CN101632878B - Distribution method and distribution device of mobile phases of chromatographic columns - Google Patents
Distribution method and distribution device of mobile phases of chromatographic columns Download PDFInfo
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- CN101632878B CN101632878B CN2009101700132A CN200910170013A CN101632878B CN 101632878 B CN101632878 B CN 101632878B CN 2009101700132 A CN2009101700132 A CN 2009101700132A CN 200910170013 A CN200910170013 A CN 200910170013A CN 101632878 B CN101632878 B CN 101632878B
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Abstract
The invention discloses a distribution method and a distribution device of mobile phases of chromatographic columns. The distribution method comprises the steps: adopting a circular distributor matched with a cross section for preparing a chromatographic column; divergently arranging distribution liquid paths of liquid phases outwards in a tree shape along the center on the distributor; installing a distribution hole on the end of each distribution liquid path of liquid phases, wherein the lengths from the center of the distributor to the same-specification distribution liquid paths of liquid phases of all the distribution holes are equal; evenly distributing the liquid phases from the center of the distributor along each distribution liquid path of liquid phases to each distribution hole; and then evenly distributing the liquid phases to fixed phases of chromatographic columns. The distribution method can effectively eliminate the defect that the residence times of the mobile phases on a distribution system have serious differences along with the increase of the diameters of the chromatographic columns, can realize the even initial distribution of the mobile phases entering the chromatographic columns and can not be influenced by the high-pressure transport of the mobile phases. The distribution device has the advantages of simple structural design, difficult blockage, easy washing and repeated use.
Description
Technical field
The invention belongs to the distribution technique of flowing phase in the chromatographic column that preparing chromatograph in industry uses, concrete relate to a kind of flowing phase distribution method and distributor thereof that is specially adapted to large diameter chromatographic column.
Background technology
The main purpose of preparing chromatograph in industry is from mixture, to obtain pure material.In order to accelerate the efficient that separation time is separated with raising; The preparative chromatography device to advance sample size very big, cause the corresponding increasing of the segregational load of preparative chromatography post, also just must strengthen chromatographic column filler; Increase the diameter and the length of preparative chromatography, many relatively flowing phase of use.After pending liquid is injected into chromatographic column; Move in fixing mutually through pressure; Because different material is different with the interaction of fixing phase in the pending liquid; Different materials leaves chromatographic column in proper order, obtains different peak-to-peak signals through detector, the material of judging that through these signals of analysing and comparing trickle contains at last.
Mostly the employed chromatographic column of preparing chromatograph in industry is vertical tubular body, in this tubular body, is provided with the packed bed that porous particle is formed.Carrying out uniform fluid distribution to packed bed is the important technology in the preparing chromatograph in industry, and desirable fluid distributing apparatus can be introduced liquid fluid on the whole surface at the top of packed bed uniformly, and flows through on the packed bed cross section with identical speed.If the distribution of this liquid fluid phase exists the top of packed bed to have uneven situation, will cause the dispersion of same substance in the chromatographic column to increase, use a material to produce uneven residence time, finally cause separating effect relatively poor.
In the prior art; The communicated styletable filter of porous of liquid flow distributes to filler; This styletable filter generally is to be made up of for three layers distribution plate, filter screen and filter paper; Its make the flowing phase warp-wise be evenly distributed, to distributing to packing layer under the little state of the phase resistance power that flows, make the stable performance of chromatographic column, life-span long.But for the bigger chromatographic column of diameter; The diameter of the chromatographic column of especially existing preparing chromatograph in industry increases gradually; The distributing uniformity of joining passage through the segmentation behind the central inlet entering filter of the flowing phase on the distribution system can reduce along with the diameter increase of chromatographic column; Finally cause uneven initial fluid distribution, influence separating effect.
Summary of the invention
The invention provides a kind of flowing phase distribution method and distributor thereof that especially can be used in large diameter chromatographic column; It can eliminate the residence time of flowing phase on distribution system has serious differentiation with the increase of column diameter defective effectively; Can realize getting into the even original allocation of the flowing phase of chromatographic column, and the high pressure that can not receive flowing phase is carried influence.The structural design of this distributor is simple, and difficult the obstruction cleaned and use repeatedly easily.
