Method for preparing titanium-based graphene coating for solid phase microextraction

A technology of carboxylated graphene and graphene, which is applied in the fields of analytical chemistry and environmental analysis, can solve the problems of limiting the service life of quartz fibers and being easy to break, and achieve the effects of long-term use, strong adsorption, and improved extraction efficiency

Inactive Publication Date: 2013-06-05
BEIJING NORMAL UNIVERSITY
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The surface of the quartz fiber is rich in hydroxyl groups, which is very beneficial to the bonding of the micro-extraction coating, but the quartz fiber material itself is brittle and easily broken during the extraction process, which limits the service life of the quartz fiber

Method used

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  • Method for preparing titanium-based graphene coating for solid phase microextraction
  • Method for preparing titanium-based graphene coating for solid phase microextraction
  • Method for preparing titanium-based graphene coating for solid phase microextraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] see figure 1 —— image 3 , Take a 10cm-long titanium wire, and sonicate it in 5mL acetone, methanol and deionized water for 5min to remove surface dirt. After taking it out, it was immersed in a 1mol / L sodium hydroxide solution for hydroxylation treatment in a water bath at 70°C for 1 hour, and immediately placed in an oven at 120°C to react for 30 minutes. After the titanium wire is taken out, use 1 mol / L hydrochloric acid solution, methanol and deionized water to wash the free hydroxide ions on the surface. After drying, the titanium wire was immersed in a 10% toluene solution of 3-propyltriethoxysilane for 12 hours for silanization. Under ultrasonic conditions, 0.1 mg of carboxylated graphene was added to 5 mL of N,N'-dimethylformamide, followed by 0.1 mg of N,N'-dicyclohexylcarbodiimide, and mixed well. Remove the titanium wire from the silanization reagent, and immediately put it in the oven for drying and stabilization; after the drying, insert the titanium wire ...

Embodiment 2

[0036] According to the above experimental scheme, the prepared titanium-based graphene solid phase microextraction coating was compared with the commercial solid phase microextraction coating PDMS:

[0037] 1) Use commercial SPME's 100μm thick PDMS to age at 280°C for 30min, immerse it in 8mL 0.1μg / L phthalate solution at 70°C in a water bath, 400r / min speed, potassium chloride At a concentration of 20%, extract for 40 minutes; insert the extracted extraction head directly into the GC port, analyze at 280°C for 5 minutes, and perform GC-MS analysis to obtain Figure 5 The result shown.

[0038] 2) Use the titanium-based graphene solid phase microextraction coating to extract the prepared phthalate solution under the same conditions, and then perform GC-MS analysis to obtain Figure 5 The result shown.

[0039] by Figure 5 As shown, the extraction effect of the titanium-based graphene micro-extraction coating prepared in Example 1 is better than that of a commercial 100 μm thick ...

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Abstract

The invention discloses a method for preparing a titanium-based graphene coating for solid phase microextraction. The method comprises five steps. According to the method, a silanization agent serves as an intermediate carrier, graphene is modified on the surface of a metal titanium wire, a coating which has a multi-layer sheet graphene structure is formed on the titanium-based surface, and the material can be applied to the extraction head in the solid phase microextraction technology. The method is advanced in thought, clear in concept, simple and convenient in coating preparation, the thickness is controllable, and the obtained coating is uniform, stable and high-temperature resistant. According to the solid phase microextraction head, trace phthalate in different water samples such as running water, underground water and lake water can be extracted at high efficiency, the corresponding detection limit can be 0.030mu g / L, the reproducibility is 2.2-12.6 percent, the marked recovery rate is 73.8-104.5 percent, and the repeated extraction frequency exceeds 200 times. The method has wide application prospects in the technical field of analytical chemistry and environmental analysis.

Description

Technical field [0001] The invention relates to a method for preparing a multilayer graphene structure solid-phase micro-extraction coating based on titanium wire, in particular to a method for preparing a titanium-based graphene coating for solid-phase micro-extraction, belonging to analytical chemistry and environmental analysis Technical field. Background technique [0002] Solid phase microextraction technology (SPME) is a new sample pretreatment technology developed in the 1990s, integrating extraction, concentration and analysis. After successful development by the Canadian Pawliszyn research group, Supelco launched a commercial SPME device in 1993. After SPME was launched, in just a few decades, it has been widely used in sample pretreatment, and has successfully realized online coupling with gas chromatography (GC) and liquid chromatography (HPLC), greatly reducing The pre-treatment time and the extraction efficiency are improved. The selection and loading of the coati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/32B01D15/20
Inventor 张波涛郑晓霞滕彦国李海芳林金明
Owner BEIJING NORMAL UNIVERSITY
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