CN101632878A - 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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- CN101632878A CN101632878A CN200910170013A CN200910170013A CN101632878A CN 101632878 A CN101632878 A CN 101632878A CN 200910170013 A CN200910170013 A CN 200910170013A CN 200910170013 A CN200910170013 A CN 200910170013A CN 101632878 A CN101632878 A CN 101632878A
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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 the phase that flows in the chromatographic column that preparing chromatograph in industry uses, be specifically related to a kind of mobile 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 to obtain pure material from mixture.The efficient of separating with raising for the time of accelerating to separate, 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 mobile phases of use.After pending liquid is injected into chromatographic column, move in fixing mutually by pressure, because different material is different with the interaction of fixing phase in the pending liquid, different materials leaves chromatographic column in proper order, obtain different peak-to-peak signals by detector, at last the material of judging that by these signals of analysing and comparing trickle contains.
The employed chromatographic column of preparing chromatograph in industry mostly is vertical tubular body, is provided with the packed bed that porous particle is formed in this tubular body.Carrying out to packed bed that uniform fluid distributes is 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 of for three layers distribution plate, filter screen and filter paper, its make the phase warp-wise that flows 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 that a central inlet by the mobile phase on the distribution system enters the fine distribution passage behind the filter can increase along with the diameter of chromatographic column and reduce, finally cause uneven initial fluid distribution, influence separating effect.
Summary of the invention
The invention provides a kind of mobile phase distribution method and distributor thereof that especially can be used in large diameter chromatographic column, it can eliminate the residence time that flows on distribution system has serious differentiation with the increase of column diameter defective effectively, can realize entering the even original allocation of the mobile phase of chromatographic column, and the high pressure of the phase that can not be subjected to flowing is carried influence.The structural design of this distributor is simple, and difficult the obstruction cleaned and use repeatedly easily.
The technical solution adopted in the present invention is as follows:
A kind of mobile phase distribution method of chromatographic column is used for the fixedly distribution mutually of flowing of phase upper surface of preparative chromatography post, it is characterized in that described distribution method comprises:
Adopt a 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 described distributor center to the fluid of 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, described distribution method further comprises: liquid divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center mutually, 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 described second minute dosing road is 1/2nd of first fen dosing road, and the distribution flow quantity on described the 3rd minute dosing road is 1/2nd of second fen dosing road.
Described distribution method further comprises: each dispensing orifice is the matrix setting that evenly distributes along described rounded dispensers, is the setting of H type between the one fen dosing road that connects two dispensing orifices and another fraction dosing road that is connected this fraction dosing road.
Described distribution method further comprises: adopt a secondary splitter, this secondary splitter is arranged at the bottom of described rounded dispensers, distribute on this secondary splitter and be provided with allocation units, 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, 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 described rounded dispensers.
Miniature dispensing orifice on the described secondary splitter is matrix along the circular end surface of secondary splitter and evenly distributes; Each dispensing orifice equates the distribution flow quantity of each miniature dispensing orifice by dividing the dosing road together with a plurality of miniature dispensing orifices, adjust chi footpath, the liquid road of dividing the dosing road.
A kind of mobile phase distribution system of chromatographic column is used for the fixedly distribution mutually of flowing of phase upper surface of preparative chromatography post, it is characterized in that described 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 described distributor center to the fluid of the same specification of each dispensing orifice.
Described liquid divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center mutually, 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.
Described each dispensing orifice is the matrix setting that evenly distributes along described rounded dispensers, is the setting of H type between one fen dosing road that part connects two dispensing orifices and another fraction dosing road that is connected this fraction dosing road.
Described mobile phase distribution system further comprises a secondary splitter, this secondary splitter is a rounded dispensers, distribute on this secondary splitter and be provided with allocation units, 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, 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 described rounded dispensers.
The mobile phase distribution method of this chromatographic column and distributor thereof adopt rounded dispensers, by dispersing multistage minute dosing road of setting, realized that each dispensing orifice to the grade at distributor center divides the dosing road to be provided with mutually, what make flows mutually evenly, constant speed, is 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 evenly, 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, so promptly can guarantee the distribution circulation phase of each dispensing orifice while and equivalent.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 be subjected to liquid by 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 is subjected to 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 by rounded dispensers distributes by 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 each miniature dispensing orifice is identical with specification to the length on the branch dosing road of corresponding dispensing orifice.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 mobile phase transmission time of micropore identical with flow to it accordingly.
By 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 mobile phase distribution method and the distributor thereof of this chromatographic column especially can be used in large diameter preparative chromatography post, it can eliminate the residence time that flows on distribution system has serious differentiation with the increase of column diameter defective effectively, can realize entering the even original allocation of the mobile phase of chromatographic column, and the high pressure of the phase that can not be subjected to flowing is carried influence.The structural design of this distributor is simple, and difficult the obstruction cleaned and use repeatedly easily.
The present invention is described further below in conjunction with the drawings and specific embodiments.
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 mobile phase distribution method of this chromatographic column is to be used for the fixedly distribution mutually of flowing of phase upper surface of preparative chromatography post, it adopts a 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 distributor center to the fluid of 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.Liquid divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center mutually, 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 matrix setting that evenly distributes along described rounded dispensers, is the setting of H type between the one fen dosing road that connects two dispensing orifices and another fraction dosing road that is connected this fraction dosing road.