The technical scheme that the present invention adopted is following:
A kind of flowing phase distribution method of chromatographic column is used for the fixedly flowing phase distribution of phase upper surface of preparative chromatography post, it is characterized in that said distribution method comprises:
The rounded dispensers that employing one matches with the cross section of preparative chromatography post; In this distributor upper edge wherein outside the mind-set tree-like dispersing fluid be set divide the dosing road mutually; Each fluid divides the end on dosing road to be provided with dispensing orifice mutually, divides the identical length on dosing road etc. mutually by the fluid of said distributor center to the same specification of each dispensing orifice;
Fluid divides the uniform distribution of dosing road to each dispensing orifice from the center of distributor along each fluid mutually, distributes to the fixing of chromatographic column then uniformly and goes up mutually.
Concretely; Said distribution method further comprises: liquid phase divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center; The end on this first fen dosing road connects second fen dosing road; This second fen dosing road terminal and then connect the 3rd fen dosing road, the subordinate after the 3rd fen dosing road continues to be dispensed to again then divides the dosing road.
The distribution flow quantity on said second minute dosing road is 1/2nd of first fen dosing road, and the distribution flow quantity on said the 3rd minute dosing road is 1/2nd of second fen dosing road.
Said distribution method further comprises: each dispensing orifice is the even distributed and arranged of matrix along said rounded dispensers, is the setting of H type between the one fen dosing road that connects two dispensing orifices and another grade branch dosing road that is connected this grade branch dosing road.
Said distribution method further comprises: adopt a secondary splitter; This secondary splitter is arranged at the bottom of said rounded dispensers; Distributed and arranged has allocation units on this secondary splitter, and each allocation units comprises the branch dosing road of a plurality of connections, and the end on each minute dosing road is provided with miniature dispensing orifice; The dosing road comprised multistage minute dosing road in wherein said minute, and wherein the middle part on the branch dosing road of maximum allocated flow quantity is positioned at the dispensing orifice below of said rounded dispensers.
Miniature dispensing orifice on the said secondary splitter is matrix along the circular end surface of secondary splitter and evenly distributes; Each dispensing orifice is through dividing the dosing road together with a plurality of miniature dispensing orifices, and adjustment divides the chi footpath, liquid road on dosing road, and the distribution flow quantity of each miniature dispensing orifice is equated.
A kind of flowing phase distribution system of chromatographic column is used for the fixedly flowing phase distribution of phase upper surface of preparative chromatography post, it is characterized in that said distribution system comprises:
One rounded dispensers; Its external diameter matches with the cross section of preparative chromatography post; In this distributor upper edge wherein outside the mind-set tree-like dispersing fluid be set divide the dosing road mutually; Each fluid divides the end on dosing road to be provided with dispensing orifice mutually, divides the identical length on dosing road etc. mutually by the fluid of said distributor center to the same specification of each dispensing orifice.
Said liquid phase divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center; The end on this first fen dosing road connects second fen dosing road; This second fen dosing road terminal and then connect the 3rd fen dosing road; Subordinate after the 3rd fen dosing road connects then divides the dosing road, divides the dosing road until afterbody.
Said each dispensing orifice is the even distributed and arranged of matrix along said rounded dispensers, is the setting of H type between one fen dosing road that part connects two dispensing orifices and another grade branch dosing road that is connected this grade branch dosing road.
Said flowing phase distribution system further comprises a secondary splitter; This secondary splitter is a rounded dispensers; Distributed and arranged has allocation units on this secondary splitter, and each allocation units comprises the branch dosing road of a plurality of connections, and the end on each minute dosing road is provided with miniature dispensing orifice; The dosing road comprised multistage minute dosing road in wherein said minute, and wherein the middle part on the branch dosing road of maximum allocated flow quantity is positioned at the dispensing orifice below of said rounded dispensers.
