CN106730998A - A kind of distributor in liquid-phase chromatographic column - Google Patents
A kind of distributor in liquid-phase chromatographic column Download PDFInfo
- Publication number
- CN106730998A CN106730998A CN201710094906.8A CN201710094906A CN106730998A CN 106730998 A CN106730998 A CN 106730998A CN 201710094906 A CN201710094906 A CN 201710094906A CN 106730998 A CN106730998 A CN 106730998A
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- CN
- China
- Prior art keywords
- chromatographic column
- distributor
- chromatographic
- sieve plate
- liquid
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/14—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
-
- 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
- G01N30/6004—Construction of the column end pieces
- G01N30/6017—Fluid distributors
-
- 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
Abstract
The present invention be it is a kind of can change mobile phase in liquid-phase chromatographic column and migrate the device of state, the device be may be mounted at after chromatographic column arrival end sieve plate or before port of export sieve plate, and inequality in chromatographic column is weakened to a certain extent, is conducive to improving post and is imitated.Distributor is made up of central solid region and peripheral permeable region, and wherein outer peripheral areas are the annular porous structures concentric with central area.The device can be under conditions of original chromatographic column structure and separating technology parameter not be changed, lifting chromatographic column integral post effect, it is applied widely, as the new structural member in a kind of liquid-phase chromatographic column, it is with a wide range of applications in the application field of analytic type chromatogram and preparative scale chromatography.
Description
Technical field
The present invention relates to chromatographic technology field, and in particular to a kind of distributor in liquid-phase chromatographic column.
Background technology
Liquid chromatography technology is that one kind efficiently separates purification technique, is widely applied in many fields, such as：Chemical industry,
Biology, food, medicine etc..Wherein, chromatographic column is the core of liquid chromatogram, is to realize the main place that material is separate, energy
The performance for isolating and purifying is directly affected, is all the time core and the forward position of liquid chromatography technology research field.
The separating effect of chromatographic column is depending on the property of fixing phase and its power interacted with solute (mainly by separating
The property of medium is determined)；Meanwhile, also with widening about (the main flow regime institute by mobile phase inside chromatographic column
Determine, and good flow regime can promote the uniform adsorption of media on target thing, improve post effect).Traditional chromatographic theory
Assuming that chromatographic column is homogeneous, it is believed that the flow velocity of mobile phase is equally distributed, the chromatographic peak of Pulsed Sampling inside chromatographic column
Shape is approximate " rectangle ".But increasing research finds that the flow velocity of mobile phase is different in different radial distances.It is logical
Very close to the low 2%-8% of flow velocity of the velocity ratio central area at chromatographic column post jamb, velocity flow profile parabolically shape, analyte bar
Approximate " the Gaussian Profile of band actual flow pattern in chromatographic column.It is that one, chromatogram research field is not allowed for the research of radial direction inequality
Ignorance problem.
1966, Knox et al. disclosed common filled-type chromatographic column and there is radial direction heterogeneity by the method for local detection
Property.Afterwards, the inhomogeneity of the chromatographic column such as integral post is confirmed successively.Research shows：Mobile phase linear flow rate, chromatographic column office
There is radial direction inhomogeneity in the local concentration of portion post effect and determinand, the relation of these values and radial position parabolically shape
Shape.Wherein, the linear flow rate at chromatographic column post jamb is lower than central region flow velocity by about 2%~8%, and occurrence depends on filling
Property；The component efficiency highest of chromatographic column central area；Analyte concentration shows certain in the radial direction in chromatographic column
Fluctuation.
Then, G.Guiochon researchs show to imitate chromatographic column higher for post, and inhomogeneity influences bigger to it；And
In card actual efficiency highest chromatographic column, the difference that gained local velocity, component efficiency and analyte local concentration show is most
It is small.
Tivadar Farkas etc. are examined by the continuation to column outlet end section various location analyte concentration
Survey and the radial direction inequality phenomenon of chromatographic column is studied.Experimental result demonstrate again that radial direction inequality phenomenon in AG and
Generally existing in preparation scale chromatographic column.In the chromatography column, central area (in the range of about 1/2nd diameters) are relatively uniform
, and borderline region in addition is that, with inequality, and the scope of borderline region is not changeless.In analysis
In level chromatographic column, borderline region distance about in the range of 30-50 times of media diameters, and for large scale chromatographic column,
This distance can be bigger.Between the two without obvious border.
D.V.Dusschoten et al. thinks that the post effect of chromatographic column depends on the radially uniform property of chromatographic column, fills close
The localised waving of degree can corresponding affect on local porosity, permeability and chromatographic column keeping characteristics.
The radial direction inequality of chromatographic column directly results in analyte band distance stretching diametrically, causes chromatographic peak to become
Width, hangover increases, column efficiency reduction.And this radial direction inequality is generally existing and is difficult to eliminate, column efficiency
Chromatographic column higher, the influence that its radial direction inequality is brought is bigger.
