Solid phase extraction column based on graphene bonded silica gel, and preparation method and application thereof

A technology of solid-phase extraction column and bonded silica gel, which is applied in the field of sample pretreatment in analytical chemistry, can solve the problems of inconvenient extraction and elution of target substances, difficult-to-elute analytes, and clogged extraction columns, etc., achieving fast extraction speed, The effect of large extraction capacity and improved adsorption performance

Inactive Publication Date: 2013-01-16
XINYANG NORMAL UNIVERSITY
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  • Abstract
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Problems solved by technology

However, due to the strong surface energy of graphene, it is easy to agglomerate itself, which seriously clogs the extraction column and brings inconvenience to the extraction and elution of the target.
[0006] Therefore, to provide a graphene material can be covalently bonded to silica gel, to prepare a new type of solid phase extraction column, to solve the problem of simply using graphene to prepare and extract Difficult-to-elute analytes due to graphene agglomeration on columns

Method used

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  • Solid phase extraction column based on graphene bonded silica gel, and preparation method and application thereof
  • Solid phase extraction column based on graphene bonded silica gel, and preparation method and application thereof
  • Solid phase extraction column based on graphene bonded silica gel, and preparation method and application thereof

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Effect test

Embodiment 1

[0030] like figure 1 , place the porous lower sieve plate 3 at the bottom of the solid-phase extraction column tube 1, weigh 10 mg of graphene-bonded silica gel filler 4 and put it into the solid-phase extraction column tube 1, and then place the porous upper sieve plate 2 on the graphite The upper part of the olefin-bonded silica gel is compacted to obtain a graphene-bonded silica gel solid-phase extraction column.

Embodiment 2

[0032] The synthesis of graphene-bonded silica can be divided into the following four steps:

[0033] (1) Graphite oxide was prepared according to the literature (W. Hummers, R. Offeman, J. Am. Chem. Soc. 80 (1958) 1339-1340.), and the graphene oxide dispersion was obtained by ultrasonic exfoliation in twice distilled water;

[0034] (2) Add 5.0 g of silica gel to 6 mol / L hydrochloric acid, stir and heat to reflux state, and keep it for 4 h, after cooling, wash with distilled water until neutral, and dry at 70°C to obtain pretreated silica gel ; Then take 1 g of pretreated silica gel and add it to 75 mL of toluene, after heating to reflux state, add 5 mL of 3-aminopropyltriethoxysilane dropwise, continue to stir and reflux for 12 h, cool, and wash off the toluene with ethanol and a silylating agent, washed with distilled water, and dried at 70°C to obtain secondary treatment silica gel;

[0035] (3) Add secondary treatment silica gel to 150 mL graphene oxide dispersion, heat ...

Embodiment 3

[0038] Silica gel particle size optimization: The amount of graphene bonded to silica gel with different particle sizes is different, and the gap size between the fillers is also different, which affects its extraction performance and elution effect. Silica gel a1, silica gel a2 with a particle size of 74~165 microns, and silica gel a3 with a particle size of 47~74 microns were optimized for experiments: the experimental results are as follows figure 2 As shown, the extraction column packing made of silica gel a1 with a particle size of 245 microns has the highest extraction efficiency.

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Abstract

The invention relates to a solid phase extraction column based on graphene bonded silica gel, which is used in concentration and separation of organic pollutants in an environmental water sample. A graphene bonded silica gel padding is prepared by taking 3-aminopropyl triethoxy silane (APTES) as the cross-linking agent; then graphene is bonded on the surface of silica gel; after product graphene bonded silica gel granules are evenly filled in a solid phase extraction column, the graphene bonded silica gel based solid phase extraction column is obtained. The performance indicators of the solid phase extraction column are tested through polycyclic aromatic hydrocarbons, including naphthalene, acenaphthylene, fluorene, phenanthrene, fluoranthene and pyrene, and the test result shows that the solid phase extraction column has good extraction efficiency, reproducibility and stability. The graphene bonded silica gel has the characteristics of big specific surface area, strong Pi electron adsorption ability and high extraction capacity of the graphene, and the stable mechanical property and good adsorption ability of the silica gel. Moreover, the solid phase extraction column based on the graphene bonded silica gel is low in preparation cost and simple to operate and is suitable to be used for pretreatment of low-concentration organic pollutants in a big-volume water sample. The solid phase extraction column has a good application prospect in the concentration and separation of environmental organic pollutants.

Description

technical field [0001] The invention relates to the technical field of sample pretreatment in analytical chemistry, in particular to a solid-phase extraction column based on graphene-bonded silica gel and a preparation method thereof, which are mainly used for enriching and separating organic pollutants in environmental water samples. Background technique [0002] Environmental sample matrices are generally diverse and complex, and the concentration of target pollutants in many samples is relatively low. As the main object of environmental monitoring, obtaining accurate and reliable data, pre-enrichment and purification of samples has become a key link. At present, there are many technical researches on sample pretreatment, such as solid-phase extraction, liquid-phase extraction, supercritical fluid extraction and microwave-assisted extraction. Among them, solid phase extraction has the advantages of low cost, simple operation, fast, easy automation, less use of organic sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/22C02F1/28G01N30/06
Inventor 黄克靖谢宛珍刘彦明李靖
Owner XINYANG NORMAL UNIVERSITY
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