The flowing phase distribution method of this chromatographic column and distributor thereof adopt rounded dispensers; Through dispersing multistage minute dosing road of setting; The grade that has realized each dispensing orifice to distributor center divides the dosing road to be provided with mutually; The flowing phase that makes evenly, constant speed, be dispensed to each dispensing orifice simultaneously stably, and can have dispensing orifice to be directly dispensed in the preparative chromatography post the fixedly upper surface of phase, and make it even, constant speed, flow through the post bed stably.Branch dosing road on this rounded dispensers can be provided with on most branch dosing roads by the one-to-two form; The first order that promptly is communicated with the distributor center divides the chi footpath on dosing road maximum; And the end connection one on one first fen dosing road has the middle part on second fen dosing road of its size 1/2nd; And the middle part with the 3rd fen dosing road in chi footpath, second fen dosing road 1/2nd also connects the size middle part on one second fen dosing road; Like this then the branch dosing road that can realize the same size of most of dispensing orifice, and the length on the branch dosing road of ad eundem is identical can guarantee promptly that so each dispensing orifice simultaneously and the distribution of equivalent circulation phase.Can't satisfy the requirement on the multistage minute dosing road that H type structure is set for the part edge of rounded dispensers, this can receive liquid through arranging in pairs or groups with the different minutes dosing roads that above-mentioned dispensing orifice has corresponding specification and length when realizing with other dispensing orifices.Dispensing orifice is matrix type along the end face of rounded dispensers and evenly distributes, and evenly receives liquid with what form fixing phase.Can be according to the requirement of different preparative chromatography posts, the branch dosing road and the dispensing orifice quantity of design different size.For larger-diameter preparative chromatography post, then can carry out overabsorption hole uniform distribution once more mutually to the fluid that the dispensing orifice through rounded dispensers distributes through the mode that secondary splitter is set.Multicomponent dosing road group is set on this secondary splitter; The corresponding dispensing orifice of each component dosing road group; Each component dosing road group of while also correspondence is provided with a plurality of miniature dispensing orifices, and the length on the branch dosing road of each miniature dispensing orifice to corresponding dispensing orifice is identical with specification.For the miniature dispensing orifice of edge, length and the specifications design that can divide the dosing road accordingly with reference to the dispensing orifice of the edge of distributor are so that each dispensing orifice distributes the flowing phase transmission time of micropore identical with flow to it accordingly.
Through adopting above-mentioned design, can be according to the account form of routine, the specification and the design length that calculate every branch dosing road of science.
Beneficial effect of the present invention is; The flowing phase distribution method of this chromatographic column and distributor thereof especially can be used in large diameter preparative chromatography post; It can eliminate the residence time of flowing phase on distribution system has serious differentiation with the increase of column diameter defective effectively; Can realize getting into the even original allocation of the flowing phase of chromatographic column, and the high pressure that can not receive flowing phase is carried influence.The structural design of this distributor is simple, and difficult the obstruction cleaned and use repeatedly easily.
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is done further explanation.
Description of drawings
Fig. 1 is the structural representation of distributor in the specific embodiment of the invention;
Fig. 2 is the structural representation of secondary splitter in the specific embodiment of the invention.
The specific embodiment
The flowing phase distribution method system of this chromatographic column is used for the fixedly flowing phase distribution of phase upper surface of preparative chromatography post; It adopts the rounded dispensers that matches with the cross section of preparative chromatography post; In this distributor upper edge wherein outside the mind-set tree-like dispersing fluid be set divide the dosing road mutually; Each fluid divides the end on dosing road to be provided with dispensing orifice mutually, divides the identical length on dosing road etc. mutually by the fluid of the same specification of distributor center to each dispensing orifice; Fluid divides the uniform distribution of dosing road to each dispensing orifice from the center of distributor along each fluid mutually, distributes to the fixing of chromatographic column then uniformly and goes up mutually.Liquid phase divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center; The end on this first fen dosing road connects second fen dosing road; This second fen dosing road terminal and then connect the 3rd fen dosing road, the subordinate after the 3rd fen dosing road continues to be dispensed to again then divides the dosing road.Wherein the distribution flow quantity on second fen dosing road is 1/2nd of first fen dosing road; The distribution flow quantity on the 3rd fen dosing road is 1/2nd of second fen dosing road; Each dispensing orifice is the even distributed and arranged of matrix along said rounded dispensers, is the setting of H type between the one fen dosing road that connects two dispensing orifices and another grade branch dosing road that is connected this grade branch dosing road.
So can be in the range of flow of 20-80L/min, with flowing phase evenly, constant speed, be assigned in the preparative chromatography post the fixedly upper surface of phase stably, and make it even, constant speed, flow through the post bed stably.
Flowing phase for the chromatographic column of big format diameter is distributed; Can further adopt secondary splitter, this secondary splitter is arranged at the bottom of said rounded dispensers, and distributed and arranged has allocation units on this secondary splitter; Each allocation units comprises the branch dosing road of a plurality of connections; The end on each minute dosing road is provided with miniature dispensing orifice, wherein divides the dosing road to comprise multistage minute dosing road, and wherein the middle part on the branch dosing road of maximum allocated flow quantity is positioned at the dispensing orifice below of said rounded dispensers.Miniature dispensing orifice on the secondary splitter is matrix along the circular end surface of secondary splitter and evenly distributes; Each dispensing orifice is through dividing the dosing road together with a plurality of miniature dispensing orifices, and adjustment divides the chi footpath, liquid road on dosing road, and the distribution flow quantity of each miniature dispensing orifice is equated.
