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Graphene material based disperse and quick solid-phase extraction method

A graphene and extraction technology, applied in material separation, analysis materials, instruments, etc., can solve the problem of low graphene density, and achieve the effect of simple operation, simplified cumbersome operation, and good separation effect.

Active Publication Date: 2014-12-17
SINOPHENE NOVEL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, direct use of graphene for dispersive and rapid solid phase extraction is not very suitable for operation, mainly because the density of graphene is too small, it is difficult to fully separate graphene from the sample during centrifugation
Moreover, in the current technology, graphene is only used as a strong non-polar solid phase extraction agent, and the advantages of graphene have not been fully utilized to obtain a better separation effect.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] 1. Put single-layer graphene into a tube furnace, feed nitrogen, heat to 300°C in a nitrogen atmosphere, stop feeding nitrogen, and feed water vapor into the tube furnace for activation for 3 hours, wherein the flow rate of water vapor It is 5mL / min. Then, stop feeding water vapor, change to nitrogen, stop heating after 5 minutes, take out the graphene material, rinse with deionized water for 3 times, and dry at 60°C for 2 hours to obtain activated single-layer graphene.

[0081] 2. Mix phenol, 4,4'-dichlorobiphenyl, biphenyl, naphthalene and pyrene to prepare a working solution with the concentration of each component being 100 μg / Kg. The solvent is dichloromethane, and then add porphyrin As an impurity component, the concentration of porphyrin was 1 mg / L.

[0082] 3. Take 5g of the above-mentioned working solution, add the above-mentioned activated single-layer graphene into 5g of the above-mentioned working solution according to the ratio of adding 30mg of solid-pha...

Embodiment 2

[0086] 1. Put the aminated graphene into a tube furnace, feed nitrogen, heat to 500°C in a nitrogen atmosphere, stop feeding nitrogen, and feed water vapor into the tube furnace for activation for 1 hour, wherein the flow rate of water vapor 0.5mL / min. Then, stop feeding water vapor, change to nitrogen gas, stop heating after 1 min, take out the graphene material, rinse with deionized water for 3 times, and dry at 80°C for 1 h to obtain activated aminated graphene.

[0087] 2. Mix phenylalanine, leucine, histidine, and lysine to prepare a working solution with a concentration of 100 μg / L for each component. The solvent is acetonitrile, and methyl violet is added as an impurity group Minutes, the concentration of methyl violet is 1mg / L.

[0088] 3. Take 5g of the above-mentioned working solution, add the above-mentioned activated aminated graphene into 5g of the above-mentioned working solution according to the ratio of adding 5mg of solid phase extractant per gram of each com...

Embodiment 3

[0092] 1. Put carboxylated graphene into a tube furnace, feed nitrogen, heat to 400°C in a nitrogen atmosphere, stop feeding nitrogen, and feed water vapor into the tube furnace for activation for 2 hours, wherein the flow rate of water vapor It is 2mL / min. Then, stop feeding water vapor, change to nitrogen gas, stop heating after 3 minutes, take out the graphene material, rinse with deionized water for 3 times, and dry at 70° C. for 1.5 h to obtain activated carboxylated graphene.

[0093] 2. Grind Coptis Rhizoma with a food grinder and pass it through a 100-mesh sieve to obtain Coptis Rhizoma powder, then take 0.5g of Coptis Rhizoma powder and add it to 200ml of mixed solvent of hydrochloric acid-methanol (the volume ratio of hydrochloric acid and methanol is 1:100), and extract in a water bath at 60°C 2h, and then ultrasonically crush the remaining Coptis rhizome residue. Finally, the residue of Coptidis rhizome was removed by filtration, and the extract solution of Coptid...

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Abstract

The invention relates to a graphene material based disperse and quick solid-phase extraction method. The graphene material based disperse and quick solid-phase extraction method comprises the steps of performing pore forming and activation on a graphene material to obtain an activated graphene material, wherein the graphene material is graphene or modified graphene; adding the activated graphene material into a chemical sample to be processed to obtain a mixture, shaking and extracting the mixture, then performing centrifugation to obtain a precipitate and supernate, wherein the supernate contains a target component to be detected. The grid cross-linking degree of the activated graphene material is improved, and the graphene material is easily separated in the centrifugal or filtered operation. By means of the method, a disperse solid-phase extraction technology and the activated graphene material serving as a solid-phase extraction solution can be combined, and a complicated operation in traditional solid-phase extraction is simplified and is simple. Impurities can be selectively absorbed by the activated graphene material, and accordingly impurity removal is effectively performed on chemical samples. Therefore, the method is good in separation effect.

Description

technical field [0001] The invention relates to the technical field of chemical sample pretreatment, in particular to a graphene material-based dispersive fast solid-phase extraction method. Background technique [0002] In order to perform chromatographic analysis better, the most commonly used sample pretreatment technology is solid-phase extraction (SPE) technology, that is, to achieve adsorption and extraction through the affinity between specific components in the components and solid-phase extraction agents, so as to achieve specific components. separation. Therefore, the choice of solid phase extraction agent is extremely important. [0003] Traditional solid-phase extraction technology requires a series of operations such as activation, column loading, and elution, which complicates the detection process. Therefore, the improved and efficient dispersive rapid solid-phase extraction (DSPE) technology is gradually replacing the position of SPE. The DSPE operation pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08
Inventor 张明东张麟德
Owner SINOPHENE NOVEL MATERIALS
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