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Monolithic silica gel adsorption column, and solid phase extraction device and application thereof

A technology of extraction device and solid phase extraction column, which is applied in solid solvent extraction, measuring devices, and other chemical processes, can solve problems that have not been reported before, and achieve the effects of ensuring adsorption efficiency, low environmental requirements, and using a small amount of solvent

Inactive Publication Date: 2010-01-20
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, there is no report about a kind of silica gel monolithic adsorption column and its solid phase extraction device and application

Method used

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  • Monolithic silica gel adsorption column, and solid phase extraction device and application thereof
  • Monolithic silica gel adsorption column, and solid phase extraction device and application thereof
  • Monolithic silica gel adsorption column, and solid phase extraction device and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Silica monolithic adsorption column preparation

[0032] Weigh 1.2830g of polyethylene glycol (MW: 10000), dissolve it in 20ml of 0.01M acetic acid solution, add 10ml of tetramethylsiloxane under ice bath, and stir for 40min at the same temperature. After the tetramethylsiloxane solified mixture was ultrasonically degassed, it was poured into a straight tube mold (the straight tube mold is a glass tube with a diameter of 30 mm and a length of 15 cm). At 40°C, stand for 2 hours to gel. Aged for 24 hours at the same temperature. It was then treated with 0.01 M aqueous ammonium hydroxide at 120 °C for 9 hr. The wet silica gel column was soaked in 0.1M HNO3 for 3 hours, water for 2 hours, and 60% (volume ratio) N, N-dimethylformamide aqueous solution for 5 hours. Finally, the wet silica gel column was dried at a constant temperature of 60°C for 10 hours, and then burned at 700°C for 2 hours. Cut a 1cm long cylinder and set aside.

Embodiment 2

[0034] Silica monolithic adsorption column preparation

[0035] Weigh 1.2830g of polyethylene glycol (MW: 10000), dissolve it in 20ml of 0.01M acetic acid solution, add 10ml of tetramethylsiloxane under ice bath, and stir for 40min at the same temperature. After the tetramethylsiloxane solified mixture is ultrasonically degassed, it is poured into a straight tube mold (the straight tube mold is a plastic tube with a diameter of 50 mm and a length of 20 cm). At 45°C, stand for 2 hours to gel. Aged for 24 hours at the same temperature. It was then treated with 0.01 M aqueous ammonium hydroxide at 120 °C for 9 hr. The wet silica gel column was soaked in 0.1M HNO3 for 3 hours, water for 2 hours, and 60% (volume ratio) N, N-dimethylformamide aqueous solution for 5 hours. Finally, the wet silica gel column was dried at a constant temperature of 50°C for 12 hours, and then burned at 800°C for 1 hour. Cut a 15cm cylinder and set aside.

Embodiment 3

[0037] Silica monolithic adsorption column preparation

[0038] Weigh 1.2830g of polyethylene glycol (MW: 10000), dissolve it in 20ml of 0.01M acetic acid solution, add 10ml of tetramethylsiloxane under ice bath, and stir for 40min at the same temperature. After the tetramethylsiloxane solified mixture was ultrasonically degassed, it was poured into a straight tube mold (the straight tube mold is a metal tube with a diameter of 6 mm and a length of 5 cm). At 40°C, stand for 2 hours to gel. Aged for 24 hours at the same temperature. It was then treated with 0.01M aqueous ammonium hydroxide at 100°C for 11 hr. The wet silica gel column was soaked in 0.1M HNO3 for 3 hours, water for 2 hours, and 60% (volume ratio) N,N-dimethylformamide aqueous solution for 5 hours. Finally, the wet silica gel column was dried at a constant temperature of 60°C for 10 hours, and then burned at 700°C for 2 hours. Cut a 1cm cylinder and set aside.

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Abstract

The invention relates to a monolithic silica gel adsorption column, and a solid phase extraction device and application thereof. The monolithic silica gel adsorption column is prepared by a sol-gel method. The solid phase extraction device comprises a container, a solid phase extraction column, a filter flask, and a water circulating vacuum pump; and the lower end of the solid phase extraction column is provided with the monolithic silica gel adsorption column. The monolithic silica gel adsorption column is applied to solid phase extraction; compared with the common particle filler, the convective mass transfer speed of the monolithic silica gel adsorption column is greatly improved, samples can be quickly distributed in balance between a mobile phase and a fixed phase, and the monolithic silica gel adsorption column ensures purification and enrichment effects and realizes quick purification and enrichment of analyzed substances.

Description

【Technical field】 [0001] The invention relates to a monolithic adsorption column, in particular to a silica gel monolithic adsorption column and its solid-phase extraction device and application. 【Background technique】 [0002] Solid-phase extraction (SPE for short) mainly realizes the separation, purification and enrichment of samples through the selective adsorption and desorption process of solid-phase fillers on sample components. Its main purpose is to reduce sample matrix interference and improve detection sensitivity. . For convenience, solid-phase extraction generally uses solid-phase extraction cartridges, which have various specifications according to different needs, and the common ones are 1ml, 6ml and 10ml. [0003] The most commonly used fillers in solid phase extraction are granular silica gel or bonded phase silica gel. In order to achieve higher adsorption efficiency and reduce sample loss, the traditional granular packing has small particle size, but the ...

Claims

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Application Information

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IPC IPC(8): B01J20/283B01D11/02G01N30/08
Inventor 杜一平卫雪梅黄子夏张磊张维冰
Owner EAST CHINA UNIV OF SCI & TECH
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