As shown in Figure 1; This flowing phase distributor is a rounded dispensers; Its external diameter matches with the cross section of preparative chromatography post; In this distributor upper edge wherein outside the mind-set tree-like dispersing fluid be set divide the dosing road mutually, each fluid divides the end on dosing road to be provided with dispensing orifice 30 mutually, divides the identical length on dosing road etc. mutually by the fluid of said distributor center 10 to the same specification of each dispensing orifice.Body divides the dosing road to comprise many first fen dosing road 21 of outwards being dispersed setting by the center mutually; The end on this first fen dosing road connects second fen dosing road 22; This second fen dosing road terminal and then connect the 3rd fen dosing road 23; Subordinate after the 3rd fen dosing road connects then divides the dosing road, divides dosing road 24 until afterbody.It is 1/2nd of this grade branch dosing road that computational short cut during for the realization design, the next stage that each grade branch dosing road connects divide the circulation chi footpath (and flowing phase actual internal area) on dosing road.Each dispensing orifice is the even distributed and arranged of matrix along said rounded dispensers, is the setting of H type between one fen dosing road that part connects two dispensing orifices and another grade branch dosing road that is connected this grade branch dosing road.
It is as shown in Figure 2,, this flowing phase distributor also can comprise a secondary splitter; This secondary splitter is a rounded dispensers; Distributed and arranged has allocation units 40 on this secondary splitter, and each allocation units comprises the branch dosing road 41 of a plurality of connections, and the end on each minute dosing road is provided with miniature dispensing orifice 42; Wherein divide the dosing road to comprise multistage minute dosing road, wherein the middle part on the branch dosing road of maximum allocated flow quantity is positioned at the dispensing orifice below of rounded dispensers.High-pressure flow gets into from the centre bore of distributor, through several sub-distribution, simultaneously and evenly, constant speed, flow out by dispensing orifice stably, again through secondary splitter once more simultaneously and evenly, constant speed, distribute stably.
Among the present invention; No matter distributor or secondary splitter; Realize that it receives liquid level to put the equal correspondent equal of length of run apart from the branch dosing road of dispensing orifice or miniature dispensing orifice; At different levels minutes dosing roads are dividing the timing sectional area to successively decrease each time simultaneously, for upper level divides 1/2nd of dosing road, flow to guarantee flowing phase constant speed in minute dosing road.
Claims (7)
1. the flowing phase distribution method of a chromatographic column is used for the fixedly flowing phase distribution of phase upper surface of preparative chromatography post, it is characterized in that said distribution method comprises:
The rounded dispensers that employing one matches with the cross section of preparative chromatography post; In this distributor upper edge wherein outside the mind-set tree-like dispersing fluid be set divide the dosing road mutually; Each fluid divides the end on dosing road to be provided with dispensing orifice mutually, divides the identical length on dosing road etc. mutually by the fluid of said distributor center to the same specification of each dispensing orifice;
Fluid divides the uniform distribution of dosing road to each dispensing orifice from the center of distributor along each fluid mutually, distributes to the fixing of chromatographic column then uniformly and goes up mutually;
It further comprises: adopt a secondary splitter; This secondary splitter is arranged at the bottom of said rounded dispensers; Distributed and arranged has allocation units on this secondary splitter, and each allocation units comprises the branch dosing road of a plurality of connections, and the end on each minute dosing road is provided with miniature dispensing orifice; The dosing road comprised multistage minute dosing road in wherein said minute, and wherein the middle part on the branch dosing road of maximum allocated flow quantity is positioned at the dispensing orifice below of said rounded dispensers; Miniature dispensing orifice on the said secondary splitter is matrix along the circular end surface of secondary splitter and evenly distributes; Each dispensing orifice is through dividing the dosing road together with a plurality of miniature dispensing orifices, and adjustment divides the chi footpath, liquid road on dosing road, and the distribution flow quantity of each miniature dispensing orifice is equated.
2. the flowing phase distribution method of chromatographic column according to claim 1; It is characterized in that said distribution method further comprises: liquid phase divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center; The end on this first fen dosing road connects second fen dosing road; This second fen dosing road terminal and then connect the 3rd fen dosing road, the subordinate after the 3rd fen dosing road continues to be dispensed to again then divides the dosing road.
