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Silver sol modified by silver ions, preparation method of silver sol and application of silver sol in quantitative detection of arsenic through surface enhanced Raman spectroscopy

A surface-enhanced Raman, silver ion technology, applied in nanotechnology for materials and surface science, Raman scattering, metal processing equipment, etc., can solve the poor repeatability of the SERS substrate activity of silver sol, and the quantitative analysis ability needs to be improved. , Unable to use rapid detection and other problems to achieve the effect of improving sensitivity and repeatability

Active Publication Date: 2022-04-12
SHANDONG UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the quantitative analysis capability of this method needs to be improved
At the same time, due to the poor repeatability of the SERS substrate activity of silver sol synthesized by different batches or different laboratories, this method cannot be used for rapid detection in the actual environment.

Method used

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  • Silver sol modified by silver ions, preparation method of silver sol and application of silver sol in quantitative detection of arsenic through surface enhanced Raman spectroscopy
  • Silver sol modified by silver ions, preparation method of silver sol and application of silver sol in quantitative detection of arsenic through surface enhanced Raman spectroscopy
  • Silver sol modified by silver ions, preparation method of silver sol and application of silver sol in quantitative detection of arsenic through surface enhanced Raman spectroscopy

Examples

Experimental program
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Effect test

Embodiment 1

[0028] A silver sol modified with external silver ions (AgNP@Ag + ), the AgNP@Ag + With nano-silver sol as the core, silver ions are adsorbed on the surface of nano-silver sol, AgNP@Ag + The concentration of silver ions in the system is 1.1×10 -7 mol / L.

[0029] The AgNPs@Ag + It is prepared through the following steps: using silver nitrate as raw material, sodium citrate as reducing agent and protective agent, and preparing nano-silver sol with a diameter of about 40-60nm by chemical reduction method, the specific process is: 0.027g of silver nitrate powder and Add 150mL of ultrapure water into the round bottom flask, stir and heat to a slight boil, quickly inject 3mL of 1% sodium citrate solution with a syringe, continue to heat and boil for 30min, and observe that the solution turns gray-green, that is, the nano-silver is produced Sol. Then, mix 1mL nano-silver sol with 100μL concentration of 1.0×10 -2 mol / L NaBH 4 Mix the solution in an ice-water bath and place it i...

Embodiment 2 Embodiment 10

[0032] In order to verify the AgNP@Ag in Example 1 + The silver ion concentration in the system is 1.1×10 -7 mol / L, the AgNPs@Ag + When analyzing As (Ⅲ), better effect is arranged, and the present application has also specially carried out embodiment two to ten, and wherein, in embodiment two to ten, only the adding situation of silver nitrate in bare silver sol is different from embodiment one, implements Examples 2 to 10 prepared AgNP@Ag with different silver ion concentrations by adjusting the concentration of silver nitrate solution added to the "bare silver sol". + system, and then the AgNP@Ag with different silver ion concentrations prepared above + The system was used as the SERS substrate, and the concentration of As(Ⅲ) was 1×10 -6 mol / L of the solution to be tested was analyzed by SERS, and it was found that the system contained 1.1×10 -7 mol / L AgNP@Ag of silver ions + The system has the best response to As(Ⅲ), as shown in Fig. 3(a). Among them, in Examples 2 to...

Embodiment 11

[0036] A silver sol modified with external silver ions (AgNP@Ag + ), the AgNP@Ag + With nano-silver sol as the core, silver ions are adsorbed on the surface of nano-silver sol, AgNP@Ag + The silver ion concentration in the system is 4.3×10 -4 mol / L.

[0037] The AgNPs@Ag + It is prepared through the following steps: using silver nitrate as raw material, sodium citrate as reducing agent and protective agent, and preparing nano-silver sol with a diameter of about 40-60nm by chemical reduction method, the specific process is as follows: 0.027g silver nitrate powder and Add 150mL of ultrapure water into the round bottom flask, stir and heat to slight boiling. Quickly inject 3 mL of 1% sodium citrate solution with a syringe, continue heating and boiling for 30 min, and when the solution turns gray-green, the nano-silver sol is obtained. Then, mix 1mL nano-silver sol with 100μL concentration of 1.0×10 -2 mol / L NaBH 4 Mix the solution in an ice-water bath and place it in the i...

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Abstract

The invention discloses silver ion modified silver sol (AgNP (at) Ag < + >), a preparation method thereof and application of the silver sol in surface enhanced Raman spectroscopy quantitative detection of arsenic. According to the silver ion modified silver sol, nano-silver sol serves as an inner core, silver ions are adsorbed on the surface of the inner core, and the concentration of the silver ions of an AgNP (at) Ag < + > system is controlled by controlling the concentration of added silver nitrate. When the concentration of silver ions in the AgNP (at) Ag < + > system is 1.1 * 10 <-7 >-4.3 * 10 <-4 > mol / L, the sensitivity of analyzing arsenite (As (III)) and arsenate (As (V)) by taking AgNP (at) Ag < + > as the SERS substrate is higher than that of a nano-silver sol substrate, and meanwhile, the repeatability of SERS response of AgNP (at) Ag < + > synthesized in different batches to As (V) and As (III) is remarkably enhanced, so that a basis is provided for further developing the method into a rapid detection method.

Description

technical field [0001] The invention relates to the fields of surface-enhanced Raman spectroscopy technology and environmental analysis, in particular to a silver ion-modified silver sol, a preparation method thereof, and an application in the quantitative detection of arsenic by surface-enhanced Raman spectroscopy. Background technique [0002] At present, about 140 million people in the world drink groundwater containing arsenic (Science, 2013, 341, 852-853). The toxicity of arsenic-containing substances depends on its residual concentration and the chemical form of arsenic (Science, 2003, 300, 939-943). In general, arsenous acid is more toxic than arsenic acid. Therefore, the rapid and quantitative detection of arsenite (As(Ⅲ)) and arsenate (As(V)) in water is a prerequisite for risk assessment of arsenic pollution and has attracted increasing attention (Food Control, 2021, 121 ,107588.). The analysis methods of As(Ⅲ) and As(V) mainly include high performance liquid ch...

Claims

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Application Information

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IPC IPC(8): B22F1/0545B22F1/145B22F9/24B82Y30/00B82Y40/00B82Y15/00G01N21/65
Inventor 陈静吕晓晨苏明明王楠来永超程世博
Owner SHANDONG UNIV