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Woven aromatic ring polymer-based open tubular capillary column and application thereof

An open-tube capillary column and capillary column technology, which is applied in the field of chromatographic columns, can solve problems such as low column capacity, and achieve the effects of low cost, good separation effect and easy operation.

Active Publication Date: 2017-09-15
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the open-tube capillary column has the advantages of easy preparation, no need for a plunger, and is not easy to generate air bubbles. It has certain advantages in capillary electrochromatography, but there are still some shortcomings in the open-tube capillary column, such as relatively small and low column capacity.

Method used

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  • Woven aromatic ring polymer-based open tubular capillary column and application thereof
  • Woven aromatic ring polymer-based open tubular capillary column and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A 33.5 cm long quartz capillary (50 µm i.d. × 375 µm o.d.) was first washed with 1 M NaOH solution for 2 h, and then sequentially washed with H 2 O, 1 M HCl solution rinsed for 10 min, H 2 O was rinsed for 30 min, blown dry with nitrogen, and finally dried in an oven at 100 °C for 1 h. The isopropanol solution (50%, v / v) of trimethyloxyphenylsilane was continuously passed into the quartz capillary with a syringe for 10 min, then both ends of the capillary were sealed with a Teflon tube, and placed in a 70 °C water bath for reaction 10 h, repeat this operation step again. Then the capillary column was rinsed with methanol for 30 min, and dried with nitrogen to obtain a capillary column with a phenyl-terminal modified inner wall. The obtained capillary column was flushed with 1,2-dichloroethane solution for 10 min, and dried with nitrogen. Prepare a solution of 50 mg / mL anhydrous ferric chloride in 1,2-dichloroethane, dissolve it by ultrasonication for 10 min, centrifu...

Embodiment 2

[0027] A 33.5 cm long quartz capillary (50 µm i.d. × 375 µm o.d.) was first washed with 1 M NaOH solution for 2 h, and then sequentially washed with H 2 O, 1 M HCl solution rinsed for 10 min, H 2 O was rinsed for 30 min, blown dry with nitrogen, and finally dried in an oven at 100 °C for 1 h. The isopropanol solution of trimethyloxyphenylsilane (50%, v / v) was continuously passed into the quartz capillary with a syringe for 10 min, then both ends of the capillary were sealed with a Teflon tube, and placed in a water bath at 80°C for reaction 10 h, repeat this operation step again. Then the capillary column was rinsed with methanol for 30 min, and dried with nitrogen to obtain a capillary column with a phenyl-terminal modified inner wall. The obtained capillary column was flushed with 1,2-dichloroethane solution for 30 min, and dried with nitrogen. Prepare a solution of 50 mg / mL anhydrous ferric chloride in 1,2-dichloroethane, dissolve it by ultrasonication for 10 min, centri...

Embodiment 3

[0029] A 33.5 cm long quartz capillary (50 µm i.d. × 375 µm o.d.) was first washed with 1 M NaOH solution for 2 h, and then sequentially washed with H 2 O, 1 M HCl solution rinsed for 10 min, H 2 O was rinsed for 30 min, blown dry with nitrogen, and finally dried in an oven at 100 °C for 1 h. The isopropanol solution of trimethyloxyphenylsilane (50%, v / v) was continuously passed into the quartz capillary with a syringe for 10 min, then both ends of the capillary were sealed with a Teflon tube, and placed in a water bath at 80°C for reaction 12 h, repeat this operation step again. Then the capillary column was rinsed with methanol for 30 min, and dried with nitrogen to obtain a capillary column with a phenyl-terminal modified inner wall. The obtained capillary column was flushed with 1,2-dichloroethane solution for 30 min, and dried with nitrogen. Prepare a solution of 100 mg / mL anhydrous ferric chloride in 1,2-dichloroethane, dissolve it by ultrasonication for 10 min, centr...

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Abstract

The invention relates to a woven aromatic ring polymer-based open tubular capillary column and application thereof. A preparation method of the open tubular capillary column comprises the following steps: replenishing a pretreated capillary column with a trimethyl oxyl phenyl silane solution so as to enable the surface of the capillary column to be modified by a phenyl terminus; then, replenishing the phenyl terminus-containing capillary column with a mixed solution of a catalyst-anhydrous ferric trichloride and an external cross-linking agent-dimethoxymethane; finally, carrying out an in-situ reaction to form the woven aromatic ring polymer-modified open tubular capillary column. The preparation method has the advantages of simple technology, easy operation, low cost and no pollution to environment. The prepared woven aromatic ring polymer-modified capillary column has a better separating effect on chlorinated benzene series materials.

Description

technical field [0001] The invention belongs to the technical field of chromatographic columns, and relates to an open-tube capillary column based on a braided aromatic ring polymer and an application thereof. Background technique [0002] As a separation technique, capillary electrochromatography has attracted widespread attention because it combines the high separation efficiency of capillary electrophoresis and the high selectivity of liquid chromatography. It has the advantages of fast analysis speed, high separation efficiency, and less consumption of samples and organic solvents. According to different preparation methods, it can be divided into open-tubular column, monolithic column and packed column. Among them, the open-tube capillary column has the advantages of easy preparation, no need for a plunger, and is not easy to generate air bubbles. It has certain advantages in capillary electrochromatography, but there are still some shortcomings in the open-tube capilla...

Claims

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Application Information

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IPC IPC(8): B01D15/20B01D15/38C08G77/04
CPCB01D15/20B01D15/3885C08G77/04C08G77/80
Inventor 陈子林唐平秀
Owner WUHAN UNIV