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Mercury ion probe and its preparation method and use

A technology of mercury ions and probes, which is applied in the direction of analyzing materials through chemical reactions, organic chemistry, and material analysis through observation of the influence of chemical indicators. It can solve the problem of low detection concentration, limited development and practical application. , low sensitivity and other issues, to achieve the effect of easy purification, excellent selectivity and anti-interference ability, high sensitivity

Inactive Publication Date: 2015-08-12
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the sensitivity of this method is better in solution, due to the limitation of the reaction itself, its sensitivity in practical application as a test strip is often low, generally only 10 -4 ~10 -5 The minimum detection concentration of mol / L limits its further development and practical application

Method used

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  • Mercury ion probe and its preparation method and use
  • Mercury ion probe and its preparation method and use
  • Mercury ion probe and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The synthesis of compound TPE-S, synthetic route is as follows:

[0035]

[0036] (1) First, compound TPE-O was synthesized by Friedel-Crafts acylation reaction. The specific synthesis steps are as follows: SOCl 2 (1mL) was added to the nitrobenzene solution of p-nitrophenylacetic acid (0.181g, 1mmol), stirred overnight at 65°C, and the excess SOCl 2 Vacuum extraction with oil pump at room temperature; then under ice bath, add tetraphenylethylene (TPE) (0.332g, 1mmol) and AlCl to the above reaction solution 3 (0.133g, 1mmol), react at room temperature for 4 hours; after the reaction, extract the reaction solution with dichloromethane, combine the organic phases, and evaporate nitrobenzene under reduced pressure. The crude product was separated by silica gel column chromatography to obtain a light yellow solid product with a yield of 64%.

[0037] 1 H NMR (300MHz, CDCl 3)δ (ppm): 8.21 (d, J = 8.4, 2H, ArH), 7.75 (d, J = 8.1, 2H, ArH), 7.40 (d, J = 8.1, 2H, ArH), ...

Embodiment 2

[0041] Embodiment 2: Compound TPE-S is to the fluorescence detection of mercury ion in solution

[0042] The preparation concentration is 1×10 -1 mol / L of Hg(ClO 4 ) 2 ·3H 2 O, AgNO 3 ,Al(NO 3 ) 3 9H 2 O,Cr(NO 3 ) 3 9H 2 O,FeCl 3 ·6H 2 O,CoCl 2 ·6H 2 O,Ba(NO 3 ) 2 , Ca(NO 3 ) 2 4H 2 O,Pb(NO 3 ) 2 ,Ni(NO 3 ) 2 ·6H 2 O,Zn(NO 3 ) 2 ·6H 2 O,MnSO 4 2H 2 O,Cu(NO 3 ) 2 ·3H 2 O,Cd(NO 3 ) 2 4H 2 O,Mg(ClO 4 ) 2 ,Fe(SO 4 ) 2 ·7H 2 O,NaNO 3 ,KNO 3 Aqueous solution, diluted to the required concentration when performing the test.

[0043] CH of compound TPE-S prepared in preparation example 1 3 CN solution at a concentration of 1 × 10 -3 mol / L. Various metal cations (1×10 -1 mol / L,Hg 2+ 9μL, other metal ions 18μL) added to the CH of TPE-S 3 CN solution (60 μL), and then added deionized water to dilute to a total volume of 3 mL (volume fraction of water is 98%) to help form the aggregated state of the product. The changes in the fluorescence in...

Embodiment 3

[0045] Embodiment 3: The solution of compound TPE-S is to the fluorescence response of mercury ion in the presence of other metal ions

[0046] Various metal cations (9 μL) prepared in Example 2 were added to the CH of TPE-S 3 CN solution, then add mercury ions (9 μL), and then add deionized water to dilute to a total volume of 3 mL (the volume fraction of water is 98%) to help form the aggregated state of the product. Record the change of the fluorescence intensity of each reaction solution with a fluorometer, and study the fluorescence response to mercury ions in the presence of other metal ions. image 3 In, I 0 is the initial fluorescence intensity, and I is the fluorescence intensity of compound TPE-S after adding metal ions. Ordinate I / I 0 -1 represents the change of the fluorescence emission intensity of the solution after adding different metal ions. image 3 The middle black strips represent the changes in fluorescence intensity caused by adding other metal ions o...

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Abstract

The invention discloses a mercury ion probe and its preparation method and use. The mercury ion probe can be used as a fluorescent and colorimetric sensor of a mercury ion aqueous solution, can be prepared by simple processes, and has very good selectivity and sensitivity of mercury ion detection and very fast reaction time. A test paper strip prepared from the mercury ion probe has very high sensitivity of mercury ions, a mercury ion fluorescence response detection limit of 1*10<-6> mol / L and a mercury ion colorimetric response detection limit of 1*10<-7> mol / L (20ppb). In practical application, only by naked eyes, the test paper strip prepared from the mercury ion probe has mercury ion aqueous solution detection limit of 20ppb without other apparatuses. Through convenient and cheap preparation of the test paper strip, storage convenience and actual operation convenience, the mercury ion sensor can be developed into a practical application tool for on-site examination of mercury ion pollution.

Description

technical field [0001] The invention relates to a novel mercury ion probe and a preparation method thereof, in particular to the practical application performance of the probe: it can be used as a test strip for ultra-high sensitivity detection of mercury ions. Background technique [0002] Mercury and its various forms are extremely toxic to humans and the environment. Although governments and environmental protection agencies of various countries have established strict standards on mercury use and discharge, due to human activities and natural emissions, the increasingly serious mercury pollution has caused serious threats to humans and the environment. Therefore, it is more and more urgent to develop fast, convenient, economical and high-performance mercury ion detection methods. In recent years, due to people's unremitting efforts, fluorescence, colorimetric, electrochemical and many other types of mercury ion sensors have been developed and applied. Among these metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D339/06G01N21/78
CPCC07D339/06G01N21/78
Inventor 李振阮志军秦金贵
Owner WUHAN UNIV
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