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A core-shell SERS probe, its preparation method and its application in the detection of trace arsenate ions

A core-shell and probe technology, applied in the field of drinking water safety detection, achieves the effects of improved stability, quick and controllable assembly, and reduced detection limit

Active Publication Date: 2018-09-04
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, no in situ growth of Fe with spherical Ag nanoparticles as nuclei 3 o 4 shell reports
Especially without precious metals yet @Fe 3 o 4 A report on the application of core-shell SERS probes in the detection of arsenate ions

Method used

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  • A core-shell SERS probe, its preparation method and its application in the detection of trace arsenate ions
  • A core-shell SERS probe, its preparation method and its application in the detection of trace arsenate ions
  • A core-shell SERS probe, its preparation method and its application in the detection of trace arsenate ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] a) Take 10mL of citrate-stabilized Ag nanoparticles (prepared with reference to the document J.Phys.Chem.C, 2009, 113, 657., wherein the quality of the Ag nanoparticles is 1.1mg, and the diameter of the Ag nanoparticles is 40nm) at a rotating speed After being centrifuged under the condition of 6000rpm for 8 minutes, the lower layer of concentrate (volume is 0.2mL);

[0027] b) Disperse the concentrated solution obtained in step a) into 3 mL of ethylene glycol solution, and add 1 g of sodium acetate and 0.02 g of ferric nitrate in sequence, and then stir vigorously to completely dissolve the reactants;

[0028] c) Put the mixture obtained in step b) in a reactor, and conduct a hydrothermal reaction at 200°C for 10 hours to obtain Ag@Fe 3 o 4 Colloidal solution of core-shell nanoparticles, the product quality is 3.3 mg.

[0029] Embodiment 1 performance test

[0030] a) 2mg Ag@Fe 3 o 4 The core-shell nanoparticles were dispersed in 2 mL of sodium arsenate aqueous so...

Embodiment 2

[0037] a) get 10mL of citrate-stabilized Ag nanoparticles (wherein the quality of Ag nanoparticles is 1.1mg, and the diameter of Ag nanoparticles is 60nm) after centrifugation under the condition of 5000rpm for 6 minutes, take the lower layer concentrated solution (volume is 0.2mL);

[0038] b) Disperse the concentrated solution obtained in step a) into 3 mL of ethylene glycol solution, and add 1 g of sodium acetate and 0.02 g of ferric nitrate in sequence, and then stir vigorously to completely dissolve the reactants;

[0039] c) Put the mixture obtained in step b) in a reactor, and conduct a hydrothermal reaction at 200°C for 10 hours to obtain Ag@Fe 3 o 4 Colloidal solution of core-shell nanoparticles, the product quality is 4.1 mg.

[0040] Ag@Fe 3 o 4 The core-shell SERS probe has a diameter of 80nm; the Ag core has a diameter of 60nm, Fe 3 o 4 The thickness of the shell layer is 10 nm.

[0041] attached Figure 5 yes get Ag@Fe 3 o 4 Core-shell SERS probe detect...

Embodiment 3

[0043] a) Get 10mL of citrate-stabilized Ag nanoparticles (wherein the quality of Ag nanoparticles is 1.1mg, and the diameter of Ag nanoparticles is 80nm) after centrifugation under the condition of 3000rpm for 5 minutes, take the lower layer concentrated solution (volume is 0.2mL);

[0044] b) Disperse the concentrated solution obtained in step a) into 3 mL of ethylene glycol solution, and add 1 g of sodium acetate and 0.02 g of ferric nitrate in sequence, and then stir vigorously to completely dissolve the reactants;

[0045] c) Put the mixture obtained in step b) in a reactor, and conduct a hydrothermal reaction at 200°C for 10 hours to obtain Ag@Fe 3 o 4 Colloidal solution of core-shell nanoparticles, the product quality is 4.6mg.

[0046] Ag@Fe 3 o 4 The core-shell SERS probe has a diameter of 100nm; the Ag core has a diameter of 80nm, Fe 3 o 4 The thickness of the shell layer is 10 nm.

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Abstract

The invention discloses a core-shell SERS (surface enhanced Raman spectroscopy) probe, a method for preparing the same and application of the core-shell SERS probe to trace arsenate ion detection, and belongs to the technical field of drinking water safety detection. The method includes the steps: concentrating 5-20 mL of citrate-stable precious metal nano-particle colloidal solution by the aid of centrifugal separation processes until the volume of the citrate-stable precious metal nano-particle colloidal solution is 1.5-3% of the original volume of the citrate-stable precious metal nano-particle colloidal solution so as to obtain concentrated solution; dispersing the obtained concentrated solution into 2-5 mL of organic alcohol solvents, sequentially adding 0.5-2 g of sodium acetate and 0.01-0.05 g of iron salt into the organic alcohol solvents, then strenuously stirring the sodium acetate, the iron salt, the concentrated solution and the organic alcohol solvents and completely dissolving reactants to obtain mixtures; carrying out hydrothermal reaction on the mixtures under the condition of the temperature of 180-250 DEG C for 8-18 h to obtain precious metal @Fe3O4 core-shell nano-particles. The core-shell SERS probe, the method and the application have the advantages that physical and chemical characteristics of precious metal cores and Fe3O4 shell layers can be effectively integrated on the core-shell SERS probe, and arsenate ions can be adsorbed by the Fe3O4 shell layers and accordingly can be effectively enriched on the surface of precious metal; the limit of detection of the arsenate ions of the core-shell SERS probe can be obviously lowered, and the core-shell SERS probe and the method can have important application prospects in the field of drinking water safety detection owing to magnetic separation and desorption recycling.

Description

technical field [0001] The invention belongs to the technical field of drinking water safety detection, and in particular relates to a core-shell SERS probe, a preparation method and its application in the detection of trace arsenate ions. The core-shell SERS probe can effectively integrate the SERS enhancement effect of the noble metal core and the Fe 3 o 4 The adsorption and magnetic response characteristics of the shell to arsenate ions show a high SERS detection activity for arsenate ions in water, and can be regenerated and reused through desorption activation. Background technique [0002] Arsenic is a toxic substance, a carcinogen / mutagenic factor, and a teratogenic effect on animals. Arsenic is usually included in copper, lead, tin, nickel, cobalt, zinc, gold and other ores in the form of sulfide, and enters the environment with tailings, waste water and waste gas during the mining and refining of these ores. Arsenic-containing fertilizers and pesticides used in a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65B82Y40/00B82Y30/00
CPCB82Y30/00B82Y40/00G01N21/65G01N21/658
Inventor 孙航尹升燕曾珊商殷兴金娥田丽梅
Owner JILIN UNIV
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