how to supercritical CO
2Accurately shunting is to need to solve an important problem in the research of Supercritical fluid chromatography instrument.
Summary of the invention
The purpose of this invention is to provide a kind of accurate shunt that is applied in the half preparation/preparation type supercritical fluid chromatograph, utilize this precision shunt, after success is shunted the fluid of large flow, it is directly entered in the detecting devices such as ELSD, MS, FID, NPD, carry out follow-up testing.
The present invention relates to an accurate shunt---drive gauge stick by stepper motor and move up and down, gauge stick is in mobile process and between the adjustable rod lining transition fit occurs, change flow passage resistance force of waterproof, thereby control the flow percentage of the fluid of two subchannels, reach the accurate split ratio of fluid.
Description of drawings
Fig. 1 represents 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 discharge pump 6, liquid CO
2Discharge pump 7, mixer 8, automatic sampler 9, chromatographic column and column oven 10, shunt 11, back pressure device 12, detecting device 13, gatherer
Fig. 2 represents the structure of accurate shunt of the present invention
As shown in the figure: 1, gauge stick 2, replaceable inlet filter 3, inlet 4, adjustable thread bar 5, stepper motor input shaft 6, replaceable outlet liquid core 7, low speed shunting liquid outlet 8, high speed are shunted liquid outlet 9, adjustable rod lining.
Embodiment
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 discharge 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; The shunt 10 that is used for the accurate shunting of large flow fluid; Back pressure device 11 as pressure adjustment assembly; For detection of the detecting device 12 by the material in the mobile phase of chromatographic column; Be used for storing the gatherer 13 of the liquid that separates through supercritical fluid.
CO
2From storage tank 1, discharge through reduction valve 2 and tensimeter 3 and arrive plate type heat exchanger 4, liquid CO
2Be connected with semiconductor chilling plate on the pump head of discharge pump 6, make CO
2Reach Supercritical Conditions, the modifier of carrying with modifier discharge pump 5 is mixed into the mobile phase of supercritical fluid chromatograph at mixer 7, and sample enters chromatographic column 9 through automatic sampler 8, and then obtains separating.After sample flow goes out chromatographic column, behind accurate shunt shunting 10 and counterbalance valve 11, advance detecting device 12 and detect, use gatherer 13 to collect according to this testing result.
In this embodiment, adopt stepper motor to drive gauge stick 1 and move up and down, transition fit and occurs between the adjustable rod lining 9 in gauge stick in mobile process, changed the fluid space size, thereby affected split ratio.Solution enters from inlet 3, behind replaceable inlet filter 2 and adjustable rod lining 9, respectively from low speed liquid outlet 7, the 8 proportional outflows of high speed liquid outlet.By stepper motor input shaft 5 accurate rotational angles, two screw thread controls of adjustable thread bar 4 form very accurate split ratio.
The principle of work of shunting adjustable precision device is equivalent to ohm circuit fast.Comprise the path in parallel that two resistors (high speed liquid outlet 8, low speed liquid outlet 7) consist of, large flow enters liquid and passes fixing inlet filter 2 through inlet, adjustable rod lining 9, and two fluid resistance ratios of generation have been created split ratio.Because flow is directly proportional indirectly with resistance, changes the flow passage resistance force of waterproof result and also changed split ratio.Change inlet filter, for parallel route different resistance earning rates will be arranged.The variation meeting of flow and viscosity produces pressure at divider, but this does not affect actual split ratio.Because the liquid resistance of extremely low internal volume, solvent composition is the same at two resistors at any crash time, is not affect the gradient split ratio so the variation of viscosity links together.
Constantly adjust kapillary and compare for the split ratio optimization with tradition, the single pipeline of liquid condenser utilization can reach the split ratio of wanting, and split ratio is stable and reproducible, is not subjected to the impact of viscosity or pressure; Quick shunting adjustable flow prepares divider can carry out accurate direct control to split ratio; Simple to operate, the changeable liquid damper reaches the split ratio of wanting.Utilize simultaneously stepper motor can reach more accurate split ratio to the control of its gauge stick.
Claims (3)
1. one and half preparation/preparation type supercritical fluid chromatographs are by liquefaction fluid tank, reduction valve, tensimeter, plate type heat exchanger, liquid CO
2Discharge pump, the modifier discharge pump, mixer, automatic sampler, accurate shunt, detecting device, automatic back pressure regulator, pressure transducer, the component gatherer forms.
