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Gas-driving dispersive liquid-liquid microextraction method

A dispersion liquid-liquid and gas-driven technology, which is applied in the field of sample pretreatment in analytical chemistry, can solve the problems of uneven shaking force, difficulty in automation, poor reproducibility of analysis results, etc., and achieve the effect of efficient extraction

Inactive Publication Date: 2014-01-22
MINNAN NORMAL UNIV
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  • Claims
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Problems solved by technology

[0003] (1) The reproducibility of the analysis results is poor due to the uneven shaking strength of each extraction;
[0004] (2) This method can only be carried out in a closed space and there is a hidden danger of solution leakage during violent shaking;
[0005] (3) It is not easy to realize automation

Method used

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Embodiment

[0033] Determination of benzene, toluene, ethylbenzene and xylene (BTEX) content in environmental water samples by gas-driven dispersion liquid-liquid microextraction method of the present invention

[0034] Add 2.3 g sodium bicarbonate to 100 mL BTEX standard solution or environmental water sample to prepare a water sample solution containing 2.3 % (w / v) sodium bicarbonate; then accurately pipette 3 mL of the above solution and place it in a 10 mL centrifuge tube Accurately add 300 μL of extractant ethyl acetate and 500 μL of dispersant methanol; quickly add 0.2-0.5 g of foaming agent ascorbic acid to the solution to generate a large number of bubbles instantly, and drive the extractant to fully disperse in the solution , let it stand for 5 min, and centrifuge at a speed of 300 rpm until the ethyl acetate and the water sample are separated; use a microsampler to take 1.00 μL of ethyl acetate and inject it into gas chromatography for analysis.

[0035] The optimization of extr...

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Abstract

The invention discloses a gas-driving dispersive liquid-liquid microextraction method. The method comprises specific steps of: preparing a water sample into a sodium bicarbonate solution having a concentration of 2.0-5.0% (w / v); pipetting the treated water sample into a centrifuge tube, and adding an extractant and a dispersant; adding rapidly a foaming agent ascorbic acid into the solution to produce a large amount of bubbles instantly and to drive the extractant to uniformly disperse in the solution; permitting the solution to stand until the bubbles disappear, putting the centrifuge tube in a centrifugal machine to be centrifuged until the extractant is separate with the water sample; and taking 1.00-2.00 [mu]L of the extractant by a microsyringe, and detecting. According to the method, an organic liquid film is formed on the surface of the water sample by adding the extractant having a slightly lighter density than water into the water sample, the large amount of bubbles are produced instantly by a chemical reaction in the water sample, and the extractant is drove to disperse uniformly in the water sample by a method of utilizing gas effervescence in the solution, thereby replacing effectively a manual shaking manner to promote extractant dispersion, and achieving efficient extraction of target molecules in the water sample.

Description

technical field [0001] The invention belongs to the technical field of sample pretreatment in analytical chemistry, specifically relates to liquid-liquid dispersion micro-extraction technology, and is suitable for the separation and enrichment of trace substances in environmental water samples. Background technique [0002] Dispersive liquid-liquid microextraction (DLLME) is a novel solvent-less separation and enrichment technique proposed by Assadi et al. in 2006. Under the action of the dispersant, the micro-extractant forms a large number of metastable micro-droplets in the sample solution through vigorous shaking. Because the amount of the extractant is small (micro-upgrade) and the contact area with the water phase is large, it can be rapidly extracted. When the extraction balance is reached and there is a high extraction efficiency and enrichment factor, the extraction agent is collected by centrifugation and analyzed and detected by gas chromatography, liquid chromato...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/04C02F1/26G01N30/08
Inventor 张茂升
Owner MINNAN NORMAL UNIV
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