CN103091432A - Method for coating stationary phase in capillary column - Google Patents
Method for coating stationary phase in capillary column Download PDFInfo
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- CN103091432A CN103091432A CN2011103356762A CN201110335676A CN103091432A CN 103091432 A CN103091432 A CN 103091432A CN 2011103356762 A CN2011103356762 A CN 2011103356762A CN 201110335676 A CN201110335676 A CN 201110335676A CN 103091432 A CN103091432 A CN 103091432A
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- capillary column
- coating liquid
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- closed container
- stationary phase
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Abstract
The invention discloses a method for coating a stationary phase in a capillary column. The method comprises the following steps: 1, filling a coating liquid into a closed container, wherein the closed container only has a top outlet, and the top outlet is communicated with the first port of two ports of the capillary column; 2, heating the coating liquid in the closed container to make volatile matters in the coating liquid enter the first port of the capillary column and be discharged from the second port of the capillary column; 3, inserting the first port of the capillary column into the coating liquid after the coating liquid is boiling until the coating liquid enters and fills up the capillary column; and 4, closing the second port of the capillary column, pulling the first port of the capillary column out of the closed container, and carrying out vacuum drying of the coating liquid in the capillary column until residues form a stationary phase at the inner wall of the capillary column. The coating method allows the degassing and perfusion of the coating liquid to be once completed, so the coating success rate of the stationary phase of the capillary column is improved to above 95%, and the thickness homogeneity of the formed stationary phase is good.
Description
Technical field
The present invention relates to a kind of perfusion in the capillary column, apply the fixedly method of phase.
Background technology
Capillary chromatographic column is applied in the analyzing and testing field widely, capillary chromatographic column mainly is comprised of capillary column and the related accessory of glass or metal material, wherein the inwall of capillary column is coated with fixedly phase, and its performance has critical impact to detecting effect.
Add man-hour and be generally fixing phased soln or be dispersed in and be configured to coating liquid in organic solvent, then coating liquid is fed in capillary column, then make fixedly through vacuum drying that the phase material is covering at the capillary column inwall.
In prior art, coating liquid is dissolved with a small amount of air, if do not processed the film that is difficult to form the thickness homogeneous after fixing drying mutually, makes to apply success ratio only in 10% left and right.
Summary of the invention
The invention provides a kind of air that can remove in coating liquid, and can disposablely complete the painting method of coating liquid perfusion.
A kind of painting method of stationary phase in capillary column comprises the steps:
(1) coating liquid is packed into closed container, this closed container only has top exit, and this top exit only is communicated with the first port in two ports of capillary column.
(2) coating liquid in the heating closed container, and the first port of capillary column is remained on the liquid level of coating liquid, make the volatile matter in coating liquid enter the first port of capillary column, and discharge from the second port of capillary column.
The existing solvent of volatile matter in coating liquid also has the air that dissolves in coating liquid, and coating liquid heats up the air dissolves degree is reduced, volatilization then.
(3) after coating liquid boiling, the first port of capillary column is inserted under the liquid level of coating liquid, make coating liquid enter the first port of capillary column until be full of capillary column inside.
As preferably, kept 1～10 minute after the coating liquid boiling, and then the first port of capillary column is inserted under the liquid level of coating liquid, the air that dissolves in coating liquid is discharged as much as possible fully.
(4) the second port of sealing capillary column, extract closed container with the first port of capillary column, and the coating liquid in the vacuum drying capillary column is until residue forms fixedly phase at the capillary column inwall.Temperature during as preferred described vacuum drying is 35～40 degrees centigrade.
Painting method of the present invention can disposablely complete the degassed of coating liquid and the perfusion, with capillary column fixedly the coating success ratio of phase be increased to more than 95%, the fixedly phase thickness homogeneity of formation is good.
Description of drawings
Fig. 1 is the structural representation of the coating unit of painting method employing of the present invention;
Fig. 2 is that the coating unit in Fig. 1 is completed the structural representation when pouring into after degassed.
Embodiment
Referring to accompanying drawing, in order to realize that coating unit that painting method of the present invention adopts comprises the closed container 1 for splendid attire coating liquid 2, this closed container 1 top is provided with interface, this interface place is filled with resilient seal plug 4, resilient seal plug 4 is provided with for the through hole that inserts capillary column 5, interference fit between the outer wall of the inwall of through hole and capillary column to be processed 5.
