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MIL-53 needle tube-type solid phase microextraction probe and preparation method thereof

A MIL-53, needle tube technology, applied in chemical instruments and methods, material separation, instruments, etc., can solve the problems of fragile SPME silica matrix probes, poor coating stability, short service life, etc., and achieve thermal stability Good resistance and chemical stability, solvent washing resistance, easy material effect

Inactive Publication Date: 2014-09-17
CHINA UNIV OF PETROLEUM (EAST CHINA)
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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a MIL-53 needle-tube solid-phase microextraction probe and its preparation method to solve the problem of the commercial SPME silica matrix probe being fragile, poor coating stability, easy to fall off, uneven surface, and long service life. short wait

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  • MIL-53 needle tube-type solid phase microextraction probe and preparation method thereof
  • MIL-53 needle tube-type solid phase microextraction probe and preparation method thereof
  • MIL-53 needle tube-type solid phase microextraction probe and preparation method thereof

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Embodiment Construction

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

[0022] The MIL-53 needle-tube solid-phase microextraction probe of the present invention includes a probe substrate and a coating material, and is characterized in that the substrate of the probe is made of tubular stainless steel, and the coating material is a porous metal organic framework material. A kind of solid-phase microextraction probe based on MIL-53 (Al) coating material is prepared by following steps:

[0023] ① Mix aluminum nitrate, terephthalic acid and deionized water evenly according to the molar ratio of 1:0.5:80, then put them into a 100ml polytetrafluoroethylene reactor and react at 220°C for 3 days. After cooling, filter and wash with distilled water four times, then reheat to 280 ° C for 1 hour to remove unreacted terephthalic acid, and prepare MIL-53 (Al) powder for later use;

[0024] ②Cut off 5 μl of gas-phase micro-sampling nee...

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Abstract

The invention discloses a MIL-53 needle tubing-type solid phase microextraction probe and a preparation method thereof. The MIL-53 needle tube-type solid phase microextraction probe comprises a stainless steel matrix and a coating material. The stainless steel matrix is made of a stainless steel material and is a tube-shaped structure. The coating material is a metal organic skeletal material MIL-53 (M) (wherein M represents Fe, Al or Cr). According to the preparation method, the coating material directly coheres to the surface of the stainless steel matrix by high temperature-resistant epoxy resin glue so that the MIL-53 needle tube-type solid phase microextraction probe is prepared. The MIL-53 needle tube-type solid phase microextraction probe has a simple structure, good heat stability and good chemical stability, is convenient for operation and carrying, can be used for determination of polycyclic aromatic hydrocarbons (PAHs) in an environmental complex sample and is prepared from easily available materials. The preparation method has simple processes and a low cost. The coating material has a pore structure, high extraction efficiency and analysis efficiency, good gluing firmness and solvent flushing resistance, can be used repeatedly and greatly reduces an analysis cost.

Description

technical field [0001] The invention relates to the field of sample pretreatment technology and environmental sample analysis and detection, in particular to a solid-phase microextraction probe and a preparation method thereof, which is characterized in that the metal organic framework material MIL-53 ( M) (M=Al;Fe;Cr) nanoparticles are directly glued to the surface of stainless steel substrates to prepare solid-phase microextraction (SPME) probes. Background technique [0002] Among many pretreatment techniques, solid phase microextraction (SPME) is a fast, sensitive and convenient novel and environment-friendly sample pretreatment for gas and liquid samples proposed and developed rapidly in the early 1990s. technology. Solid phase microextraction is a simple and solvent-free sample processing method that integrates sampling and sample pretreatment. It has the advantages of simple device, convenient operation, less time-consuming, small sample consumption, good reproducibi...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01D15/08G01N30/08
Inventor 鲁效庆邵洋朱青魏淑贤张明敏王伟丽陈相峰
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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