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Electrochemical preparation method of silver wire sensing electrode

A sensing electrode and electrochemical technology, which is applied in the field of electroanalysis and detection, can solve the problems of poor stability and reproducibility, poor electrochemical activity, cumbersome preparation process of nano-powder state particles, etc., and achieve good binding force and high activity. Effect

Active Publication Date: 2020-06-05
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The electrochemical sensor constructed by this kind of chemically modified electrode is a common method at present. Its disadvantages are the tedious preparation process of nano-powder particles, weak binding force after attachment, poor stability and reproducibility.
However, pure silver solid electrodes such as silver wire, silver sheet, and silver mesh cannot be directly used for electrochemical analysis and detection due to their poor electrochemical activity.

Method used

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  • Electrochemical preparation method of silver wire sensing electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The surface treatment method of high-purity silver wire with a diameter of 0.5 mm is as follows: immerse the silver wire in acetone, ultrasonically clean it for 5 minutes, wash it with water at 30 °C, and then immerse it in HCl:CH 3 CH 2 OH:H 2 Etch in a mixed solution of O = 2:1:1 (mass ratio) for 60 seconds, control the temperature at 30°C, take it out, wash it with running water, and then wash it with warm water at 60°C, and use a polishing solution at 60°C for chemical polishing. Polishing 1 minute, described polishing liquid is Cu(NO 3 ) 2 :urea:HNO 3 :H 2 o 2 :H 2 O = a mixture of 1:1:2:2:4 (mass ratio), and finally wash the polished silver wire with running water to obtain a surface-treated silver wire.

[0023] The surface-treated silver wire was used as the working electrode, the platinum wire (0.5 mm in diameter) was used as the auxiliary electrode, and Ag / AgCl was used as the reference electrode, and placed in a 10 mL electrolytic cell with a stirring ...

Embodiment 2

[0026] Ten sets of high-purity silver wire electrode surface treatment methods are according to the method of embodiment 1, after degreasing-water washing-etching-hot water washing-polishing-water washing, the diameter of each set of silver wire electrodes is 0.5 mm, and the opposite electrode is platinum wire ( 0.5 mm in diameter), in a 10 mL electrolytic cell with a stirring device, add different template molecules and 0.2 M potassium nitrate solution. Table 1 lists the electrical analysis detection results of activated silver wire sensing electrodes prepared from different template molecules in the activation solution.

[0027] No. 1 is that the template molecule in the activation solution is acetic acid, the concentration is 0.5 M, and the voltammetry scanning is activated for 10 weeks. After the completion, a silver-white porous nano-silver membrane electrode is obtained. The electrode was taken out, washed with running water, and stored in absolute ethanol solution. Usi...

Embodiment 3

[0040] Polish the electrode serial number 4 that has completed electroanalysis detection in Example 2 with metallographic sandpaper, rinse it with deionized water, and perform fine surface treatment again. The method is as follows: immerse the silver wire of serial number 10 in acetone, and ultrasonically clean it for 5 After 30 minutes, wash with water at 30°C, and then immerse in HCl:CH 3 CH 2 OH:H 2 Etch in a mixed solution of O = 2:1:1 (mass ratio) for 60 seconds, control the temperature at 30°C, take it out, wash it with running water, and then wash it with warm water at 60°C, and use a polishing solution at 60°C for chemical polishing. Polishing for 1 minute, the polishing liquid is Cu(NO 3 ) 2 :urea:HNO 3 :H 2 o 2 :H 2 O = a mixture of 1:1:2:2:4 (mass ratio), and finally wash the polished silver wire with running water to obtain a surface-treated silver wire.

[0041] Put the surface-treated No. 4 silver wire as the working electrode, platinum wire (0.5mm in dia...

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Abstract

The invention discloses an electrochemical preparation method of a silver wire sensing electrode. The electrochemical preparation method comprises the following steps: 1) setting reaction conditions:taking template molecule concentration of 0.1 M-2. 0M and potassium nitrate concentration of 0.02 M-0. 2M as supporting electrolytes; 2) setting preparation conditions: taking a silver wire as a working electrode, taking a platinum wire as a counter electrode, and taking Ag / AgCl as a reference electrode; and 3) silver wire activation: performing cyclic voltammetry scanning for 1-30 weeks at the temperature of 10-45 DEG C within the range from -0.5 V to + 1.0 V while stirring, and performing oxidation-reduction etching on the surface of the tip of the silver wire working electrode, thereby obtaining the activated silver wire sensing electrode. The invention also provides a method for detecting chloroacetic acid by utilizing the active silver wire electrode obtained by the method through electro-analysis. Electrochemical cyclic voltammetry is mainly adopted and applied to electro-analysis and detection of corresponding template molecules. According to the method, direct activation of thesurface of the solid silver wire electrode is achieved, manufacturing is easy and convenient, the continuous electrocatalytic activity and stability of the electrode are improved, and the solid silver sensing electrode is long in service life, short in response time, high in sensitivity and low in detection limit as a sensing electrode.

Description

technical field [0001] The invention relates to an electrochemical preparation method of a silver wire sensing electrode and a method for using the silver wire sensing electrode obtained by the method for electrical analysis and detection. Background technique [0002] Electrochemical sensors are the cutting-edge technology of chemistry, biology, and physics, which have the advantages of wide application range, high sensitivity, high accuracy and good selectivity. Chemically modified electrodes are the core components of electrochemical sensors, enabling specific electrochemical reactions to be carried out exclusively and rapidly on the electrode surface, which is a research hotspot in the field of chemically modified electrodes. [0003] Nano-silver is a tiny elemental silver particle with a particle size of less than 100nm. It has quantum size effect, volume effect and surface effect. These characteristics endow it with unique chemical, physical and biological properties, ...

Claims

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Application Information

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IPC IPC(8): G01N27/26G01N27/30G01N27/48
CPCG01N27/26G01N27/30G01N27/48
Inventor 赵峰鸣王玲巧褚有群
Owner ZHEJIANG UNIV OF TECH