A kind of preparation method of graphene-coated solid-phase microextraction fiber

A technology for extracting fibers and graphene, applied in chemical instruments and methods, material separation, instruments, etc., can solve the problems of easy falling off of graphene coating and short service life, and achieve improved convenience, improved fragility, and improved use. effect of life

Inactive Publication Date: 2016-10-19
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Graphene has also been applied to the preparation of solid-phase microextraction fiber coatings, showing good extraction performance, but the existing preparation methods are mostly limited to physical coating and sol-gel methods, because there is no solid-phase microextraction between the graphene coating and the carrier. Chemical bonding, resulting in easy peeling of graphene coating and short service life

Method used

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  • A kind of preparation method of graphene-coated solid-phase microextraction fiber
  • A kind of preparation method of graphene-coated solid-phase microextraction fiber
  • A kind of preparation method of graphene-coated solid-phase microextraction fiber

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Effect test

Embodiment 1

[0026] Embodiment 1: Preparation of graphene-coated stainless steel wire solid-phase microextraction fiber

[0027] Include the following steps A and B in turn:

[0028] A. Metal wire electroless silver plating

[0029] After 10 centimeters of long 0.15 millimeters thick stainless steel wire one end 3 centimeters are washed with water, methanol successively, put into electroless silver plating solution, the mass percent composition of glucose is 10%, and the mol ratio of silver ammonia ion and glucose is 1: 1. The silver plating reaction time is 2 hours at 20°C, and a layer of silver is deposited on the wire;

[0030] B. Preparation of Graphene Coating

[0031] Put the silver-plated end of the metal wire into a toluene solution of 20mmol / L 3-mercaptopropyltrimethoxysilane for 24 hours, self-assemble a layer of 3-mercaptopropyltrimethoxysilane molecules on the silver coating, and then place it in 0.1 Hydrolyze in mol / L dilute hydrochloric acid for 5 hours to hydroxylate the ...

Embodiment 2

[0032] Embodiment 2: Preparation of graphene-coated iron wire solid-phase microextraction fiber

[0033] Include the following steps A and B in turn:

[0034] A. Metal wire electroless silver plating

[0035] Wash one end 3 cm of a 15 cm long and 0.2 mm thick iron wire with water and methanol, and then put it into the electroless silver plating solution, the mass percentage of glucose is 15%, and the molar ratio of silver ammonia ion to glucose is 1:1.5 , the reaction time of silver plating at 25°C is 1.5 hours, and a layer of silver is deposited on the wire;

[0036] B. Preparation of Graphene Coating

[0037] Put the silver-plated end of the metal wire into a toluene solution of 10mmol / L 3-mercaptopropyltrimethoxysilane for 36 hours, self-assemble a layer of 3-mercaptopropyltrimethoxysilane molecules on the silver coating, and then place it in 0.5 Hydrolyze in mol / L dilute hydrochloric acid for 3 hours to hydroxylate the wire, take it out and dry it, put it in 20% ethanol...

Embodiment 3

[0038] Embodiment 3: Preparation of graphene-coated titanium wire solid-phase microextraction fiber

[0039] Include the following steps A and B in turn:

[0040] A. Metal wire electroless silver plating

[0041] 15 centimeters long 0.18 millimeters thick titanium wire one end 2 centimeters cleans up successively with water, methanol, puts into electroless silver plating solution, the mass percentage composition of glucose is 20%, and the mol ratio of silver ammonia ion and glucose is 1: 2. The reaction time of silver plating at 30°C is 1 hour, and a layer of silver is deposited on the wire;

[0042] B. Preparation of Graphene Coating

[0043] Put the silver-plated end of the metal wire into a toluene solution of 50mmol / L 3-mercaptopropyltrimethoxysilane for 8 hours, self-assemble a layer of 3-mercaptopropyltrimethoxysilane molecules on the silver coating, and then place Hydrolyze in 0.3mol / L dilute hydrochloric acid for 5 hours to hydroxylate the wire, take it out and dry ...

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Abstract

The invention discloses a method for preparing a solid phase micro-extraction fiber of a graphene coating on a metal wire carrier, and particularly relates to a method for bonding graphene on a functionalized metal wire surface by using ionic liquid as a crosslinking agent. The new method is characterized by comprising the following steps: selecting a metal wire as a carrier; firstly carrying out chemical silvering; then carrying out hydroxylation; finally, bonding graphene oxide on the hydroxylated metal wire by taking the functionalized ionic liquid as the crosslinking agent, so as to obtain a novel solid phase micro-extraction fiber of the graphene coating. The solid phase micro-extraction fiber prepared by the method has the characteristics of high mechanical strength, stable extracting coating, high enrichment capacity, long service life, good application potentiality and the like, and can be applied to enrichment analysis of trace components in samples such as foods, environments, medicines and biochemistry.

Description

technical field [0001] The invention relates to a technique for preparing solid-phase microextraction fiber of graphene bonding coating on a metal wire carrier. Background technique [0002] Solid-phase microextraction is a new type of sample pretreatment technology developed in the 1990s. It has the advantages of low cost, strong enrichment ability, fast analysis speed, easy operation, low solvent demand or even no solvent, convenient on-site analysis and It has been widely used in the enrichment analysis of trace components in food, environmental, pharmaceutical and biochemical samples due to its advantages of being easy to combine with chromatographic instruments. The core component of this technology is the solid-phase microextraction fiber, and the performance of the solid-phase microextraction fiber depends on the properties of the carrier and the extraction coating. The original solid-phase microextraction fiber uses fused silica rod as the carrier, which affects the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30G01N30/56
CPCB01J20/286B01J20/30B01J2220/48G01N30/06
Inventor 孙敏冯娟娟罗川南步亚南王俊凯
Owner UNIV OF JINAN
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