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Zirconium-containing metal organic framework material modified open tubular capillary column and application thereof

A metal-organic framework and open-tube capillary column technology is applied in the field of chromatographic columns to achieve the effects of simple process, easy operation and good separation effect

Active Publication Date: 2017-09-19
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no reports on the use of zirconium-containing metal-organic framework materials as stationary phases for capillary electrochromatography at home and abroad.

Method used

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  • Zirconium-containing metal organic framework material modified open tubular capillary column and application thereof
  • Zirconium-containing metal organic framework material modified open tubular capillary column and application thereof
  • Zirconium-containing metal organic framework material modified open tubular capillary column and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 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. Take 2.125 g of iminodiacetic acid (IDA), add 25 mL of water, and adjust the pH to 11 with 10 mol / L sodium hydroxide. Under ice-bath conditions, stir and add 0.7 mL of 3-glycidyloxypropyltrimethoxysilane (GLYMO). The mixture was stirred at 65 °C for 6 h, then the ice bath was lowered to 0 °C, and 0.8 mL of GLYMO was added. Continue to stir at 65 °C for 6 h, then lower the ice bath to 0 °C, add 0.85 mL GLYMO, stir overnight at 65 °C, and finally adjust the pH to 6 with concentrated hydrochloric acid. The obtained solution was passed into the pretreated capillary column, and reacted in a water bath at 95 °C for 12 h, then washed with methanol and water respectively, and dried with nitrog...

Embodiment 2

[0026] 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. Take 2.125 g of iminodiacetic acid (IDA), add 25 mL of water, and adjust the pH to 11 with 10 mol / L sodium hydroxide. Under ice-bath conditions, stir and add 0.7 mL of 3-glycidyloxypropyltrimethoxysilane (GLYMO). The mixture was stirred at 65 °C for 6 h, then the ice bath was lowered to 0 °C, and 0.8 mL of GLYMO was added. Continue to stir at 65 °C for 6 h, then lower the ice bath to 0 °C, add 0.85 mL GLYMO, stir overnight at 65 °C, and finally adjust the pH to 6 with concentrated hydrochloric acid. The obtained solution was passed through the pretreated capillary column, reacted in a water bath at 90 °C for 16 h, then washed with methanol and water, and dried with nitrogen to obtain a...

Embodiment 3

[0028] 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 2O was rinsed for 30 min, blown dry with nitrogen, and finally dried in an oven at 100 °C for 1 h. Take 2.125 g of iminodiacetic acid (IDA), add 25 mL of water, and adjust the pH to 11 with 10 mol / L sodium hydroxide. Under ice-bath conditions, stir and add 0.7 mL of 3-glycidyloxypropyltrimethoxysilane (GLYMO). The mixture was stirred at 65 °C for 6 h, then the ice bath was lowered to 0 °C, and 0.8 mL of GLYMO was added. Continue to stir at 65 °C for 6 h, then lower the ice bath to 0 °C, add 0.85 mL GLYMO, stir overnight at 65 °C, and finally adjust the pH to 6 with concentrated hydrochloric acid. The obtained solution was passed into the pretreated capillary column, reacted in a water bath at 100 °C for 16 h, then washed with methanol and water, and dried with nitrogen to obtain a ca...

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Abstract

The invention discloses an open tubular capillary column of a zirconium-containing metal organic framework material NH2-UiO-66 and application of the open tubular capillary column. A preparation method of the open tubular capillary column includes the following steps: feeding a GLYMO-IDA-silane solution in a pretreated capillary column, and modifying a carboxyl on the surface of a capillary tube; and then successively feeding zirconium chloride, a 2-aminoterephthalic acid solution and a mixture of the zirconium chloride and the 2-aminoterephthalic acid solution in the capillary column successively, and enabling the zirconium-containing metal organic framework material NH2-UiO-66 to grow on the surface of the capillary column in situ. The preparation method is simple in process, easy to operate and low in cost, and is pollution-free to the environment. The prepared NH2-UiO-66 modified capillary column has good separating effect on phenoxyacetic acids water quality pollutants and nucleosides analytes.

Description

technical field [0001] The invention belongs to the technical field of chromatographic columns, and relates to a zirconium-containing metal organic framework material NH 2 - Preparation and application of open-tube capillary column of UiO-66. Background technique [0002] As a high-efficiency separation technology, 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 high separation efficiency, fast analysis speed, and less consumption of samples and organic solvents. Etc. Compared with monolithic columns and packed columns, capillary open-tube columns have the advantages of easy preparation, no need for plungers, and less air bubbles, etc., which have obvious advantages in capillary electrochromatographic separation and analysis. However, open-tube capillary columns still have some disadvantages, such as low column capacit...

Claims

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Application Information

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IPC IPC(8): B01D15/20B01D15/38C07C51/47C07C59/68C07C59/70C07H1/06C07H19/167C07H19/067
CPCB01D15/206B01D15/3885C07C51/47C07H1/06C07H19/067C07H19/167C07C59/68C07C59/70
Inventor 陈子林唐平秀
Owner WUHAN UNIV
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