CN1657915A - Method for preparing silver sol for investigating raman spectrum - Google Patents
Method for preparing silver sol for investigating raman spectrum Download PDFInfo
- Publication number
- CN1657915A CN1657915A CN200510037832.1A CN200510037832A CN1657915A CN 1657915 A CN1657915 A CN 1657915A CN 200510037832 A CN200510037832 A CN 200510037832A CN 1657915 A CN1657915 A CN 1657915A
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- CN
- China
- Prior art keywords
- raman spectrum
- silver
- sol
- silver sol
- raman
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 26
- 239000004332 silver Substances 0.000 title claims abstract description 26
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000009835 boiling Methods 0.000 claims description 6
- 150000003378 silver Chemical class 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 10
- 238000001069 Raman spectroscopy Methods 0.000 description 10
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 238000007788 roughening Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- BPRHUIZQVSMCRT-VEUZHWNKSA-N rosuvastatin Chemical compound CC(C)C1=NC(N(C)S(C)(=O)=O)=NC(C=2C=CC(F)=CC=2)=C1\C=C\[C@@H](O)C[C@@H](O)CC(O)=O BPRHUIZQVSMCRT-VEUZHWNKSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a production technique of a silver collosol for measuring the Raman spectrum. The silver collosol produced in the technique maintains for long period, and has a stable quality which considerably enhances the Raman spectrum and effectively eliminates the fluorescence obtaining clear and stable Raman spectrum figure fast. It is effective especially on biological molecular Raman spectrum measure.
Description
Affiliated technical field
The present invention relates to a kind of method for preparing silver sol for investigating raman spectrum, the silver sol for preparing can long preservation, and the effect of significant Surface enhanced raman spectroscopy is arranged, and is remarkable to the biomacromolecule effect especially.The invention belongs to the technical field of Raman spectrum test.
Background technology
At present, the laser raman technology is used to survey the molecular structure of protein and other more and more frequently, particularly their native conformations in the low concentration aqueous solution.But most protein fluorescence can occur under laser radiation, and fluorescence needs only appearance, and its intensity always surpasses Raman signal, so that be difficult to obtain clear and legible Raman collection of illustrative plates.For a long time, in order to eliminate fluorescence, mainly the method that all adopts high power laser that specimen is carried out the long period irradiation makes fluorescence intensity degenerate to acceptable level.1974, the Fleischmann of Britain (Fleischman) found that at first the Raman spectrum that the pyridine molecule obtains has had enhancing on the silver electrode surface with the electrochemical method roughening.But they think that this is because the roughening of electrode surface, long-pending the increasing of electrode real surface and the amount increase of the pyridine molecule of absorption is caused, and do not recognize the humidification of rough surface to the raman spectral signal of absorbing molecules.Until 1977, Fan Duoen (Van Duyne) and two seminar of Creston (Creighton) find independently of one another, and the Raman signal of each pyridine molecule that is adsorbed on coarse silver electrode surface is approximately stronger by 10 than the Raman signal of single pyridine molecule in the solution
6Doubly.They think that the enhancing of this unusual high Raman signal can not ascribe the increase of the pyridine molecular amounts of adsorbing behind the silver electrode surface roughening simply to, and certain physical influence must be arranged in action.
When the molecular adsorption with resonance Raman effect during silver, gold or the copper of roughening surperficial, its resonance raman signal also is enhanced, and this phenomenon is called as Surface enhanced raman spectroscopy (Surface Enhanced RamanScattering).When measuring the Raman spectrum of biomolecule; be subjected to the interference of fluorescence through regular meeting, but when biomolecule was adsorbed onto silver, gold or copper surperficial of roughening, its fluorescence can be by quencher; the Raman spectrum summit is enhanced, and is easy to obtain high-quality Surface enhanced raman spectroscopy spectrum.
Obtain high-quality Surface enhanced raman spectroscopy spectrum, except making with electrochemical method the surface of metal electrode roughening, the another kind of method that makes the metallic matrix roughening commonly used is to make metal-sol, particularly silver sol.The method for preparing metal-sol is a lot, but ultimate principle is similar, promptly the soluble metal salt solusion is obtained metal-sol through electronation.The silver sol of making can use immediately, also can deposit standby.But the silver sol quality instability of general preparation, the effect of cancellation fluorescence is bad when also being fashion.Especially the silver sol storage period of making, is not long, is generally several days, at most several weeks, has to when often using prepare again.
Summary of the invention
The present invention is exactly a kind of method for preparing silver sol for investigating raman spectrum to the deficiency proposition of existing method, the silver sol of this method preparation can keep for a long time, steady quality, the effect that significant Surface enhanced raman spectroscopy is arranged, quench fluorescence obtains steady and audible Raman spectrogram rapidly effectively.Remarkable to test organisms molecule Raman spectrum effect especially.
