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Raman probe used for detection of mercury ions and preparation method thereof

A technology of Raman probes and mercury ions, applied in Raman scattering, material excitation analysis, etc., can solve the problems of insufficient mercury sensitivity, long detection time, complicated preparation methods of Raman probes, etc., and achieve Raman enhancement effect Good, short preparation time, rapid detection effect

Inactive Publication Date: 2013-11-20
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the prior art, surface-enhanced Raman spectroscopy is used to detect mercury in water bodies. The preparation method of the Raman probe is complicated, and the sensitivity to mercury detection is not high enough, and the detection time is relatively long.

Method used

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  • Raman probe used for detection of mercury ions and preparation method thereof
  • Raman probe used for detection of mercury ions and preparation method thereof
  • Raman probe used for detection of mercury ions and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of nano-silver dispersion:

[0032] Mix 0.001mol / L silver nitrate and 0.001mol / L sodium phytate at a volume ratio of 30:1; heat to boiling and keep the temperature at 90-100°C. Add a trisodium citrate solution with a mass concentration of 1% and a volume of 1 / 50 of the volume of the above-mentioned silver nitrate solution, and react for 3 hours at 90-100° C. to obtain a nano-silver dispersion (silver) protected by phytic acid micelles. The particle size of nanoparticles is <10nm);

[0033] (2) Preparation of gold nano-sol:

[0034] Add 10mL of nano-silver dispersion protected by phytic acid micelles prepared in step (1), add 15mL of secondary deionized water, heat to 50°C under stirring, add 0.002mol / L perchlorauric acid solution 5mL (the dropping time of perchlorauric acid solution is 1 minute), stir for 15 minutes, quickly drop 1.5mL of 0.002mol / L trisodium citrate solution (the dropping time of trisodium citrate solution is 2 minutes), continue The...

Embodiment 2

[0041] (1) The preparation of nano-silver dispersion is the same as in Example 1

[0042] (2) Preparation of gold nano-sol:

[0043] Add 10mL of nano-silver dispersion protected by phytic acid micelles prepared in step (1), add 20mL of secondary deionized water, heat to 45°C under stirring, add 0.002mol / L perchlorauric acid solution 7mL (dropping time of perchlorauric acid solution is 1 minute), stir for 17 minutes, quickly drop 2mL of 0.002mol / L trisodium citrate solution (dropping time of trisodium citrate solution is 2 minutes), continue stirring The nano-sol was obtained in 17 minutes.

[0044] (3) Take 0.1 mL of the gold nano-sol in step (2) as the substrate, add 0.1 mL of crystal violet with a concentration of 0.12 nmol / L and mix to prepare a Raman probe for mercury ion detection.

[0045] According to the method of embodiment 1, detect mercury ion with the obtained Raman probe, the result is the same as embodiment 1, and the detection limit of the obtained Raman probe...

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Abstract

The invention especially relates to a Raman probe using a gold nanosol as a substrate for detection of mercury ions and a preparation method thereof, which belongs to the technical field of Raman spectrum detection. The preparation method comprises the following steps: adding secondary deionized water into a nano-silver dispersion liquid with phytic acid micelle as a protective agent, carrying out stirring, heating to a temperature of 40 to 60 DEG C, adding a perchloroauric acid solution drop by drop, carrying out stirring for 10 to 20 min, then adding trisodium citrate drop by drop and carrying out stirring for 10 to 20 min and cooling so as to prepare the gold nanosol; and adding crystal violet into the prepared gold nanosol and carrying out uniform mixing. The preparation method for the Raman probe is simple and convenient and needs short preparation time. A gold nanoparticle in the Raman probe has good stability; and the Raman probe has the advantages of capacity of rapid detection of mercury, high sensitivity, good selectivity and a mercury ion detection limit of 0.5*10<-12> mol / L.

Description

technical field [0001] The invention belongs to the technical field of Raman spectrum detection, and in particular relates to a Raman probe for mercury ion detection based on gold nano sol and a preparation method thereof. Background technique [0002] Surface-enhanced Raman scattering is an unusual surface optical phenomenon that can amplify the Raman signal of absorbing molecules by a million-fold. In recent years, due to its high sensitivity, surface-enhanced Raman spectroscopy has been widely used in scientific and technical fields such as chemistry, biological science and its qualitative and quantitative analysis. A suitable substrate is the prerequisite for obtaining a good surface enhancement effect. Metal sols are widely used for their low cost, simple preparation, and good enhancement effect. [0003] Mercury is a heavy metal pollutant with strong biological toxicity in the environment. It is difficult to be excreted after entering the organism, which seriously thr...

Claims

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Application Information

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IPC IPC(8): G01N21/65
Inventor 杨海峰傅书悦
Owner SHANGHAI NORMAL UNIVERSITY
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