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Method for preparing xerogel fixed ligand polymer micro-extraction membrane device

A technology of coordination polymers and extraction membranes, applied in the preparation of test samples, ion exchange treatment devices, chemical/physical processes, etc., can solve the problems of poor experimental accuracy and reproducibility, adsorbent leakage, and material bag rupture and other problems, to achieve the effect of shortening the experiment time, manpower and material resources, less cost, and good thermal stability

Inactive Publication Date: 2015-03-25
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the experimental operation of adsorption / desorption, the steps of ultrasonic or magnetic stirring will cause the complete heat-sealed bag to rupture and fail, resulting in the leakage of the adsorbent, making the accuracy and reproducibility of the experiment poor; At the same time, when preparing the μ-SPE device, there are also certain technical difficulties in heat-sealing the hollow fiber membrane, which requires repeated and repeated experiments.

Method used

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  • Method for preparing xerogel fixed ligand polymer micro-extraction membrane device
  • Method for preparing xerogel fixed ligand polymer micro-extraction membrane device
  • Method for preparing xerogel fixed ligand polymer micro-extraction membrane device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: immobilization of polymer Co 3 (C 9 h 6 o 6 )·12H 2 0 xerogel microextraction membrane

[0023] A. Weigh 2.0 mg of polymer Co 3 (C 9 h 6 o 6 )·12H 2Add 0 material into a 1.5ml microcentrifuge tube, then add 100μl of N,N-dimethylformamide (DMF) solution and 50μl of ultrapure water to it, and sonicate for 30min;

[0024] B. After the sonication is over, take out the centrifuge tube and add 350 μl of tetraethoxysilane (TEOS) and 50 μl of hydroxyl-terminated polydimethylsiloxane (PDMS) to the mixed solution, and continue to sonicate for 120 minutes;

[0025] C. After step B, take out the centrifuge tube again, shake it up and down to make it evenly mixed; open the cap of the tube, add 70 μl of trifluoroacetic acid (TFA) catalyst into it, cover the cap and shake it up and down, let it react for 5 minutes;

[0026] D. After 5 minutes, use a sampling tube to absorb the sol solution, and place it on the cap of a 10ml centrifuge tube as a substrate. Open th...

Embodiment 2

[0029] Embodiment 2: Immobilization of polymer Zn 3 (C 8 h 8 o 4 ) xerogel microextraction membrane

[0030] A. Weigh 2.0mg of polymer Zn 3 (C 8 h 8 o 4 ) material into a 1.5ml microcentrifuge tube, then add 100μl of N,N-dimethylformamide (DMF) solution and 50μl of ultrapure water to it, and sonicate for 30min;

[0031] B. After the sonication is over, take out the centrifuge tube and add 350 μl of tetraethoxysilane (TEOS) and 50 μl of hydroxyl-terminated polydimethylsiloxane (PDMS) to the mixed solution, and continue to sonicate for 120 minutes;

[0032] C. After step B, take out the centrifuge tube again, shake it up and down to make it evenly mixed; open the cap of the tube, add 70 μl of trifluoroacetic acid (TFA) catalyst into it, cover the cap and shake it up and down, let it react for 5 minutes;

[0033] D. After 5 minutes, use a sampling tube to absorb the sol solution, and place it on the cap of a 10ml centrifuge tube as a substrate. Open the fume hood to age ...

Embodiment 3

[0036] Embodiment 3: fixed polymer Cu(C 9 h 6 o 6 )(C 3 h 7 NO) xerogel microextraction membrane

[0037] A. Weigh 2.0 mg of polymer Cu(C 9 h 6 o 6 )(C 3 h 7 NO) material was added to a 1.5ml microcentrifuge tube, then 100μl of N,N-dimethylformamide (DMF) solution and 50μl of ultrapure water were added to it, and ultrasonicated for 30min;

[0038] B. After the sonication is over, take out the centrifuge tube and add 350 μl of tetraethoxysilane (TEOS) and 50 μl of hydroxyl-terminated polydimethylsiloxane (PDMS) to the mixed solution, and continue to sonicate for 120 minutes;

[0039] C. After step B, take out the centrifuge tube again, shake it up and down to make it evenly mixed; open the cap of the tube, add 70 μl of trifluoroacetic acid (TFA) catalyst into it, cover the cap and shake it up and down, let it react for 5 minutes;

[0040] D. After 5 minutes, use a sampling tube to absorb the sol solution, and place it on the cap of a 10ml centrifuge tube as a substrat...

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Abstract

The invention provides a method for preparing a xerogel fixed ligand polymer micro-extraction membrane device. The preparation method comprises the following steps of: directly dispersing a fixed ligand polymer adsorbing agent material into a sol solution by a sol-gel method to prepare silicic acid xerogel of the fixed ligand polymer absorbing material; and further selectively extracting a durable organic pollutant poly-brominated diphenyl ether in the water body and the soil by using the silicic acid xerogel. The preparation method has the characteristics of simple and rapid method, low cost, high stability and heat stability on intensity of the membrane and high sensitivity, rapidness and enrichment efficiency in experiment.

Description

technical field [0001] The invention relates to a preparation method of a micro-solid-phase extraction membrane, in particular to a preparation method of a xerogel immobilized coordination polymer micro-extraction membrane device. Background technique [0002] Micro-solid-phase extraction (μ-SPE) is a new sample pretreatment technology first proposed by Lee's research group at the National University of Singapore in 2006. Lee et al. folded a 0.2 μm pore diameter polypropylene membrane into a 2 cm × 1.5 cm μ-SPE bag, filled it with 6 mg of multi-walled carbon nanotubes, and then heat-sealed the bag to make a μ-SPE device. Supplemented with a magnetic stirring device, it is used for the pre-concentration and analysis of organophosphorus pesticides in sediments, and has been carried out with hollow fiber membrane solid-phase microextraction (HFM-SPME) and headspace solid-phase microextraction (HS-SPME). Compared with experimental studies, lower detection limit and better repro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/08G01N1/40
Inventor 周友亚王林谢亚勃张超艳唐艳冬周惠艳颜增光白利平李发生
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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