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Surface-enhanced Raman scattering spectroscopy detection method based on capillary

A surface-enhanced Raman and detection method technology, applied in the field of analysis and detection, can solve the problems of complex SERS substrate preparation process and expensive equipment, and achieve the effects of shortening the detection time, real-time on-site detection, and avoiding detection steps

Inactive Publication Date: 2012-10-17
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003]Since the discovery of the SERS effect, SERS substrates with super-strong Raman enhancement effects and easy access have been a research hotspot. In recent decades, various SERS substrates with different morphological structures have been continuously prepared by researchers, although SERS substrates with a detection limit of 10-12-10-14 mol / L have been obtained by researchers reported, but the preparation process of these SERS substrates is complicated, the required equipment is expensive, and there is still a certain gap between these substrates and practicality, so they can only exist in the laboratory

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  • Surface-enhanced Raman scattering spectroscopy detection method based on capillary
  • Surface-enhanced Raman scattering spectroscopy detection method based on capillary
  • Surface-enhanced Raman scattering spectroscopy detection method based on capillary

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Embodiment 1

[0036] Decorate gold particles on the inner wall of the capillary and detect the Raman enhancement effect of the gold particle-modified capillary:

[0037] In this experiment, the inner wall of the capillary was pre-hydroxylated, and then the treated capillary was immersed in 3-aminopropyl-trimethoxysilane (APTMS), so that the inner wall was modified with a layer of amino groups. The coordination between gold particles uniformly decorates its inner wall. Under the action of hydroxylamine hydrochloride and chloroauric acid, the gold particles gradually grow up to a suitable particle size and particle spacing (see image 3 ).

[0038] The SERS substrate obtained by this method uses R6G (chemical name rhodamine 6G) as the probe molecule, and its detection limit can reach 1 mmol / l. From Figure 4 It can be seen that when ethanol solutions with different concentrations of R6G are detected with 514nm excitation light under the Raman spectrometer, as the concentration of R6G decre...

Embodiment 2

[0040] Silver particles are modified on the inner wall of the capillary and the Raman enhancement effect of the capillary modified by Ag particles is detected:

[0041]Under the action of boric acid and ammonium hexafluorotitanate, a thin layer of titanium dioxide can be pre-deposited on the inner wall of the capillary, and then the capillary is immersed in an aqueous solution of stannous chloride, so that a layer of divalent tin ions is adsorbed on the surface of titanium dioxide. In this way, when the capillary is immersed in the silver ammonia solution, a layer of silver particles can be uniformly grown on the inner wall in situ through the reduction of divalent tin ions, thereby having the SERS effect (see Figure 5 ).

[0042] R6G was also used as a probe molecule to study the Raman enhancement effect of Ag particle-modified capillaries, and the results showed that 10 -5 The R6G ethanol solution of mol / L can produce stronger SERS signal under the Raman spectrometer with ...

Embodiment 3

[0044] SERS characterization of other organic pollutants in ethanol solutions using gold particle-modified capillaries as the SERS substrate:

[0045] The capillary decorated with gold particles was used as the SERS substrate, and the 10 -5 mol / L other organic pollutants 4-ATP (p-mercaptoaniline) and Paraoxon (ethyl paraoxon) were simulated on-site detection. Figure 7 , Figure 8 They are the detection results of 4-ATP and Paraoxon respectively. The specific operation method is to directly inhale the ethanol solution of the analyte into the capillary, and use 514nm excitation light to detect under the Raman spectrometer. The results showed that the SERS signal was strong, indicating that the SERS active substrate had wide applicability.

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Abstract

The invention provides a surface-enhanced Raman scattering (SERS) spectroscopy detection method based on capillary. The invention belongs to the field of chemical analysis and detection. The detection method comprises the steps that: (1) gold / silver particles are modified on the inner wall of a capillary; (2) a solution of a substance requiring detection is absorbed with capillarity into the capillary modified by using the gold / silver particles; and (3) the capillary SERS substrate with the absorbed substance requiring detection is detected by using a Raman spectrometer. A traditional SERS substrate is constructed based on a plane. In actual operation, the solution of the target substance requiring detection needs to be dropped onto the substrate by using other tools; and the detection can be carried out by using the Raman spectrometer when the solution is dried. The process is complicated, and the tools are not convenient to carry. With the capillary-based SERS substrate, auxiliary operations of other tools are not needed. With the capillarity of the SERS substrate, the target substance requiring detection can be directly absorbed into the capillary SERS substrate. The amount of the needed sample is small, and the tools are convenient to carry. The method provided by the invention is suitable for actual field tests.

Description

technical field [0001] The invention relates to an analysis and detection method, in particular to a surface-enhanced Raman spectrum detection method. Background technique [0002] In 1928, the Indian scientist C.V. Raman experiment discovered that when light passes through a transparent medium and is scattered by molecules, the frequency changes. This phenomenon is called Raman scattering. Raman spectroscopy, like infrared spectroscopy, can reflect the information of molecular vibration-rotational energy levels, but the signal of Raman scattering is very weak, and its intensity is only one millionth of the incident light intensity. Not widely appreciated by the scientific community. Until 1974, Fleishmann et al. found that after roughening the surface of a smooth silver electrode, the high-quality Raman spectrum of a monolayer of pyridine molecules adsorbed on the surface of a silver electrode was obtained for the first time, and its intensity was comparable to that of pyr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
Inventor 杨良保陈晋刘洪林刘锦淮
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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