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Method for qualitatively detecting CU<2+> in solution directly by eye

A qualitative detection, solution technology, applied in the field of surface functionalized gold nanoparticles, eyes to detect Cu2+ in solution, to achieve the effect of obvious experimental phenomenon, cost saving and easy operation

Inactive Publication Date: 2011-05-11
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although Cu 2+ The detection limit of the concentration is as low as one part per billion, but these methods need to use sophisticated instruments to detect it, which has certain limitations in practical application

Method used

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  • Method for qualitatively detecting CU&lt;2+&gt; in solution directly by eye
  • Method for qualitatively detecting CU&lt;2+&gt; in solution directly by eye
  • Method for qualitatively detecting CU&lt;2+&gt; in solution directly by eye

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1, concrete steps are as follows:

[0034] 1.1: Synthesis of terminal alkyne-functionalized thiols

[0035] 0.5g of 11-alkylthiol carboxylic acid was dissolved in 20mL of anhydrous DMF, then 0.26mL of propyne bromide and 0.1g of anhydrous potassium carbonate were added, and the mixture was stirred at room temperature for 24 hours. The reaction solution was filtered, and DMF was removed by rotary evaporation to obtain 0.593g of crude product; the crude product was further dissolved with 30mL of dichloromethane, washed twice with 30mL of deionized water, and then separated, and the organic phase of dichloromethane was washed with anhydrous magnesium sulfate Drying, rotary evaporation to remove dichloromethane to obtain terminal alkyne functionalized mercaptan 0.475g, its yield was 81%, 1 H-NMR (400MHz, CDCl 3 ): δ2.46(s, 1H), δ2.68(t, J=7.2Hz, 2H), δ2.35(t, J=7.4Hz, 2H), δ1.63~1.28(m, 16H). MS, m / z: 256 (M+1).

[0036] 1.2: Synthesis of terminal azido-funct...

Embodiment 2

[0047] According to the steps of 1.1 and 1.2 in Example 1, a thiol functionalized with a terminal alkynyl group and a terminal azido group was synthesized using a 5-alkylthiol carboxylic acid. 0.05g of 5-alkylthiol carboxylic acid was dissolved in 5mL of anhydrous DMF, then 0.026mL of propyne bromide and 0.01g of anhydrous potassium carbonate were added, and the mixture was stirred at room temperature for 24 hours. The reaction solution was filtered, and DMF was removed by rotary evaporation to obtain the crude product of terminal alkyne functionalized thiol, which was then dissolved in dichloromethane, washed with water, dried over anhydrous magnesium sulfate, and rotary evaporated to obtain the purified terminal alkyne functionalized thiol ;

[0048] Add 0.1mL of chloroethanol and 0.2g of sodium azide to 10mL of DMF, and stir vigorously at 60°C for 48 hours under airtight conditions. After the reaction, wash with water, extract with dichloromethane, dry with anhydrous magnes...

Embodiment 3

[0050] According to the steps of 1.1 and 1.2 in Example 1, a thiol functionalized with a terminal alkynyl group and a terminal azido group was synthesized using a 9-alkylthiol carboxylic acid. 0.1 g of 9-alkylthiol carboxylic acid was dissolved in 10 mL of anhydrous DMF, then 0.1 mL of propyne bromide and 0.05 g of anhydrous potassium carbonate were added, and the mixture was stirred at room temperature for 24 h. The reaction solution was filtered, and DMF was removed by rotary evaporation. The crude product was dissolved in dichloromethane, washed with water, dried over anhydrous magnesium sulfate, and rotary evaporated to obtain terminal alkyne-functionalized mercaptans; 0.2mL chloroethanol and 0.4g sodium azide were added to 10mL In DMF, the reaction was vigorously stirred at 60°C for 48 hours under airtight conditions. After the reaction was completed, it was washed with water, extracted with dichloromethane, dried over anhydrous magnesium sulfate, and rotary evaporated to ...

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Abstract

The invention provides a method of directly using eyes to qualitatively detect Cu<2+> in a solution. The method comprises the following steps: terminal alkynyl functionalized mercaptan and terminal azido functionalized mercaptan are synthesized respectively; sodium citrate is used as a stabilizer to prepare gold nano-particles with the particle size of 14 nanometers; monomolecular layers of which the tail ends are provided with acetylene linkage and azide groups are self-assembled and formed on the surfaces of the gold nano-particles respectively by a ligand exchange method; the gold nano-particles subjected to two types of surface modification are mixed and added with blue vitriod and reducing agent; Cu(I) formed through reduction is taken as a catalyst, so as to allow the acetylene linkage to have cyclization reaction with the azide groups and cause the gold nano-particles to be accumulated; and the Cu<2+> in the solution is detected by observing the changes of the color and precipitation phenomenon of the gold nano-particles through naked eyes. The method can detect the existence of the Cu<2+> in a mixed solution with a plurality of metal cations. The method has characteristic of good function of detecting and identifying ions, obvious phenomenon and simple operation.

Description

technical field [0001] The invention relates to a method for detecting Cu2 in solution + The method, especially involving a surface-functionalized gold nanoparticle, undergoes a 1,3-dipolar cycloaddition reaction under the catalysis of Cu(I), resulting in the accumulation of gold nanoparticles to form a precipitate, while directly using the eyes to detect Cu in solution 2+ Methods. Background technique [0002] In recent years, metal chelating agents, organic fluorophores, chromogenic sensors, quantum dots and peptides have been gradually developed to detect Cu in solution. 2+ detection method, such as the US patent: US 3898042, and the Chinese patent with publication number CN 1477385. Although Cu 2+ The detection limit of the concentration is as low as one part per billion, but these methods all need to use sophisticated instruments to detect it, which has certain limitations in practical application. For example in US3898042, although Cu in solution can be continuous...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/02
Inventor 蒋兴宇周阳王仕兴
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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