In order to the post for further improving chromatographic column is imitated, many researchs at present are placed on research emphasis the innovation of chromatographic media
On, post effect is improved by changing the performance of separating medium；Also some researchs pay close attention to the improvement of this body structure of chromatographic column, such as：
Taper chromatographic column, expansion bed, chromatographic cake etc..Obtained extensively by a kind of active flow chromatography technology of the propositions such as Camenzuli in the recent period
General accreditation and research.The core design of this brand new ideas is the fluid segmentation ring and supporting for being located at chromatographic column port
Piecing devices.Segmentation ring is a structure for donut, and its core and outer peripheral portion is normal permeable porous material
Material, and a ring of centre is non-permeable peek materials.Matching is special termination design, middle permeable part with
The centre bore of joint is connected, and the permeable part of annulus periphery communicates with three holes for being distributed in joint periphery, so i.e. can be with
Mobile phase is divided into two parts：Outer peripheral portion and core.This technology is respectively placed in the arrival end of chromatographic column and goes out
Mouth end can obtain two kinds of different application theories.When segmentation ring structure is placed in the arrival end of chromatographic column, if taken therefrom
The mode of heart hole sample introduction, then analyte band is to be not exposed to chromatographic column borderline region within the starting stage for entering chromatographic column
, this just can effectively be avoided influence of the boundary effect to analyte band, reduce the influence of radial direction inequality, so as to improve
The separating effect of chromatographic column.When this structure is placed in the port of export of chromatographic column, central area can be only collected in sampling
Sample, can thus exclude is influenceed larger borderline region, great optimizing detection peak by radial direction inequality.But this method is only
It is suitable for analytic type chromatographic column, and there is certain error during for needing quantitative.
Mobile phase distributes the function of fluid by sieve plate after entering in chromatographic column, and mobile phase enters color with parallel planar
In spectrum post, its flow regime is determined by the property and occupied state of interior media.And research shows, flow regime is straight in chromatographic column
Influence its column efficiency is connect, therefore, by changing chromatographic column internal structure, so as to change in chromatographic column flow regime to improve chromatogram
Column efficiency.With theoretical foundation and feasibility.
The content of the invention
It is an object of the invention to by adding a chromatographic column after the arrival end sieve plate in chromatographic column or before port of export sieve plate
Interior distributor changes the migration state of mobile phase in chromatographic column, weakens the radial direction inequality of liquid flow pattern in chromatographic column,
The parabola flow pattern of mobile phase script in chromatographic column can be made to become approximately " stopper " flow pattern, so as to weaken because of bands of a spectrum exhibition in chromatographic column
The asynchronous peak stretching for causing wide or peak are asymmetric, improve post effect.
Currently invention addresses chromatographic column the inner mouth structure, by after the arrival end sieve plate in chromatographic column or port of export sieve plate
Distributor in a preceding plus chromatographic column, changes the migration state of mobile phase in chromatographic column.The distributor is by making chromatographic column
Inner fluid speed faster turn back by longer flow distance by central area, realizes and the slower periphery of flow velocity (nearly wall) region
Converge, optimization chromatographic column enter, port of export interior flow field, so as to weaken the radial direction inequality of liquid flow pattern in chromatographic column.And can
With the column length according to chromatographic column, post footpath adjusts the waterproof area size of the distributor so that the parabola flow pattern of script is adjusted
It is approximate " stopper " flow pattern to save, and weakens the influence of widening in chromatographic column, and optimizing detection chromatographic peak profile improves dividing for chromatographic column
From efficiency.No matter distributor in the chromatographic column is tried out, and equal to qualitative, quantitative for analytic type or preparative scale chromatography
Without influence, make simple, easily operation, effect is significant is with a wide range of applications.
Brief description of the drawings
Fig. 1：The structural representation of the distributor in chromatographic column of the present invention：Central area is impermeable material, by branch
Frame is fixed in peripheral circles.
Fig. 2：The structural representation of the distributor in chromatographic column of the present invention：Central area is impermeable material, external zones
Domain is porous network structure.
Fig. 3：The chromatographic column of distributor (the waterproof a diameter of 3.0mm in region) is added to be contrasted with common chromatographic column peak shape
Figure.
Fig. 4：The chromatographic column of distributor (the waterproof a diameter of 6.0mm in region) is added to be contrasted with common chromatographic column peak shape
Figure.
Specific embodiment
The present invention devises the distributor in a kind of chromatographic column, by the way that after chromatographic column arrival end sieve plate, the port of export is sieved
This distributor is added before plate, thus it is possible to vary the migration state of mobile phase in chromatographic column, weakened in chromatographic column to a certain extent
The radial direction inequality of mobile phase flow pattern, weaken because in chromatographic column widening it is asynchronous caused by chromatogram peak stretching or peak it is not right
Claim, so as to improve detection spectrogram quality, improve post effect.By the size for changing the impermeable water section of distributor, it is possible to achieve right
Different post footpaths, the flow pattern regulation of the chromatographic column of column length, effectively improve the peak shape quality of detection chromatogram, improve post effect.
