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Mil-101 ​​type mof material micro solid phase extraction probe and preparation method

A MOF and extraction technology, applied in the field of sample pretreatment technology and environmental sample analysis and detection, can solve the problems of high price, limited life, adsorption overload, etc., and achieve the effect of convenient operation, low detection limit and less organic solvent.

Inactive Publication Date: 2016-06-01
CHINA UNIV OF PETROLEUM (EAST CHINA)
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Problems solved by technology

[0006] The purpose of the present invention is to provide a MIL-101 metal-organic framework (MOF) micro-solid-phase extraction probe and its preparation method, which can solve the shortcomings of traditional solid-phase extraction probes such as limited life, high price, adsorption overload and easy breakage. , to reduce the loss of target substances during the extraction process and make the extraction process have both the advantages of hollow fiber membrane protection and solid phase extraction, which can be used for direct analysis and detection of PCBs in complex environmental samples

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  • Mil-101 ​​type mof material micro solid phase extraction probe and preparation method
  • Mil-101 ​​type mof material micro solid phase extraction probe and preparation method
  • Mil-101 ​​type mof material micro solid phase extraction probe and preparation method

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Embodiment Construction

[0021] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0022] The MIL-101 type MOF material micro-solid-phase extraction probe of the present invention includes an extraction film bag and an extraction filler. The extraction film bag is made of polypropylene film, and the extraction filler is made of a porous MOF material with strong adsorption performance. A micro solid phase extraction probe based on MIL-101 metal-organic framework (MOF) is prepared by the following steps:

[0023] ① First, Cr(NO 3 ) 3 9H 2 O (400mg, 1mmol), terephthalic acid (166mg, 1mmol), hydrofluoric acid (1mmol) and deionized water (4.8mL, 265mmol) were mixed uniformly, and then the mixture was put into a polytetrafluoroethylene reactor, Put the reaction kettle into an oven and heat it to 220°C for 8 hours. After natural cooling, filter and collect, and prepare MIL-101 material for use;

[0024] ②Purify the synthesized M...

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PUM

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Abstract

The invention discloses a micro solid phase extraction probe made by an MIL-101 type metal organic framework (MOF) material and a preparation method of the probe. The probe comprises an extraction membrane bag and extraction packing. According to the membrane bag, the extraction packing is protected by adopting a hollow fiber membrane, macromolecules, particle impurities and the like can be effectively prevented from entering the membrane bag, micromolecular target compounds are adsorbed by the extraction packing, and trace organic solvents can be analyzed. The extraction packing is a MOF material MIL-101, has high specific surface area and relatively large particle size and has high adsorptive property on targets in water; the hollow fiber membrane is a polypropylene membrane, can prevent the macromolecules, particle impurities and the like and has high sensitivity, high matrix interference resistance, sample purification function and satisfactory recycling rate; moreover, the probe is simple to produce, convenient to operate and wide in substrate analysis range, can be repeatedly recycled and can be used for directly analyzing complex environmental samples.

Description

technical field [0001] The invention relates to the field of sample pretreatment technology and environmental sample analysis and detection, in particular to a micro-solid-phase extraction probe and its preparation method, which is characterized in that metal-organic framework materials (MOFs) synthesized by hydrothermal method are directly filled into the hollow space by using a syringe. Micro-solid-phase extraction (μ-SPE) probes were fabricated in fiber membranes. Background technique [0002] In the chemical analysis of real water samples, sample pretreatment is a very important step, and the pretreatment process directly affects the accuracy, precision and quantification limit of the analysis results. Among many pretreatment methods, solid phase extraction has developed rapidly and been widely used due to its advantages of simple application, flexible solvent selection, high recovery rate and stability. However, typical solid-phase extraction is time-consuming and labo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01D15/20G01N30/08
Inventor 鲁效庆邵洋魏淑贤朱青靳栋梁史晓凡陈相峰
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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