3. the flowing phase distribution method of chromatographic column according to claim 2; The distribution flow quantity that it is characterized in that said second minute dosing road is 1/2nd of first fen dosing road, and the distribution flow quantity on said the 3rd minute dosing road is 1/2nd of second fen dosing road.
4. the flowing phase distribution method of chromatographic column according to claim 2; It is characterized in that said distribution method further comprises: each dispensing orifice is the even distributed and arranged of matrix along said rounded dispensers, is the setting of H type between the one fen dosing road that connects two dispensing orifices and another grade branch dosing road that is connected this grade branch dosing road.
5. the flowing phase distributor of a chromatographic column is used for the fixedly flowing phase distribution of phase upper surface of preparative chromatography post, it is characterized in that said distributor comprises:
One rounded dispensers; Its external diameter matches with the cross section of preparative chromatography post; In this distributor upper edge wherein outside the mind-set tree-like dispersing fluid be set divide the dosing road mutually; Each fluid divides the end on dosing road to be provided with dispensing orifice mutually, divides the identical length on dosing road etc. mutually by the fluid of said distributor center to the same specification of each dispensing orifice; Said flowing phase distributor further comprises a secondary splitter; This secondary splitter is a rounded dispensers; Distributed and arranged has allocation units on this secondary splitter, and each allocation units comprises the branch dosing road of a plurality of connections, and the end on each minute dosing road is provided with miniature dispensing orifice; The dosing road comprised multistage minute dosing road in wherein said minute, and wherein the middle part on the branch dosing road of maximum allocated flow quantity is positioned at the dispensing orifice below of said rounded dispensers.
6. the flowing phase distributor of chromatographic column according to claim 5; It is characterized in that said liquid phase divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center; The end on this first fen dosing road connects second fen dosing road; This second fen dosing road terminal and then connect the 3rd fen dosing road, the subordinate after the 3rd fen dosing road connects then divides the dosing road, divides the dosing road until afterbody.
7. the flowing phase distributor of chromatographic column according to claim 6; It is characterized in that said each dispensing orifice is the even distributed and arranged of matrix along said rounded dispensers, be the setting of H type between one fen dosing road that part connects two dispensing orifices and another grade branch dosing road that is connected this grade branch dosing road.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101700132A CN101632878B (en) | 2009-09-01 | 2009-09-01 | Distribution method and distribution device of mobile phases of chromatographic columns |
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| CN2009101700132A CN101632878B (en) | 2009-09-01 | 2009-09-01 | Distribution method and distribution device of mobile phases of chromatographic columns |
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| CN101632878B true CN101632878B (en) | 2012-02-01 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101947392B (en) * | 2010-08-13 | 2012-05-23 | 利穗科技(苏州)有限公司 | Shunt plate for preparing chromatographic column |
| CN102160937A (en) * | 2011-03-23 | 2011-08-24 | 江苏迪沃特仪器设备科技有限公司 | Dynamic axial compression column fluid distribution device |
| CN104399281A (en) * | 2014-12-15 | 2015-03-11 | 聊城万合工业制造有限公司 | Liquid flow controller for radial chromatographic column |
| CN105570493B (en) * | 2016-02-05 | 2018-10-02 | 北京创新通恒科技有限公司 | A kind of multiple valve and chromatographic column |
| CN105664526B (en) * | 2016-02-05 | 2018-02-23 | 北京创新通恒科技有限公司 | A kind of post sieve plate and chromatographic column |
| CN112923774A (en) * | 2021-01-16 | 2021-06-08 | 西安交通大学 | Distributor for shell-and-tube heat exchanger |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4537217A (en) * | 1982-12-09 | 1985-08-27 | Research Triangle Institute | Fluid distributor |
| CN101023346A (en) * | 2004-09-08 | 2007-08-22 | 拜尔技术服务有限责任公司 | Liquid distributor and liquid collector for chromatography columns |
-
2009
- 2009-09-01 CN CN2009101700132A patent/CN101632878B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4537217A (en) * | 1982-12-09 | 1985-08-27 | Research Triangle Institute | Fluid distributor |
| CN101023346A (en) * | 2004-09-08 | 2007-08-22 | 拜尔技术服务有限责任公司 | Liquid distributor and liquid collector for chromatography columns |
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| CN101632878A (en) | 2010-01-27 |
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