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Preparation method of in-tube solid-phase micro-extraction column

A solid-phase microextraction column and capillary technology, which is applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problem of automatic online combination of extraction, analysis and detection, and long extraction time of needle-type SPME fibers , unable to achieve automatic extraction and other problems, to achieve the effect of shortening the analysis time, improving precision and accuracy, and prolonging the service life

Inactive Publication Date: 2014-03-19
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solid-phase extraction operation based on graphene-modified silica particles is very complicated, and automatic extraction cannot be realized. The needle-type SPME fiber based on graphene coating has a long extraction time and limited enrichment multiples, and it is difficult to achieve extraction and analysis in the same area. Integrated automatic online connection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take a quartz capillary with an inner diameter of 0.25mm and a length of 1m, wash it with 0.1M sodium hydroxide for 0.5 hours, then with 0.1M HCL hydrochloric acid for 0.5 hours, and finally wash it with deionized water until it is neutral, and dry it with nitrogen.

[0022] The treated capillary column was filled with 20 mM APTES toluene solution, reacted at room temperature for 12 hours, then taken out and placed in a water bath at 70 °C to continue the reaction for 5 hours, then taken out, rinsed with toluene, and then rinsed with water.

[0023] After sonicating the 0.2 mg / mL graphene oxide aqueous solution for a period of time, centrifuge at 3000 rpm for 5 min, take 4 mL of the supernatant, add 10 μL of 10 mM EDC / 5 mM NHS, activate it for 0.5 hours, and pour it into the capillary, The reaction was carried out in a water bath at 70 °C for 2 hours, and dried with nitrogen to obtain a graphene microextraction column in the tube.

Embodiment 2

[0025] Take a quartz capillary with an inner diameter of 0.53 mm and a length of 1 m, first wash it with 0.1M sodium hydroxide for 0.5 hours, then with 0.1M HCL hydrochloric acid for 0.5 hours, and finally wash it with deionized water until it is neutral, and dry it with nitrogen.

[0026] The treated capillary column was filled with 20 mM APTES toluene solution, reacted at room temperature for 12 hours, then taken out and placed in a water bath at 70 °C to continue the reaction for 5 hours, taken out, rinsed with toluene, and then rinsed with water.

[0027] After sonicating the 0.2 mg / mL graphene oxide aqueous solution for a period of time, centrifuge at 3000 rpm for 5 min, take 4 mL of the supernatant, add 10 μL of 10 mM EDC / 5 mM NHS, activate it for 0.5 hours, and pour it into the capillary. , reacted in a water bath at 70°C for 2 hours, and dried with nitrogen to obtain a graphene micro-extraction column in the tube.

Embodiment 3

[0029] Take a quartz capillary with an inner diameter of 0.25mm and a length of 1m, wash it with 0.1M sodium hydroxide for 0.5 hours, then with 0.1M HCL hydrochloric acid for 0.5 hours, and finally wash it with deionized water until it is neutral, and dry it with nitrogen.

[0030] The treated capillary column was filled with 20 mM APTES toluene solution, reacted at room temperature for 12 hours, then taken out and placed in a water bath at 70 °C to continue the reaction for 5 hours, then taken out, rinsed with toluene, and then rinsed with water.

[0031] The 0.2 mg / mL carbon nanotube aqueous solution was sonicated for a period of time, centrifuged at 3000 rpm for 5 min, 4 mL of the supernatant was taken, 10 μL of 10 mM EDC / 5 mM NHS was added, and after activation for 0.5 hours, it was poured into the capillary, The reaction was carried out in a water bath at 70°C for 2 hours, and dried with nitrogen to obtain a carbon nanotube microextraction column in the tube.

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Abstract

The invention discloses an in-tube solid-phase micro-extraction column and a preparation method thereof, and belongs to the technical field of analytic chemistry sample pretreatment. The in-tube solid-phase micro extraction column is composed of a quartz capillary tube and a graphene oxide coating layer, wherein the graphene oxide coating layer is fixed on the inner wall of the quartz capillary tube through chemical bonding. During preparation, the inner wall of the quartz capillary tube is successively washed with an acid, washed with an alkali and blown to dry by nitrogen, a toluene solution containing 3-aminopropyltriethoxysilane (APTES) is poured into the capillary tube, the capillary tube has both ends sealed and is placed in a water bath for reaction, then a graphene oxide aqueous solution activated by 1-ethyl-3-(3-dimethylaminopropyl)-carbide diimine / N-hydroxy succinimide (EDC / NHS) is poured into the capillary tube, the capillary tube has the both ends sealed and is subjected to a reaction in the water bath, the graphene oxide is allowed to be bonded to the quartz capillary tube wall, and the in-tube solid-phase micro-extraction column is obtained. The in-tube solid-phase micro-extraction column has simple and rapid preparation method, allows the graphene coating layer to have good chemical property, mechanical property and thermal stability, has high extraction capacity and long service life, and has broad application prospects in the analytic chemistry and environmental analysis fields.

Description

technical field [0001] The invention discloses a preparation method of an in-tube solid-phase micro-extraction column, which is mainly used for the separation and enrichment of target substances in complex aqueous solution samples, and belongs to the technical field of analytical chemical sample pretreatment. Background technique [0002] Pretreatment is an important step in the analysis of complex samples. Through pretreatment, the interfering substances in the sample are removed and the target substance is concentrated, so as to make up for the deficiency of the existing separation technology and the detection sensitivity of the instrument. Environmental sample analysis is roughly divided into four steps: ① sample collection, ② sample pretreatment, ③ analysis and determination, and ④ data processing. For the analysis of samples with complex matrices, the time spent on sample preparation often accounts for two-thirds or more of the entire analysis process. With the contin...

Claims

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Application Information

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IPC IPC(8): B01D15/20
Inventor 谭峰李莲君陈景文全燮
Owner DALIAN UNIV OF TECH
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