2. half preparation/preparation type supercritical fluid chromatograph according to claim 1, it is characterized in that: in half preparation/preparation type supercritical fluid chromatograph, the flow of fluid is larger, after chromatographic column is separated, after need carrying out accurate shunting, carry out follow-up testing in the detecting devices such as the variable-wavelenght detector of being allowed for access (VWD), photodiode array detector (DAD), flame ionization ditector (FID), nitrogen phosphorous detector (NPD), mass spectrum (MS).
3. method according to claim 1, wherein said accurate shunt is to drive gauge stick by stepper motor to move up and down, gauge stick is in mobile process and between the adjustable rod lining transition fit occurs, change flow passage resistance force of waterproof, thereby control low speed shunting liquid outlet and high speed are shunted the flow percentage of the fluid of liquid outlet two subchannels, reach the accurate split ratio of fluid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101143573A CN103376293A (en) | 2012-04-18 | 2012-04-18 | Supercritical fluid chromatograph (SFC) and precise fluid divider applying same |
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| CN2012101143573A CN103376293A (en) | 2012-04-18 | 2012-04-18 | Supercritical fluid chromatograph (SFC) and precise fluid divider applying same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442821A (en) * | 2016-09-28 | 2017-02-22 | 泉州市晋科技术检测有限公司 | Shunting device for combined use of supercritical fluid chromatograph and mass spectrometer |
| CN106662554A (en) * | 2014-08-28 | 2017-05-10 | 株式会社岛津制作所 | Analysis device |
| CN108780026A (en) * | 2016-04-15 | 2018-11-09 | 耶鲁大学 | Systems, devices and methods for monitoring the organic compound in gaseous environment |
Citations (3)
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| CN2150559Y (en) * | 1992-10-28 | 1993-12-22 | 孙云鹏 | Accessory of super-critical fluid extraction injector |
| JP2007120972A (en) * | 2005-10-25 | 2007-05-17 | Jasco Corp | Supercritical system |
| US20090049891A1 (en) * | 2005-02-25 | 2009-02-26 | Mohamed Shaimi | Supercritical-Phase Mixed Chromatography Method and Installation for Implementing Same |
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2012
- 2012-04-18 CN CN2012101143573A patent/CN103376293A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2150559Y (en) * | 1992-10-28 | 1993-12-22 | 孙云鹏 | Accessory of super-critical fluid extraction injector |
| US20090049891A1 (en) * | 2005-02-25 | 2009-02-26 | Mohamed Shaimi | Supercritical-Phase Mixed Chromatography Method and Installation for Implementing Same |
| JP2007120972A (en) * | 2005-10-25 | 2007-05-17 | Jasco Corp | Supercritical system |
Non-Patent Citations (2)
| Title |
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| MICHEL PERRUT: "Advances in supercritical fluid chromatographic processes", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 赵锁奇等: "硅胶柱超临界流体制备色谱分离极性化合物", 《西北大学学报（自然科学版）》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106662554A (en) * | 2014-08-28 | 2017-05-10 | 株式会社岛津制作所 | Analysis device |
| CN106662554B (en) * | 2014-08-28 | 2019-04-02 | 株式会社岛津制作所 | Analytical equipment and analysis method |
| CN108780026A (en) * | 2016-04-15 | 2018-11-09 | 耶鲁大学 | Systems, devices and methods for monitoring the organic compound in gaseous environment |
| US11125732B2 (en) | 2016-04-15 | 2021-09-21 | Yale University | System, apparatus, and method for monitoring organic compounds in a gas environment |
| US11614431B2 (en) | 2016-04-15 | 2023-03-28 | Yale University | System, apparatus, and method for monitoring organic compounds in a gas environment |
| CN106442821A (en) * | 2016-09-28 | 2017-02-22 | 泉州市晋科技术检测有限公司 | Shunting device for combined use of supercritical fluid chromatograph and mass spectrometer |
| CN106442821B (en) * | 2016-09-28 | 2018-12-14 | 泉州市晋科技术检测有限公司 | Part flow arrangement associated with a kind of supercritical fluid chromatograph and mass spectrograph |
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Application publication date: 20131030 |