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Preparation method for special-shaped gold nanocrystals and application on detection of tripolycyanamide by using surface enhanced Raman scattering

A surface-enhanced Raman and melamine technology, applied in the chemical industry, can solve the problems of slow analysis speed and poor method reproducibility, and achieve the effect of enhancing electromagnetic field, increasing biological affinity, and changing the degree of tightness of arrangement

Inactive Publication Date: 2014-06-25
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a method for preparing gold nanocrystals with a special shape and to use it in the detection of melamine by surface-enhanced Raman scattering in view of the shortcomings of the existing melamine detection methods, such as slow analysis speed and poor method reproducibility.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 9.9mL of 0.25mM chloroauric acid solution and 0.1mL of 0.025M trisodium citrate solution into a three-necked flask, quickly add 0.3mL of 0.01M freshly prepared iced sodium borohydride trisodium citrate solution, and stir for 1 min. Dissolve 0.911g of cetyltrimethylammonium bromide in 25mL of 0.125mM salicylic acid solution, add 4.5mL of the above mixed solution and 4.5mL of 0.5mM chloroauric acid solution to the three flasks A, B and C respectively and 0.05mL 0.08M ascorbic acid solution, add 0.1mL 0.0025M silver perchlorate solution to C, stir and react for 10s, and prepare three kinds of growth solutions A, B and C respectively. Add 1.0mL of gold seed solution to growth solution A, stir vigorously for 10s, take out 1.0mL from it and add it to growth solution B, stir for 10s, take out 1.0mL from it and add it to growth solution C, stir for 10s and place in a constant temperature water bath at 25°C React in middle temperature for 10h, centrifuge the prepared nano-go...

Embodiment 2

[0035] Add 9.9mL of 0.25mM chloroauric acid solution and 0.1mL of 0.025M trisodium citrate solution into a three-necked flask, quickly add 0.3mL of 0.01M freshly prepared trisodium citrate solution of tetrabutylpotassium borohydride in ice, and stir React for 5 minutes. Dissolve 0.911 g of cetyltrimethylammonium bromide in a mixed solution of 25 mL of 1 mM sodium dodecylbenzenesulfonate and hydrochloric acid of equal concentration. Add 4.5mL of the above mixed solution, 4.5mL of 0.5mM chloroauric acid solution and 0.05mL of 0.08M ascorbic acid solution to the three flasks of A, B and C respectively, add 0.1mL of 0.025M silver trifluoromethanesulfonate solution to C , stirred and reacted for 10 s, and prepared three kinds of growth solutions A, B, and C respectively. Add 1.0mL of gold seed solution to growth solution A, stir vigorously for 5s, take out 1.0mL from it and add it to growth solution B, stir for 5s, take out 1.0mL from it and add it to growth solution C, stir for 5...

Embodiment 3

[0037] Add 9.9mL of 0.25mM chloroauric acid solution and 0.1mL of 0.025M trisodium citrate solution into a three-necked flask, quickly add 0.3mL of 0.01M freshly prepared ice-cold potassium borohydride aqueous solution, and stir for 3 minutes. Dissolve 0.911 g of cetyltrimethylammonium bromide in 25 mL of 0.25 mM dodecylbenzenesulfonic acid solution. Add 4.5mL of the above mixed solution, 4.5mL of 0.5mM chloroauric acid solution and 0.05mL of 0.08M ascorbic acid solution to the three flasks of A, B and C respectively, add 0.1mL of 0.01M silver acetate solution to C, and stir for 10 seconds. Three growth solutions A, B, and C were prepared respectively. Add 1.0mL gold seed solution to growth solution A, stir vigorously for 15s, take out 1.0mL from it and add it to growth solution B, stir for 15s, take out 1.0mL from it and add it to growth solution C, stir for 15s and place in a constant temperature water bath at 35°C React in medium for 7 hours, centrifuge the prepared nano-g...

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Abstract

The invention belongs to the field of chemical engineering, and provides a preparation method for special-shaped gold nanocrystals and application on detection of tripolycyanamide by using surface enhanced Raman scattering. The preparation method comprises the following steps of preparing gold by using trisodium citrate as a stabilizer; using hexadecyl trimethyl ammonium bromide, a chloroauric acid, silver-bearing salt liquor and an ascorbic acid as growth-promoting media; preparing nanogold by using an organic acid as an additive; and performing resolution after centrifugal separation. The special-shaped gold nanocrystals are used for detecting Raman spectra of standard liquor or sample liquor of the tripolycyanamide. The nanogold is prepared by using a seed induction multi-step growing method, an additive containing benzene ring is added in the nanogold, and the use level of the hexadecyl trimethyl ammonium bromide is reduced, so that the cost is obviously reduced, and purification time and purification steps are reduced. The prepared nanogold has an angular structure, and can be used for detecting an enhancement substrate of trace tripolycayanamide by using surface enhanced Raman scattering; and compared with an HPLC (high performance liquid chromatography) method, the nanogold has the advantages that the analyzing time is short, the cost and the reproducibility are high, and the nanogold can be widely applied to quickly detecting the tripolycyanamide in dairy products.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of a gold nanocrystal with a special shape and its application to surface-enhanced Raman scattering detection of melamine. Background technique [0002] Gold nanoparticles exhibit special properties in electromagnetics, optics, and sensing, and have become one of the most commonly used enhancement substrates in the study of surface Raman enhancement behavior [K.Kneipp, A.S.Haka, H.Kneipp, K.Badizadegan and N.Yoshizawa.Appl.Spectrosc., 2002, 56, 150-154], its size, structure and shape are directly related to Raman activity, especially irregularly shaped and angular nanoparticles have a greater enhancement effect. At present, the preparation methods of nano gold mainly include direct reduction method [Jeong, G.H.; Lee, Y.W.; Kim, M.; Han, S.W.J. Colloid Interface Sci.2008, 329, 97-102.] and seed template method [Zou, X .; Ying, E.; Dong, S.Nanotech...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B82Y40/00G01N21/65
Inventor 李在均周晓燕
Owner JIANGNAN UNIV
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