So can be in the range of flow of 20-80L/min, will flow mutually evenly, constant speed, be assigned in the preparative chromatography post the fixedly upper surface of phase stably, and make it evenly, constant speed, flow through the post bed stably.
Distribute mutually flowing of chromatographic column for big format diameter, can further adopt secondary splitter, this secondary splitter is arranged at the bottom of described rounded dispensers, distribute on this secondary splitter and be provided with allocation units, 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 described 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 equates the distribution flow quantity of each miniature dispensing orifice by dividing the dosing road together with a plurality of miniature dispensing orifices, adjust chi footpath, the liquid road of dividing the dosing road.
As shown in Figure 1, the phase distributor that should flow 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 described distributor center 10 to the fluid of 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.Computational short cut during for the realization design, the next stage that each fraction dosing road connects divide the circulation chi footpath (and mobile phase actual internal area) on dosing road to be 1/2nd of this fraction dosing road.Each dispensing orifice is the matrix setting that evenly distributes along described rounded dispensers, is the setting of H type between one fen dosing road that part connects two dispensing orifices and another fraction dosing road that is connected this fraction dosing road.
As shown in Figure 2, the phase distributor that should flow also can comprise a secondary splitter, this secondary splitter is a rounded dispensers, distributing on this secondary splitter is provided with allocation units 40, 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 enters 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 is subjected to 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, constant speed flows in minute dosing road to guarantee to flow.
Claims (10)
1. the mobile phase distribution method of a chromatographic column is used for the fixedly distribution mutually of flowing of phase upper surface of preparative chromatography post, it is characterized in that described distribution method comprises:
Adopt a 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 described distributor center to the fluid of 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.
2. the mobile phase distribution method of chromatographic column according to claim 1, it is characterized in that described distribution method further comprises: liquid divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center mutually, 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 mobile phase distribution method of chromatographic column according to claim 2, the distribution flow quantity that it is characterized in that described second minute dosing road is 1/2nd of first fen dosing road, and the distribution flow quantity on described the 3rd minute dosing road is 1/2nd of second fen dosing road.
4. the mobile phase distribution method of chromatographic column according to claim 2, it is characterized in that described distribution method further comprises: each dispensing orifice is the matrix setting that evenly distributes along described rounded dispensers, is the setting of H type between the one fen dosing road that connects two dispensing orifices and another fraction dosing road that is connected this fraction dosing road.
5. the mobile phase distribution method of chromatographic column according to claim 1, it is characterized in that described distribution method further comprises: adopt a secondary splitter, this secondary splitter is arranged at the bottom of described rounded dispensers, distribute on this secondary splitter and be provided with allocation units, 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, 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 described rounded dispensers.
6. the mobile phase distribution method of chromatographic column according to claim 5 is characterized in that miniature dispensing orifice on the described secondary splitter is matrix along the circular end surface of secondary splitter and evenly distributes; Each dispensing orifice equates the distribution flow quantity of each miniature dispensing orifice by dividing the dosing road together with a plurality of miniature dispensing orifices, adjust chi footpath, the liquid road of dividing the dosing road.
7. the mobile phase distributor of a chromatographic column is used for the fixedly distribution mutually of flowing of phase upper surface of preparative chromatography post, it is characterized in that described 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 described distributor center to the fluid of the same specification of each dispensing orifice.
8. the mobile phase distributor of chromatographic column according to claim 7, it is characterized in that described liquid divides the dosing road to comprise many first fen dosing road of outwards being dispersed setting by the center mutually, 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.
9. the mobile phase distributor of chromatographic column according to claim 8, it is characterized in that described each dispensing orifice is the matrix setting that evenly distributes along described rounded dispensers, be the setting of H type between one fen dosing road that part connects two dispensing orifices and another fraction dosing road that is connected this fraction dosing road.
10. the mobile phase distributor of chromatographic column according to claim 7, it is characterized in that described mobile phase distributor further comprises a secondary splitter, this secondary splitter is a rounded dispensers, distribute on this secondary splitter and be provided with allocation units, 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, 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 described rounded dispensers.
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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 CN101632878B (en) | 2012-02-01 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101947392A (en) * | 2010-08-13 | 2011-01-19 | 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 |
| CN105570493A (en) * | 2016-02-05 | 2016-05-11 | 北京创新通恒科技有限公司 | Multi-channel valve and chromatographic column |
| CN105664526A (en) * | 2016-02-05 | 2016-06-15 | 北京创新通恒科技有限公司 | Column 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4537217A (en) * | 1982-12-09 | 1985-08-27 | Research Triangle Institute | Fluid distributor |
| DE102004043362A1 (en) * | 2004-09-08 | 2006-03-09 | Bayer Technology Services Gmbh | Liquid distributor and liquid collector for chromatography columns |
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2009
- 2009-09-01 CN CN2009101700132A patent/CN101632878B/en active Active
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101947392A (en) * | 2010-08-13 | 2011-01-19 | 利穗科技(苏州)有限公司 | Shunt plate for preparing chromatographic column |
| 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 |
| CN105570493A (en) * | 2016-02-05 | 2016-05-11 | 北京创新通恒科技有限公司 | Multi-channel valve and chromatographic column |
| CN105664526A (en) * | 2016-02-05 | 2016-06-15 | 北京创新通恒科技有限公司 | Column sieve plate 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 |
| 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 |
| CN112923774A (en) * | 2021-01-16 | 2021-06-08 | 西安交通大学 | Distributor for shell-and-tube heat exchanger |
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