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Surface-enhanced Raman scattering active nanofiber (SERS) and method of detecting nitrite content in water

A surface-enhanced Raman and nanofiber technology, applied in the field of analytical chemistry, can solve the problems of difficult sample pretreatment, easily polluted electrodes, inconvenient on-site detection, etc., to achieve accurate and reliable detection results, improve Raman spectrum intensity, and accurate sex high effect

Active Publication Date: 2019-05-21
CHINA AGRI UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

In actual work, most methods such as titration and spectrophotometry are susceptible to interference from other ions and suspended solids in aquaculture water, and are not suitable for continuous monitoring of water samples, requiring pretreatment and the use of toxic chemicals etc.; the ion selective electrode method, the electrode is easily polluted, needs to be replaced frequently, and has poor anti-interference
In summary, these methods have disadvantages such as difficult sample pretreatment, cumbersome process, long detection time, and inconvenient on-site detection. Therefore, finding a fast and effective online detection method for nitrite in aquaculture water has always been a worldwide problem. It is of great practical significance to study a new method for the detection of nitrite in aquaculture water

Method used

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  • Surface-enhanced Raman scattering active nanofiber (SERS) and method of detecting nitrite content in water
  • Surface-enhanced Raman scattering active nanofiber (SERS) and method of detecting nitrite content in water
  • Surface-enhanced Raman scattering active nanofiber (SERS) and method of detecting nitrite content in water

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1SERS active nanofiber and its preparation method

[0048] 1. Preparation of Hollow Fiber Materials

[0049] The liquid core optical fiber can only detect the liquid whose refractive index is higher than that of the optical fiber, and the refractive index of the liquid has a certain linear relationship with the liquid concentration. Since the silica fiber can only be used to measure the refractive index greater than 1.463 (refractive index of silica fiber), the hollow-core fiber in this embodiment chooses Teflon-AF material with low refractive index, strong gas permeability, and weak thermal conductivity. As a specific model, Teflon-AF 2400 (refractive index=1.29) optical fiber is selected, and its inner diameter is 250 μm.

[0050] The loss factor of the Teflon-AF 2400 that the present invention adopts is 5 * 10 -3 cm -1 , the optimal length of the liquid-core optical fiber is calculated to be about 2m. In order to ensure the rationality of the present i...

Embodiment 2

[0059] Example 2 Detection of nitrite content in water based on SERS and liquid core optical fiber technology

[0060] 1. Prepare six different concentrations of NO 2 - standard solution. Prepare a certain concentration of NO 2 - Aqueous solution, and diluted into six different concentrations of aqueous solutions of 1 μmol / L, 2 μmol / L, 4 μmol / L, 5 μmol / L, 6 μmol / L, 8 μmol / L, and stored in 6 centrifuge tubes, sealed for storage. Select the samples to be tested in the seawater aquaculture water body, use the national standard method spectrophotometry to detect the concentration of nitrite in the samples to be tested, and then save them.

[0061] 2. Preparation of SERS liquid core optical fiber. like figure 2 As shown, first select 4μmol / L NO 2 - After the diazo coupling reaction, put it into a beaker, put the prepared optical fiber into the beaker and immerse it in the solution, and then inject the solution into the prepared optical fiber with a syringe, so that the liq...

Embodiment 3

[0064] The impact of other interfering ions in embodiment 3 water body

[0065] In order to further prove the practicability of this method, this embodiment measures the influence of various common cations and anions on the experimental results, and the interference ion in this experiment is K + , Ca 2+ 、Na + , NO 3 - , Cl - , CO 3 2- 、CH 3 COO - 、PO 4 3- and SO 4 2- wait. In embodiment 2 step 1, choose concentration to be 1 μ mol / L NO 2 - standard solution, add 10 -4 mol / L of interfering ions, repeat steps 2 and 3 to obtain a Raman spectrum. Analyze the change of the Raman characteristic peak position and Raman spectrum intensity of the azo compound after adding the interfering ion, the experimental results show that 10 -4 mol / L K + , Ca 2+ 、Na + , NO 3 - , CO 3 2- 、CH 3 COO - and PO 4 3- Not to NaNO 2 The generated azo dye Raman characteristic peak intensity has a great influence; when Cl - Concentration≥10 -4 mol / L will affect the characterist...

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Abstract

The invention belongs to the field of analytical chemistry, in particular to a surface-enhanced Raman scattering active nanofiber (SERS) and a method of detecting a nitrite content in water. The method comprises the following steps: (1) SERS active modification of a hollow fiber is carried out; (2) intramolecular covalent assembly-based Raman probe molecular design is carried out; (3) the hollow fiber is injected to derivatives with different NO2<-> concentrations respectively; (4) a backward acceptance mode is adopted to receive Raman signals, the obtained Raman spectrum is subjected to spectrum analysis, and the Raman spectrum characteristic peak position of an azo dye and the intensity of the Raman peak are thus acquired; and (5) a partial least squares regression method is used to perform quantitative analysis on the acquired Raman spectrum information of the azo dye, and the NO2<-> concentration is indirectly detected. The method of detecting nitrite in an aquaculture water body provided in the invention is simple in sample preparation and fast in detection speed and realizes quantitative detection on the nitrite in the aquaculture water body.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a surface-enhanced Raman scattering-based active nanofiber and a method for detecting nitrite content in water. Background technique [0002] The content of nitrite is an important indicator to judge the degree of water pollution. Nitrite is a form of nitrogen in water and is an essential source of protein synthesis. Due to the existence of bait and excrement in aquaculture water, the content of nitrite will change greatly. Excessive nitrite will also cause trophicization of water, destroy the ecological balance of water, and directly produce toxicity to aquaculture water objects. It affects its growth and development, and even causes a large number of deaths, seriously affects the output of aquaculture industry, also has different degrees of harm to the human body, and causes serious economic losses. Therefore, the nitrite index is a necessary detection item in aquaculture ...

Claims

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Application Information

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IPC IPC(8): G01N21/65G02B6/02B82Y15/00C03C25/46C03C25/66
Inventor 李道亮李震王聪周新辉
Owner CHINA AGRI UNIV
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