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
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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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