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Method for detecting content of heavy water by utilizing aggregation-induced emission molecules

A technology of aggregation-induced luminescence and molecules, which is applied in the field of fluorescent chemical sensors, can solve the problems of excited state dynamics changes, affecting fluorescence lifetime, etc., and achieve the effects of accurate heavy water content, rapid identification, and excellent anti-interference ability

Active Publication Date: 2021-06-25
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Based on the above theoretical background, if the ordinary hydrogen atoms in the ESIPT process are replaced with deuterium hydrogen, it will inevitably cause changes in the dynamics of the excited state, which in turn will affect the fluorescence lifetime of such molecules

Method used

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  • Method for detecting content of heavy water by utilizing aggregation-induced emission molecules
  • Method for detecting content of heavy water by utilizing aggregation-induced emission molecules
  • Method for detecting content of heavy water by utilizing aggregation-induced emission molecules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation of embodiment 1 AIE molecule-1H

[0027] Put 1mmol of aniline derivative (2-aminobenzenethiol) and 1mmol of salicylaldehyde in a 25mL round bottom flask, then add 5mL of absolute ethanol; stir and heat to reflux to 80°C for 1 hour. After the reaction was completed, it was cooled to room temperature, and a precipitate was deposited. Filter and wash the filter cake with 10 mL of ice (0°C) absolute ethanol three times, put the filter cake into a vacuum drying oven, and dry the filter cake under reduced pressure at 60°C to obtain 0.8 mmol of 1H.

[0028] Add the obtained product 1H into a round bottom flask containing 10 mL of tetrahydrofuran, add 5 drops of heavy water, heat and stir until solids are precipitated, and then repeat the replacement process twice. After three replacements, filter with suction, wash the filter cake three times with 15 mL ice-free ethanol, and dry under reduced pressure to obtain 1D.

[0029] The structural formulas and reactio...

Embodiment 2

[0031] Embodiment 2 Preparation of AIE molecule-2H

[0032] Put 1 mmol of aniline derivative (N-N-dimethyl-p-phenylenediamine) and 1 mmol of salicylaldehyde in a 25 mL round bottom flask, and then add 5 mL of absolute ethanol. Stir and heat to reflux to 80°C, and the reaction time is 1 hour. After the reaction was completed, it was cooled to room temperature, and a precipitate was deposited. Filter and wash the filter cake three times with 10 mL of ice (0° C.) absolute ethanol, put the filter cake in a vacuum oven, and dry under reduced pressure at 60° C. to obtain 0.8 mmol 2H of the product.

[0033] Add the obtained product 2H into a round bottom flask containing 10 mL of tetrahydrofuran, add 5 drops of heavy water, heat and stir until solids are precipitated, and then repeat the replacement process twice. After three replacements, filter with suction, wash the filter cake three times with 15 mL of ice-free ethanol, and dry under reduced pressure to obtain 2D.

[0034] Th...

Embodiment 3

[0036] Embodiment 3 Preparation of AIE molecule-3H

[0037] Put 1mmol of hydrazine hydrate and 2mmol of salicylaldehyde in a 25mL round bottom flask, and then add 5mL of absolute ethanol. Stir and heat to 80°C for a reaction time of 30 minutes. After the reaction was completed, it was cooled to room temperature, and a precipitate was deposited. Filter, and wash the filter cake three times with 10 mL of cold (0° C.) absolute ethanol, put the filter cake in a vacuum oven, and dry under reduced pressure at 60° C. to obtain 0.8 mmol 3H of the product.

[0038] Add the obtained product 3H into a round-bottomed flask containing 10 mL of tetrahydrofuran solution, add 5 drops of heavy water, heat and stir until solids are precipitated, and then repeat the replacement process twice. After three replacements, filter with suction, wash the filter cake three times with 15 mL ice-free ethanol, and dry under reduced pressure to obtain 3D.

[0039] The structural formulas and reaction pri...

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Abstract

The invention provides a method for detecting the content of heavy water by utilizing aggregation-induced emission molecules, which comprises the following steps: preparing a compound with intramolecular hydrogen bonds by utilizing a condensation reaction of an amino compound and a carbonyl compound, and preparing a stock solution with the concentration of 10<-3> mol / L from the compound which is the aggregation-induced emission molecules with excited-state intramolecular proton transfer property; and respectively adding the stock solution into D2O / H2O mixed standard water samples with different heavy water contents and a water sample to be detected, determining the fluorescence lifetime by using a transient fluorescence spectrometer to obtain a linear relationship between the fluorescence lifetime and the heavy water content, and calculating the heavy water content of the water sample to be detected. The invention provides a novel heavy water detection technology which overcomes many defects in the traditional D2O detection means. According to the technology, after active hydrogen in AIE molecules with excited-state intramolecular proton transfer property is substituted by deuterium hydrogen, the obvious change of fluorescence lifetime is used as a signal for heavy water detection and is used for distinguishing D2O and H2O signals.

Description

technical field [0001] The invention relates to a method for detecting heavy water content by using aggregation-induced luminescent molecules, belonging to the field of fluorescent chemical sensors. Background technique [0002] As regular water (H 2 Isotopically labeled version of O), heavy water (D 2 O) plays an important role in chemical analysis, medicine and the nuclear industry. However, due to highly similar structures and chemical properties, distinguishing D 2 O and H 2 O very difficult. Currently, conventional instrumental analysis methods such as atomic absorption spectroscopy (AAS), nuclear magnetic resonance (NMR) spectroscopy, and infrared laser spectroscopy are commonly used to differentiate the two water variants. However, most of the currently used detection methods usually have disadvantages including time-consuming detection, complex instruments and high cost, and these methods inevitably require complicated sample pretreatment procedures, which limit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
CPCG01N21/643Y02A20/20
Inventor 李恺彭秋晨李媛媛
Owner ZHENGZHOU UNIV
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