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Preparation method and application of solid-phase microextraction fiber of self-assembly multi-layer porphyrin organic frame compound

A technology for extracting fibers and organic frameworks, which is applied in the fields of analytical chemistry and environmental chemistry, and can solve the problems of non-specific selectivity of materials, unsatisfactory reusability, and fragile matrix

Active Publication Date: 2019-04-09
HENAN INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The development of new SPME coatings plays a decisive role in the performance of SPME. Classical SPME fibers are obtained by modifying the surface of quartz fibers with polydimethoxysiloxane PDMS and other substances. Many researchers have used carbon nanotubes, graphene and polyionic liquids to modify the surface of the fiber to obtain a new type of SPME fiber, and the preparation of only a few COFs modified SPME is prepared by a sol-gel method or a one-pot method. The above-mentioned fibers have or the matrix is ​​fragile. Repeat The usability is not ideal, or the polymeric coating is not easy to control, the reproducibility between fiber batches is poor, and the material does not have specific selectivity, etc.

Method used

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  • Preparation method and application of solid-phase microextraction fiber of self-assembly multi-layer porphyrin organic frame compound
  • Preparation method and application of solid-phase microextraction fiber of self-assembly multi-layer porphyrin organic frame compound
  • Preparation method and application of solid-phase microextraction fiber of self-assembly multi-layer porphyrin organic frame compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Prepare the extraction probe

[0030] Under ventilated conditions, prepare aqua regia solution at a volume ratio of concentrated nitric acid to concentrated hydrochloric acid of 1:3. Use scissors to intercept 0.3mm diameter stainless steel wire about 20cm, put the intercepted stainless steel wire in the aqua regia solution for 70 minutes, take it out after the corrosion is completed, rinse it with distilled water, put it under a microscope to observe that its diameter is about 0.2mm, if it is not corroded to 0.2mm, continue to corrode until the diameter reaches 0.2mm. Cut off about 2cm from the needle of the 5μL micro-injector, fix the corroded stainless steel wire to the push rod of the micro-injector, and then tighten it with a nut so that it can conveniently control the extension and retraction of the fiber .

[0031] Modification of silanol and amino groups in self-made extraction probes

[0032] Solution A consisting of 10 mL of absolute ethanol and 2 mL of tetr...

Embodiment 2

[0036] Prepare the extraction probe

[0037]Under ventilated conditions, prepare aqua regia solution at a volume ratio of concentrated nitric acid to concentrated hydrochloric acid of 1:3. Use scissors to intercept 0.3mm diameter stainless steel wire about 20cm, put the intercepted stainless steel wire in the aqua regia solution for 70 minutes, take it out after the corrosion is completed, rinse it with distilled water, put it under a microscope to observe that its diameter is about 0.2mm, if it is not corroded to 0.2mm, continue to corrode until the diameter reaches 0.2mm. Cut off about 2cm from the needle of the 5μL micro-injector, fix the corroded stainless steel wire to the push rod of the micro-injector, and then tighten it with a nut so that it can conveniently control the extension and retraction of the fiber .

[0038] Modification of silanol and amino groups in self-made extraction probes

[0039] Solution A consisting of 10 mL of absolute ethanol and 2 mL of tetra...

Embodiment 3

[0043] Prepare the extraction probe

[0044] Under ventilated conditions, prepare aqua regia solution at a volume ratio of concentrated nitric acid to concentrated hydrochloric acid of 1:3. Use scissors to intercept 0.3mm diameter stainless steel wire about 20cm, put the intercepted stainless steel wire in the aqua regia solution for 70 minutes, take it out after the corrosion is completed, rinse it with distilled water, put it under a microscope to observe that its diameter is about 0.2mm, if it is not corroded to 0.2mm, continue to corrode until the diameter reaches 0.2mm. Cut off about 2cm from the needle of the 5μL micro-injector, fix the corroded stainless steel wire to the push rod of the micro-injector, and then tighten it with a nut so that it can conveniently control the extension and retraction of the fiber .

[0045] Modification of silanol and amino groups in self-made extraction probes

[0046] Solution A consisting of 10 mL of absolute ethanol and 2 mL of tetr...

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Abstract

The invention discloses a preparation method and application of a solid-phase microextraction fiber of a self-assembly multi-layer porphyrin organic frame compound, and belongs to the field of analytical chemistry and environmental chemistry. A stainless steel wire pretreated with aqua regia is sequentially modified with silicon hydroxyl and amino, and the porphyrin / porphyrin copper organic covalent frame compound modified solid-phase microextraction fiber is obtained by adopting a layer by layer self-assembly growth mode. A method for detecting the content of trace polycyclic aromatic hydrocarbon in water by the SPME-GC coupling technique is established, and an urban actual water sample is detected by the SPME-GC combined analysis, which discovers that the actual water sample can be effectively detected, and the home-made COFs material modified solid-phase microextraction fiber has a relatively good actual operation value.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and environmental chemistry, in particular to a porphyrin-based covalent organic framework compound-modified SPME fiber and a preparation method thereof, as well as an enrichment detection technology and application of aromatic compounds. Background technique [0002] Covalent Organic Frameworks (COFs) are a class of organic porous polymers with periodicity and crystallinity. The structural units are linked together by covalent bonds to form a porous framework with a periodic structure. Due to the covalent linkage of light elements, COFs have low density, high thermal stability, and inherent porosity, and have broad application potential in the research fields of gas adsorption, heterogeneous catalysis, and energy storage. [0003] Solid-phase microextraction (SPME) is a new extraction and separation technology developed on the basis of solid-phase extraction, which can solve the leakage of or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08G01N30/02G01N30/06G01N30/08G01N30/68
CPCB01D15/08B01J20/226B01J20/28023G01N30/02G01N30/06G01N30/08G01N30/68G01N2030/062
Inventor 李英侯玉霞段瑞娟陈坤崔承幸王吉超刘露荆瑞俊张裕平
Owner HENAN INST OF SCI & TECH
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