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Preparation method for grapheme open-tube electric chromatographic column

An electrochromatographic column and graphene technology, applied in the field of chromatography, can solve the problems of long modification time and achieve the effects of low cost, increased modification amount, and easy operation

Active Publication Date: 2014-03-05
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dopamine can be polymerized on the surface of various organic or inorganic materials to form polydopamine, but the modification of polydopamine on the inner wall of capillary requires repeated coating, and the modification takes a long time

Method used

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  • Preparation method for grapheme open-tube electric chromatographic column
  • Preparation method for grapheme open-tube electric chromatographic column
  • Preparation method for grapheme open-tube electric chromatographic column

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Take a 60cm-long quartz capillary (50 μm i.d. × 375 μm o.d.), rinse it with 1M NaOH for 2 hours, rinse it with pure water for half an hour, and dry it with nitrogen; (2) Prepare N-phenyl-3-aminopropyl trimethyl Oxysilane ethanol solution (20%, v / v), put it into the pretreated capillary for silanization reaction, react at 60°C for 12h, wash with pure ethanol after the reaction, and blow dry with nitrogen; (3) Separately configure 0.2M aniline hydrochloric acid solution and 0.05M ammonium persulfate hydrochloric acid solution, the above two solutions were mixed in equal volumes and then quickly passed into the silanized capillary tube, reacted overnight, washed with pure water, and treated at 120 ° C for 3 hours, Obtain a capillary bonded with polyaniline; (4) Weigh 10 mg of dopamine and dissolve it in 5 mL of 10 mM Tris buffer, adjust the pH value to 8.5, shake the prepared dopamine solution for 10 minutes, and then dissolve it at a flow rate of 0.05 mL / h Continuousl...

Embodiment 2

[0032] (1) Take a 60cm-long quartz capillary (50 μm i.d. × 375 μm o.d.), rinse it with 1M NaOH for 2 hours, rinse it with pure water for half an hour, and dry it with nitrogen; (2) Prepare N-phenyl-3-aminopropyl trimethyl Oxysilane ethanol solution (20%, v / v), put it into the pretreated capillary for silanization reaction, react at 60°C for 24h, wash with pure ethanol after the reaction, and blow dry with nitrogen; (3) Separately configure 0.2M aniline hydrochloric acid solution and 0.05M ammonium persulfate hydrochloric acid solution, the above two solutions were mixed in equal volumes and then quickly passed into the silanized capillary tube, reacted overnight, washed with pure water, and treated at 120 ° C for 3 hours, A capillary bonded with polyaniline is obtained; (3′) repeating the polyaniline modification step once to obtain a double-layer polyaniline modified capillary. (4) Weigh 10 mg of dopamine and dissolve it in 5 mL of 10 mM Tris buffer, adjust the pH to 8.5, sha...

Embodiment 3

[0036] (1) Take a 60cm-long quartz capillary (50 μm i.d. × 375 μm o.d.), rinse it with 1M NaOH for 2 hours, rinse it with pure water for half an hour, and dry it with nitrogen; (2) Prepare N-phenyl-3-aminopropyl trimethyl Oxysilane ethanol solution (50%, v / v), put it into the pretreated capillary for silanization reaction, react at 60°C for 12h, wash with pure ethanol after the reaction, and blow dry with nitrogen; (3) Separately configure 0.2M aniline hydrochloric acid solution and 0.05M ammonium persulfate hydrochloric acid solution, the above two solutions were mixed in equal volumes and then quickly passed into the silanized capillary tube, reacted overnight, washed with pure water, and treated at 120 ° C for 3 hours, Obtain a capillary bonded with polyaniline; (4) Weigh 10 mg of dopamine and dissolve it in 5 mL of 10 mM Tris buffer, adjust the pH value to 8.5, shake the prepared dopamine solution for 10 minutes, and then dissolve it at a flow rate of 0.05 mL / h Continuousl...

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Abstract

The invention relates to a preparation method for a grapheme open-tube electric chromatographic column, and relates to the preparation method for a novel capillary electric chromatographic column. In the method, a conductive polymer polyaniline assisted polydopamine bonded graphite oxide is used as a fixed phase. The conductive polymer polyaniline is bonded to the inner wall of a capillary to serve as an underlying material, so that the specific surface area of the capillary is increased, the modification time and the modification frequency of dopamine are remarkably reduced, and the modification degree of the polydopamine is improved; and therefore, the reaction of the graphite oxide is facilitated. The preparation method is easy to operate and low in cost; the overall preparation process is performed in aqueous solution, and an organic solvent or a toxic reagent is not used; the environment is not polluted; each prepared coating has the high stability; the service life of the capillary column is long; according to the grapheme open-tube electric chromatographic column prepared by using the preparation method, the chromatographic performance of the grapheme open-tube column is remarkably improved, and the effect on separating the homologs of benzene is better compared with that of a polydopamine bonded graphite oxide open-tube.

Description

technical field [0001] The invention relates to the technical field of chromatography, in particular to a preparation method of a graphene open-tube electrochromatographic column. Background technique [0002] Capillary electrochromatography is a new type of micro-separation technology with high efficiency, rapidity and high selectivity. It is developed by combining the advantages of high efficiency of capillary electrophoresis and high selectivity of high performance liquid chromatography, and has the advantages of fast analysis speed, high column efficiency, and less consumption of samples and solvents. The preparation of electrochromatographic column is the core of capillary electrochromatographic separation and analysis. The performance of chromatographic columns such as column efficiency, column reproducibility, and column life are the evaluation indicators for the practical application of chromatographic columns. Therefore, the preparation of electrochromatographic co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30
Inventor 陈子林张娟
Owner WUHAN UNIV
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