Method for doping graphene in stationary phase of gas chromatographic column

A gas chromatographic column and graphene technology, applied in the field of analytical chemistry, can solve the problems of weak polarity of stationary phase, increase the roughness of the inner wall of capillary, single structure of stationary phase coating material, etc., and achieve strong Π-Π conjugated force. , Solve the effect of unstable fixation and high practical application value

Active Publication Date: 2020-09-18
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems that the stationary phase of the existing capillary chromatographic column is relatively weak in polarity, the structure of the stationary phase coating material is single, the specific surface area is insufficient, and the force is not rich enough, a method for doping graphene in the stationary phase of the gas chromatography column is now provided. , in order to achieve the purpose of increasing the roughness of the inner wall of the capillary, increasing the internal specific surface area, increasing the mixing force of the stationary phase, and adding graphene to the stationary phase by a physical occupying method

Method used

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  • Method for doping graphene in stationary phase of gas chromatographic column
  • Method for doping graphene in stationary phase of gas chromatographic column
  • Method for doping graphene in stationary phase of gas chromatographic column

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Experimental program
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Effect test

Embodiment 1

[0040]Embodiment one: the steps of traditional sodium chloride deposition method are as follows:

[0041] First, 10 g of solid sodium chloride powder was added to 40 ml of methanol five times at 2 g / time, ultrasonically dissolved, and left to settle to form a saturated methanol solution of sodium chloride.

[0042] Add 2ml of sodium chloride saturated methanol solution to a 50ml flat-bottomed flask, add a rotor, place it on a magnetic stirrer and stir vigorously, keep stirring, add 10ml of chloroform solution to it and continue stirring for 5min, then add 10ml to the mixed liquid Chloroform and stirred for 2min.

[0043] Move the mixed solution into a positive pressure container, make the mixed liquid pass through the cleaned capillary through the pressure, fully absorb, and transfer the whole capillary to the gas chromatography column thermostat after the liquid is emptied, pass nitrogen at 120°C for 180 minutes to obtain sodium chloride roughened capillary.

Embodiment 2

[0044] Embodiment two: sodium chloride deposition method simultaneously introduces the steps of graphene oxide as follows:

[0045] First, 10 g of solid sodium chloride powder was added to 40 ml of methanol five times at 2 g / time, ultrasonically dissolved, and left to settle to form a saturated methanol solution of sodium chloride.

[0046] Next, 0.04 g of single-layer graphene oxide was added to 40 ml of chloroform, and the mixed solution was ultrasonically pulverized for 180 min to form a uniform suspension.

[0047] Add 2ml of sodium chloride saturated methanol solution to a 50ml flat-bottomed flask, add a rotor, place it on a magnetic stirrer for vigorous stirring, keep stirring, add 10ml of trichloromethane suspension to it and continue stirring for 5min, add to the mixed liquid Continue to add 10ml of chloroform suspension and continue to stir for 2min.

[0048] Move the mixed solution into a positive pressure container, and use the pressure to make the mixed liquid pas...

Embodiment 3

[0049] Embodiment three: the preparation steps of the ionic liquid chromatographic column doped with monolayer graphene oxide in the stationary phase are as follows:

[0050] The roughened capillaries in Examples 1 and 2 were taken for use; the ionic liquid (see Chinese invention patent for details: a dicationic imidazole-based ionic liquid and its preparation method) was prepared as 1% m / v The coating solution is ready for use; take 1g of glyceryl stearate and heat it up to 80°C to liquefy it for use;

[0051] ① Move the coating liquid into a positive pressure container, connect the capillary in Example 1, and pass the positive pressure to fill the capillary with the coating liquid;

[0052] Stop the injection pressure, one end of the capillary is sealed by glyceryl stearate, and the other end is connected to the static coating capillary column in the vacuum pump;

[0053] Put the coated capillary chromatographic column into a gas chromatograph column oven at 120°C for aging...

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Abstract

The invention discloses a method for doping graphene in a stationary phase of a gas chromatographic column, and relates to the technical field of analytical chemistry. The method specifically comprises the following steps: adding sodium chloride into a methanol solution to prepare a sodium chloride saturated methanol solution, ultrasonically crushing graphene in trichloromethane for 2 h to preparetrichloromethane turbid liquid of graphene, mixing the sodium chloride saturated methanol solution with the trichloromethane turbid liquid of graphene to prepare mixed turbid liquid, and performing physical saturated adsorption treatment on a capillary tube. The method has the characteristics of simple operation, universal mode, uniform adhesion, low column loss and the like. The deposition method is suitable for various chromatographic column stationary phases, can significantly improve the roughness of the inner surface of the chromatographic column and increase the internal specific surface area, is suitable for various chromatographic column stationary phases, can significantly improve the column efficiency, and has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to a method for doping graphene in a stationary phase of a gas chromatography column. Background technique [0002] In capillary gas chromatography analysis, the effect of separation and detection is achieved through the difference in force between the stationary phase and the analyzed components. Graphene is used in the solid phase of capillary gas chromatography. Due to its unique molecular structure and π-π stacking effect with benzene ring-containing compounds, it has special selectivity for aromatic substances. In addition, it has special selectivity for amines and alcohols that are easy to tail. It has a good selective separation ability, making graphene an ideal gas chromatography stationary phase. Fan et al. directly coated graphene on the inner wall of the quartz capillary. Compared with the commercial HP-5MS column, the column with graphene as the stationary ...

Claims

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Application Information

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IPC IPC(8): B01D15/20
CPCB01D15/206
Inventor 观文娜王诗雨毛鑫涛刘婷婷
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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