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Mesoporous material coating based open-tubular capillary chromatographic column and preparation method thereof

A mesoporous material and capillary technology, applied in the field of chromatographic columns, can solve the problems of limited development, small column capacity, cumbersome preparation process, etc., and achieve the effect of increasing phase and column capacity, simple preparation process, and increasing surface area

Inactive Publication Date: 2011-08-31
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the most widely used method is packed column electrochromatography, but it needs to prepare the plug first and then fill the stationary phase into the capillary, so the column preparation process is cumbersome, and the Joule heating effect, plug effect and air bubble effect in the operation process further limit its use. develop
Among them, the preparation method of the open-tubular column is simple, only need to coat a layer of stationary phase on the inner wall of the capillary, and can eliminate the various effects mentioned above at the same time; but due to its small size, the column capacity is small

Method used

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  • Mesoporous material coating based open-tubular capillary chromatographic column and preparation method thereof
  • Mesoporous material coating based open-tubular capillary chromatographic column and preparation method thereof
  • Mesoporous material coating based open-tubular capillary chromatographic column and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 Preparation and Characterization of Open-Tube Chromatographic Column

[0020] 1 mol / L sodium hydroxide, distilled water, 1 mol / L hydrochloric acid, and distilled water rinse the quartz capillary with an inner diameter of 50 μm (54 cm long) for 1 h each, 120 o The capillary was dried under nitrogen atmosphere for 1 h.

[0021] Dissolve 0.16 g of surfactant P123 in 2 mL of ethanol, then add 360 microliters of TEOS, 72 microliters of C8-TEOS, and finally add 250 microliters of water and 35 microliters of 1mol / L hydrochloric acid, 60 o C was heated and stirred for 1 h to obtain a sol.

[0022] The sol was poured into the treated quartz capillary by pressure, and left at room temperature for 10 min, 120 o Nitrogen under C drives away the unreacted sol, 120 o C continued to pass nitrogen gas for 1 h to complete the reaction. Surfactant was removed by ethanol-concentrated hydrochloric acid solution (20%, V / V) for 12 h. The concentrated hydrochloric acid solutio...

Embodiment 2

[0024] Example 2 Preparation and Characterization of Open-Tube Chromatographic Column

[0025] 1 mol / L sodium hydroxide, distilled water, 1 mol / L hydrochloric acid, and distilled water rinse the quartz capillary with an inner diameter of 25 μm (54 cm long) for 1 h each, 120 o The capillary was dried under nitrogen atmosphere for 1 h.

[0026] Dissolve 0.16 g of surfactant F127 in 2 mL of ethanol, then add 360 microliters of TEOS, 72 microliters of C8-TEOS, and finally add 250 microliters of water and 35 microliters of 1mol / L hydrochloric acid, 60 o C was heated and stirred for 1 h to obtain a sol.

[0027] The sol was poured into the treated quartz capillary by pressure, and left at room temperature for 10 min, 120 o Nitrogen under C drives away the unreacted sol, 120 o C continued to pass nitrogen gas for 1 h to complete the reaction. Surfactant was removed by ethanol-concentrated hydrochloric acid solution (20%, V / V) for 12 h.

[0028] The resulting open-tubular column...

Embodiment 3

[0029] Example 3 Preparation and Characterization of Open-Tube Chromatographic Column

[0030] 1 mol / L sodium hydroxide, distilled water, 1 mol / L hydrochloric acid, and distilled water rinse the quartz capillary with an inner diameter of 50 μm (54 cm long) for 1 h each, 120 o The capillary was dried under nitrogen atmosphere for 1 h.

[0031] Dissolve 0.16 g of surfactant P123 in 2 mL of ethanol, then add 360 microliters of TEOS, 72 microliters of 3-aminopropyltriethoxysilane, and finally add 250 microliters of water and 35 microliters 1mol / L hydrochloric acid, 60 o C was heated and stirred for 1 h to obtain a sol.

[0032] The sol was poured into the treated quartz capillary by pressure, and left at room temperature for 10 min, 120 o Nitrogen under C drives away the unreacted sol, 120 o C continued to pass nitrogen gas for 1 h to complete the reaction. Surfactant was removed by ethanol-concentrated hydrochloric acid solution (20%, V / V) for 12 h.

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Abstract

The invention belongs to the technical field of chromatographic columns, particularly relates to a mesoporous material coating based open-tubular capillary chromatographic column as well as a preparation method and an application thereof. The preparation method provided by the invention comprises the following steps: dissolving a surfactant into a certain amount of ethanol; then, adding a certainamount of silicon sources and functionalized silicon sources into the ethanol; and finally, adding a little bit of water and hydrochloric acid into the ethanol, then heating and stirring the obtainedmixture for a considerable period at an appropriate temperature so as to obtain a sol. Through changing the type and application amount of the surfactant, the mesoporous material structure is changedfrom a one-dimensional structure to a three-dimensional structure, and the hole diameter (2nm-10nm) is adjustable. After the sol is coated on the inner wall of an open tubular column (quartz capillary with an inner diameter of 10-50 microns), an acid solution of alcohols is fed into the open tubular column so as to remove the surfactant. The obtained open tubular column is used for CEC (capillaryelectro-chromatography) and CLC (capillary liquid chromatography) separable aromatics and chiral compounds, and the like.

Description

technical field [0001] The invention belongs to the technical field of chromatographic columns, and in particular relates to a capillary open-tube chromatographic column and a preparation method thereof. Background technique [0002] Chromatographic technology has been widely used in various fields of scientific research and social production sectors. As a chromatographic technique, capillary electrochromatography (CEC) has become a new microcolumn separation method because it combines the advantages of capillary electrophoresis and high performance liquid chromatography. According to the different forms of stationary phase in the capillary, capillary electrochromatography can be divided into three categories: open column electrochromatography, packed column electrochromatography, and continuous bed electrochromatography. At present, the most widely used method is packed column electrochromatography, but it needs to prepare the plug first and then fill the stationary phase ...

Claims

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Application Information

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IPC IPC(8): B01D15/22C07C335/02C07C15/24C07C15/14C07C13/567C07C15/28C07C7/12
Inventor 张祥民雷杰
Owner FUDAN UNIV
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