Preparation method of fullerene nano-coating gas chromatographic column

A gas chromatographic column and nano-coating technology, applied in the field of chromatographic columns, can solve problems such as easy loss, slow diffusion of samples in the chromatographic column, and performance degradation of the chromatographic column, and achieve the effect of thin solid phase and excellent space selectivity

Inactive Publication Date: 2019-06-14
李笃信 +1
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Problems solved by technology

In the separation research of gas chromatography, the fixed liquid is generally used to coat the inner wall of the fused silica capillary. Such a fixed liquid is easy to lose at high temperature, which reduces the performance of the chromatographic column. Secondly, the column length of the chromatographic column is longer, and the liquid film of the fi

Method used

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  • Preparation method of fullerene nano-coating gas chromatographic column
  • Preparation method of fullerene nano-coating gas chromatographic column
  • Preparation method of fullerene nano-coating gas chromatographic column

Examples

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Effect test

Embodiment 1

[0028] 1) Activate the fused silica capillary; transport the capillary into the tube with 1.2 mol / L sodium hydroxide, distilled water, 1% hydrofluoric acid by mass fraction, and distilled water in sequence, and activate for 45 minutes each.

[0029] 2) Amination treatment: A xylene solution containing 3% by mass fraction of γ-chloropropyltrimethoxysilane was passed through the capillary tube, reacted at 90°C for 4 hours; washed three times with methanol.

[0030] 3) Preparation of fullerene p-benzoate: 1 part of fullerene and 3 parts of p-azidobenzoic acid were dissolved with 40 parts of toluene, the reaction temperature was 180 C, and the reaction time was 6 hours;

[0031] 4) Bonding fullerenes to a capillary column: Pass a xylene solution containing 5% fullerene terephthalate into the capillary at a reaction temperature of 180°C for 3 hours; wash with toluene three times;

[0032] Analysis and characterization: analyzed by infrared spectroscopic tablet method, the extra 534...

Embodiment 2

[0035] 1) Amination treatment: Pass a xylene solution containing 5% γ-chloropropyltrimethoxysilane into the capillary, react at 75°C for 4 hours; wash with methanol three times.

[0036] 2) Preparation of fullerene p-benzoate: 1 part of fullerene and 3 parts of p-azidobenzoic acid were dissolved in 26 parts of toluene, the reaction temperature was 210C, and the reaction time was 6 hours;

[0037] 3) Bonding fullerenes to the capillary column: passing through the capillary a xylene solution containing 5.5% fullerene terephthalate by mass fraction, at a reaction temperature of 180°C, and reacting for 4 hours; washing with toluene three times;

[0038] Other parts are identical with embodiment 1.

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Abstract

The invention relates to a preparation method of a fullerene nano-coating gas chromatographic column. The method comprises that (1) fused quartz capillary tubes are activated; (2) amination treatmentis performed; (3) fullerene p-benzoate is prepared, wherein fullerene and azidobenzoic acid are dissolved in methylbenzene under the reaction temperature of 100-220 DEG C for the reaction time of 5-15hours; and (4) fullerene is bonded to a capillary column, wherein an xylene solution containing fullerene p-benzoate with the mass percent of 3%-15% is introduced into the capillary tubes for a reaction for 1-4 hours under the reaction temperature of 150-220 DEG C, the capillary tubes are washed three times with methylbenzene, and then the fullerene nano-coating gas chromatographic column is obtained. According to the method, by adopting fullerene as a stationary phase, the chromatographic column has an electron-lacking polyenoid property and has a high pi-pi interaction with an aromatic compound, thereby having high selectivity; and by the adoption of fullerene and a spherical structure of fullerene, the chromatographic column has excellent spatial selectivity on samples.

Description

technical field [0001] The invention relates to the technical field of chromatographic columns, in particular to a preparation method of a fullerene nano-coated gas chromatographic column. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs for short) are a class of carcinogens with large quantity and wide distribution, which mainly come from incomplete combustion of fossil fuels. These polycyclic aromatic hydrocarbons are produced to the environment. At the same time, PAHs in the environment can be absorbed by plants, thereby affecting human health. There are 16 PAHs designated on the U.S. Environmental Protection Agency (US-EPA) Priority Pollutants List. [0003] Chromatographic methods are generally used for the analysis and detection of such substances, especially gas chromatography, which has attracted people's attention for its advantages of rapidity, sensitivity, good separation performance, accurate quantification, and no use of organic solvents. I...

Claims

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Application Information

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IPC IPC(8): G01N30/60
Inventor 李笃信段翠翠
Owner 李笃信
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