Distributor just in chromatographic column of the present invention, coordinates instantiation to describe in detail as follows below：
Example：
Embodiment 1：It is 4.6mm by internal diameter, length is turned on for the column cap of the chromatographic column column jecket arrival end of 150mm, removes it
Middle pad and sieve plate, with commerical grade silica gel that particle diameter is 10 μm as filled media, load in the space between chromatographic column tube wall,
When loading full, the distributor in the chromatographic column of a diameter of 3.0mm in waterproof region is installed, then install sieve plate, filled
Upper gasket and chromatographic column arrival end column cap, are then connected the chromatographic column for being provided with distributor by standard colour chart post interface
Tested and analyzed on liquid chromatograph.Simultaneously using the common chromatographic column for being not added with the distributor of identical size of outer tube as control
Do same detection.Experimental result is as shown in table 1 and accompanying drawing 3.
Table 1：The theoretical cam curve of common chromatographic column and the chromatographic column for adding distributor is with change in flow trend
Note：N0, NnThe theoretical cam curve of common chromatographic column and the Novel chromatographic column equipped with distributor is represented respectively.
Embodiment 2：It is 12mm by internal diameter, length is turned on for the column cap of the chromatographic column column jecket port of export of 80mm, removed wherein
Pad and sieve plate, with commerical grade silica gel that average grain diameter is 75 μm as filled media, fill in the space between chromatographic column tube wall
Fill out, when loading full, install the distributor in the chromatographic column of a diameter of 6.0mm in waterproof region, then install sieve plate,
Pad and column outlet newel post head are loaded onto, then connects the chromatographic column for being provided with distributor by standard colour chart post interface
It is connected on liquid chromatograph and tests and analyzes, while using the common chromatographic column for being not added with distributor of identical size of outer tube as control
Do same detection.Experimental result is as shown in table 2 and accompanying drawing 4.
Table 2：The theoretical cam curve of common chromatographic column and the chromatographic column for adding distributor is with change in flow trend
Note：N0, NnThe theoretical cam curve of common chromatographic column and the Novel chromatographic column equipped with distributor is represented respectively.
Claims (6)
1. a kind of distributor in liquid-phase chromatographic column, the device can change the migration state of mobile phase in chromatographic column,
Weaken the radial direction inequality in chromatographic column, reduce the influence that inequality is imitated to post.The apparatus main body structure is circular framework, in
Heart solid area and peripheral permeable region are constituted, and can be obtained not by the different proportion of central area and chromatographic column internal diameter size
Same chromatographic behavior.
2. the distributor in chromatographic column according to claim 1, it is characterised in that the waterproof region in center and chromatographic column
Pipe is concentric, and its size is the 0.1-0.8 of chromatogram column internal diameter.
3. the distributor in chromatographic column according to claim 1, it is characterised in that the thickness of distributor is 0.1-3.0
Millimeter.
4. the distributor in chromatographic column according to claim 1, it is characterised in that can be placed in the entrance point of chromatographic column
Sieve plate lower section, or port of export sieve plate top, detachably.
5. the distributor in chromatographic column according to claim 1, it is characterised in that connection center impervious zone and periphery
The support number of annulus is more than or equal to 3, or outer peripheral areas are porous network structures.
6. the distributor in the chromatographic column according to claim 1-3, it is characterised in that center impervious zone and support
Material is including but not limited to stainless steel, lucite, the material without specific adsorption such as polytetrafluoroethylene (PTFE).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710094906.8A CN106730998A (en) | 2017-02-22 | 2017-02-22 | A kind of distributor in liquid-phase chromatographic column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710094906.8A CN106730998A (en) | 2017-02-22 | 2017-02-22 | A kind of distributor in liquid-phase chromatographic column |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106730998A true CN106730998A (en) | 2017-05-31 |
Family
ID=58957583
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710094906.8A Pending CN106730998A (en) | 2017-02-22 | 2017-02-22 | A kind of distributor in liquid-phase chromatographic column |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110208445A (en) * | 2019-07-09 | 2019-09-06 | 常州三泰科技有限公司 | Liquid-phase chromatographic column column tube and liquid-phase chromatographic column |
| CN111182952A (en) * | 2017-08-31 | 2020-05-19 | 菲诺米耐斯公司 | Chromatographic column with locked packed bed and packing method thereof |
-
2017
- 2017-02-22 CN CN201710094906.8A patent/CN106730998A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111182952A (en) * | 2017-08-31 | 2020-05-19 | 菲诺米耐斯公司 | Chromatographic column with locked packed bed and packing method thereof |
| CN110208445A (en) * | 2019-07-09 | 2019-09-06 | 常州三泰科技有限公司 | Liquid-phase chromatographic column column tube and liquid-phase chromatographic column |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170531 |
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| WD01 | Invention patent application deemed withdrawn after publication |