The technical solution adopted for the present invention to solve the technical problems is: the silver nitrate of 90mg is dissolved in the 500ml deionized water, be heated to boiling, be that 1% trisodium citrate dropwise adds then with 10mg concentration, and vigorous stirring, drip the back and continue to keep boiling more than at least 2 hours.After treating this silver sol natural cooling, put in the centrifuge tube, use the centrifugal layering of hydro-extractor again, the colloidal sol that relatively clarify on the upper strata is removed, lucifuge sealing is at room temperature deposited then.This silver sol energy long-term storage after handling like this, for up to one to two year.And stable in properties is constant, as required this silver sol and deionized water are made into debita spissitudo during use, mix with all kinds of samples such as the biomolecule solution tested then, fluorescence can obtain steady and audible Surface enhanced raman spectroscopy spectrum then substantially by quencher generally speaking.
Description of drawings
Fig. 1 is the laser raman spectrum of 5%DNA solution.
Fig. 2 is a 5%DNA solution and prepare the mixed Surface enhanced raman spectroscopy spectrum of silver sol by this method.
Embodiment
The silver nitrate of 90mg being dissolved in the 500ml deionized water, being heated to boiling, is that 1% trisodium citrate dropwise adds then with 10mg concentration, and vigorous stirring, drips the back and continues to keep boiling more than at least 2 hours.After treating this silver sol natural cooling, put in the centrifuge tube, use the centrifugal layering of hydro-extractor again, the colloidal sol that relatively clarify on the upper strata is removed, lucifuge sealing is at room temperature deposited then.
After 15 months, take out this silver sol of 0.5ml, add the 0.5ml deionized water, mix with 5%DNA solution then, test obtains the Surface enhanced raman spectroscopy spectrum signal.Fig. 1 is the laser raman spectrum of 5%DNA solution.Fig. 2 is a 5%DNA solution and prepare the mixed Surface enhanced raman spectroscopy spectrum of silver sol by this method.We can know that the raman spectra seen on Fig. 2 will find that as calculated they have strengthened several times respectively to hundred times far above raman spectra corresponding among Fig. 1.
Claims (1)
1. method for preparing silver sol for investigating raman spectrum, the silver nitrate of 90mg is dissolved in the 500ml deionized water, being heated to boiling, is that 1% trisodium citrate dropwise adds then with 10mg concentration, and vigorous stirring, it is characterized in that dripping the back continues to keep boiling more than at least 2 hours, after treating this silver sol natural cooling, put in the centrifuge tube, use the centrifugal layering of hydro-extractor again, the colloidal sol that relatively clarify on the upper strata is removed, and lucifuge sealing is at room temperature deposited then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100378321A CN100362339C (en) | 2005-02-25 | 2005-02-25 | Method for preparing silver sol for investigating raman spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100378321A CN100362339C (en) | 2005-02-25 | 2005-02-25 | Method for preparing silver sol for investigating raman spectrum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1657915A true CN1657915A (en) | 2005-08-24 |
| CN100362339C CN100362339C (en) | 2008-01-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100378321A Expired - Fee Related CN100362339C (en) | 2005-02-25 | 2005-02-25 | Method for preparing silver sol for investigating raman spectrum |
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| Country | Link |
|---|---|
| CN (1) | CN100362339C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101529229B (en) * | 2006-07-25 | 2011-10-05 | 惠普开发有限公司 | Controllable surface enhanced raman spectroscopy |
| CN102901722A (en) * | 2012-09-29 | 2013-01-30 | 浙江理工大学 | Method for rapidly detecting thiabendazole residue in liquid beverage |
| CN108548805A (en) * | 2018-03-05 | 2018-09-18 | 华南理工大学 | The method that nano silver colloidal sol quenching fluorescence is used in Raman spectrum |
| CN113640275A (en) * | 2021-08-02 | 2021-11-12 | 中国科学院南海海洋研究所 | Organic matter Raman detection method based on surface enhanced Raman spectrum |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4979985A (en) * | 1990-02-06 | 1990-12-25 | E. I. Du Pont De Nemours And Company | Process for making finely divided particles of silver metal |
| JP3429958B2 (en) * | 1996-08-28 | 2003-07-28 | 三井金属鉱業株式会社 | Method for producing silver colloid liquid |
| CN1261268C (en) * | 2004-06-08 | 2006-06-28 | 刘杰 | Nanometer silver sol and preparing method thereof |
-
2005
- 2005-02-25 CN CNB2005100378321A patent/CN100362339C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101529229B (en) * | 2006-07-25 | 2011-10-05 | 惠普开发有限公司 | Controllable surface enhanced raman spectroscopy |
| CN102901722A (en) * | 2012-09-29 | 2013-01-30 | 浙江理工大学 | Method for rapidly detecting thiabendazole residue in liquid beverage |
| CN108548805A (en) * | 2018-03-05 | 2018-09-18 | 华南理工大学 | The method that nano silver colloidal sol quenching fluorescence is used in Raman spectrum |
| CN113640275A (en) * | 2021-08-02 | 2021-11-12 | 中国科学院南海海洋研究所 | Organic matter Raman detection method based on surface enhanced Raman spectrum |
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| Publication number | Publication date |
|---|---|
| CN100362339C (en) | 2008-01-16 |
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