Closed container 1 top can also be provided with gland bonnet 3, and during use, gland bonnet 3 is closed, the coating liquid 2 of being convenient to annotate when gland bonnet 3 is opened.Guarantee good impermeability after capillary column 5 inserts, resilient seal plug 4 can adopt can aitiogenic material with coating liquid, as tetrafluoroethene etc.
When utilizing said apparatus to carry out the coating of stationary phase in capillary column, comprise the steps:
(1) coating liquid is packed into closed container, this closed container only has top exit, and this top exit only is communicated with the first port in two ports of capillary column.
(2) coating liquid in the heating closed container, and the first port of capillary column is remained on the liquid level of coating liquid, make the volatile matter in coating liquid can enter along the arrow A direction the first port of capillary column, and discharge from the second port of capillary column.
(3) kept 2 minutes after the coating liquid boiling, the basic emptying of air of dissolving in coating liquid, the first port with capillary column inserts under the liquid level of coating liquid again, the coating liquid solvent of gasification raises the closed container internal pressure, the arrow B direction is exerted pressure to the liquid level of coating liquid, then coating liquid is pressed in capillary column along the arrow C direction, makes coating liquid be full of capillary column inside.
(4) the second port of sealing capillary column, extract closed container with the first port of capillary column, and the coating liquid in 40 degrees centigrade of lower vacuum drying capillary columns is until residue forms fixedly phase at the capillary column inwall.
Painting method of the present invention can disposablely complete the degassed of coating liquid and the perfusion, with capillary column fixedly the coating success ratio of phase be increased to more than 95%, the fixedly phase thickness homogeneity of formation is good.
Claims (3)
1. the painting method of a stationary phase in capillary column, is characterized in that, comprises the steps:
(1) coating liquid is packed into closed container, this closed container only has top exit, and this top exit only is communicated with the first port in two ports of capillary column;
(2) coating liquid in the heating closed container, and the first port of capillary column is remained on the liquid level of coating liquid, make the volatile matter in coating liquid enter the first port of capillary column, and discharge from the second port of capillary column;
(3) after coating liquid boiling, the first port of capillary column is inserted under the liquid level of coating liquid, make coating liquid enter the first port of capillary column until be full of capillary column inside;
(4) the second port of sealing capillary column, extract closed container with the first port of capillary column, and the coating liquid in the vacuum drying capillary column is until residue forms fixedly phase at the capillary column inwall.
2. the painting method of stationary phase in capillary column as claimed in claim 1, is characterized in that, kept 1～10 minute after the coating liquid boiling in step (3), and then the first port of capillary column is inserted under the liquid level of coating liquid.
3. the painting method of stationary phase in capillary column as claimed in claim 2, is characterized in that, the temperature during vacuum drying described in step (4) is 35～40 degrees centigrade.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103356762A CN103091432A (en) | 2011-10-31 | 2011-10-31 | Method for coating stationary phase in capillary column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103356762A CN103091432A (en) | 2011-10-31 | 2011-10-31 | Method for coating stationary phase in capillary column |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103091432A true CN103091432A (en) | 2013-05-08 |
Family
ID=48204259
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103356762A Pending CN103091432A (en) | 2011-10-31 | 2011-10-31 | Method for coating stationary phase in capillary column |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103091432A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS633260A (en) * | 1986-06-24 | 1988-01-08 | Kurita Water Ind Ltd | chromatography equipment |
| JPH04323557A (en) * | 1991-04-23 | 1992-11-12 | Hitachi Plant Eng & Constr Co Ltd | Device for filling column for chromatography |
| CN1586699A (en) * | 2004-07-16 | 2005-03-02 | 大连大学 | Gel column mounting method |
| CN101105482A (en) * | 2007-07-27 | 2008-01-16 | 福州大学 | Novel device made of monolithic column of capillary electrochromatography and its application method |
-
2011
- 2011-10-31 CN CN2011103356762A patent/CN103091432A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS633260A (en) * | 1986-06-24 | 1988-01-08 | Kurita Water Ind Ltd | chromatography equipment |
| JPH04323557A (en) * | 1991-04-23 | 1992-11-12 | Hitachi Plant Eng & Constr Co Ltd | Device for filling column for chromatography |
| CN1586699A (en) * | 2004-07-16 | 2005-03-02 | 大连大学 | Gel column mounting method |
| CN101105482A (en) * | 2007-07-27 | 2008-01-16 | 福州大学 | Novel device made of monolithic column of capillary electrochromatography and its application method |
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Application publication date: 20130508 |