A method of gas-driven dispersion liquid-liquid microextraction
A dispersion liquid-liquid and gas-driven technology, applied in the field of sample pretreatment in analytical chemistry, can solve problems such as uneven shaking force, poor reproducibility of analysis results, solution leakage, etc., and achieve efficient extraction effect
Inactive Publication Date: 2016-01-27
MINNAN NORMAL UNIV
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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 2.3g sodium bicarbonate to 100mL BTEX standard solution or environmental water sample to prepare a water sample solution containing 2.3% (w / v) sodium bicarbonate; then accurately pipette 3mL of the above solution and place it in a 10mL centrifuge tube 300μL extractant ethyl acetate and 500μL dispersant methanol; quickly add 0.2-0.5g 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 5min, 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 extraction conditions (such as the type of...
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The invention discloses a gas-driven dispersed liquid-liquid micro-extraction method. The specific steps are: preparing a water sample into a sodium bicarbonate solution with a concentration of 2.0-5.0% (w / v); pipetting the treated water sample solution Place in a centrifuge test tube and add extractant and dispersant; quickly add 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; place until the bubbles disappear, centrifuge Place the test tube in a centrifuge and centrifuge until the extractant and the water sample are separated; take 1.00-2.00 μL of the extractant with a micro-injector, and inject the sample for determination. The present invention forms a layer of organic liquid film on the surface of the water sample by adding a small amount of extractant with a density lower than water to the water sample; a large amount of gas is generated instantly in the water sample through a chemical reaction; The extraction method is used to drive the extractant to fully and evenly disperse in the water sample. Thus, it effectively replaces the artificial shaking method to promote the dispersion of the extractant, and realizes the efficient extraction of the 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 new type of separation and enrichment technology with less solvent 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, liq...
Claims
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IPC IPC(8): B01D11/04C02F1/26G01N30/08
Inventor 张茂升
Owner MINNAN NORMAL UNIV