AFc/CB/PVB modified electrode preparation and method for determining free state sulfite and amount by electrode

A technology for modifying electrodes and sulfites, applied in the field of electrochemistry, can solve the problems that the sensitivity of sulfites cannot meet the detection requirements, it is difficult to realize on-site emergency monitoring and on-line analysis, the operation is cumbersome and time-consuming, and it is inexpensive and easy to interfere. , the effect of high sensitivity

Inactive Publication Date: 2015-01-21
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have many disadvantages, such as long analysis time, high cost, cumbersome operation, etc.
These methods generally require pre-treatment of samples, cumbersome and time-consuming operations, and require a lot of supporting equipment, making it difficult to achieve on-site emergency monitoring and online analysis
[0004] Electrochemical methods have been applied to the detection of various substances due to their advantages of simple and fast operation. There are reports in the existing literature that the use of glassy carbon electrodes to detect sulfites, and the use of electrochemical methods to detect sulfites has attracted a lot of research However, the sensitivity of the bare glassy carbon electrode to detect sulfite cannot meet the detection requirements.

Method used

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  • AFc/CB/PVB modified electrode preparation and method for determining free state sulfite and amount by electrode
  • AFc/CB/PVB modified electrode preparation and method for determining free state sulfite and amount by electrode
  • AFc/CB/PVB modified electrode preparation and method for determining free state sulfite and amount by electrode

Examples

Experimental program
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Effect test

Embodiment 1

[0051] (1) Preparation of AFc / CB / PVB modifier mixture:

[0052] Weigh 0.4mg of acetylferrocene, 11.67mg of carbon powder and 10mg of polyvinyl butyral resin (PVB) and mix them evenly, add them to 1mL of absolute ethanol, stir well, and ultrasonically treat for 1-2min. Disperse the carbon powder evenly in absolute ethanol to obtain the AFc / CB / PVB modifier mixture, and let it stand for 5 minutes before use;

[0053] (2) Pretreatment of glassy carbon electrodes:

[0054] The glassy carbon electrode was polished on wet metallographic sandpaper (3000#), and then polished with a particle size of 0.3 μm polishing powder (α-Al 2 o 3 ) suspoemulsion to polish to the mirror surface, and then use 1:1 nitric acid solution, absolute ethanol and double distilled water to ultrasonically clean the glassy carbon electrode for 4 to 5 minutes respectively, and in 0.5mol / L sulfuric acid solution, the above-mentioned cleaned glassy carbon The electrode was scanned by cyclic voltammetry in the p...

Embodiment 2

[0058] (1) Preparation of AFc / CB / PVB modifier mixture:

[0059] Weigh 0.4mg of acetylferrocene, 0.67mg of carbon powder and 10mg of polyvinyl butyral resin (PVB) and mix them evenly, add them to 1mL of absolute ethanol, stir well, and ultrasonicate for 1-2min. Disperse the carbon powder evenly in absolute ethanol to obtain the AFc / CB / PVB modifier mixture, and let it stand for 5 minutes before use;

[0060] (2) Pretreatment of glassy carbon electrodes:

[0061] The glassy carbon electrode was polished on wet metallographic sandpaper (3000#), and then polished with a particle size of 0.3 μm polishing powder (α-Al 2 o 3 ) suspoemulsion to polish to the mirror surface, and then use 1:1 nitric acid solution, absolute ethanol and double distilled water to ultrasonically clean the glassy carbon electrode for 4 to 5 minutes respectively, and in 0.5mol / L sulfuric acid solution, the above-mentioned cleaned glassy carbon The electrode was scanned by cyclic voltammetry in the potential...

Embodiment 3

[0065] (1) Preparation of AFc / CB / PVB modifier mixture:

[0066] Weigh 0.033mg of acetylferrocene, 12.5mg of carbon powder and 10mg of polyvinyl butyral resin (PVB) and mix evenly, add it to 1mL of absolute ethanol, stir well, and ultrasonicate for 1-2min. Disperse the carbon powder evenly in absolute ethanol to obtain the AFc / CB / PVB modifier mixture, and let it stand for 5 minutes before use;

[0067] (2) Pretreatment of glassy carbon electrodes:

[0068] The glassy carbon electrode was polished on wet metallographic sandpaper (3000#), and then polished with a particle size of 0.3 μm polishing powder (α-Al 2 o 3 ) suspoemulsion to polish to the mirror surface, and then use 1:1 nitric acid solution, absolute ethanol and double distilled water to ultrasonically clean the glassy carbon electrode for 4 to 5 minutes respectively, and in 0.5mol / L sulfuric acid solution, the above-mentioned cleaned glassy carbon The electrode was scanned by cyclic voltammetry in the potential rang...

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Abstract

The invention discloses an AFc/CB/PVB modified electrode, which comprises a glassy carbon electrode and a modification layer fixed on the surface of the glassy carbon electrode; and the modification layer comprises a polyvinyl butyral membrane containing powdered carbon and acetylferrocene absorbed on the surface of the polyvinyl butyral membrane. The invention also discloses a method of the AFc/CB/PVB modified electrode, which comprises the following steps: dispersing acetylferrocene, powdered carbon and polyvinyl butyral resin in absolute ethyl alcohol to prepare a mixed liquor containing AFc/CB/PVB modified substrate, then polishing the glassy carbon electrode, adding the mixed liquor containing AFc/CB/PVB modified substrate drop by drop on the surface of the pretreated glassy carbon electrode, and then naturally drying to obtain the AFc/CB/PVB modified electrode. The invention also discloses a method for detecting sulfite by the AFc/CB/PVB modified electrode, and comprises an application for determining free state sulfite and amount. The method has the advantages of strong anti-interference capability, good stability and high sensitivity.

Description

technical field [0001] The invention relates to the field of electrochemistry, in particular to an AFc / CB / PVB modified electrode and a preparation method of the AFc / CB / PVB modified electrode, and the determination of free sulfite and its total amount by using the AFc / CB / PVB modified electrode Applications. Background technique [0002] Sulfurous acid and its salts and sulfur dioxide produced by sulfur combustion are often used as food additives because of their bleaching, anti-oxidation, and antiseptic effects. They are widely used in food processing, but excessive use will cause harm to human health. FAO / WHO stipulates that the human body can allow SO 2 The intake is 0.35-1.50mg / kg (as SO 2 count). Sulfur dioxide is a colorless gas with a pungent smell. People ingest sulfur, sodium sulfite, sodium metabisulfite and other sulfur dioxide-based substances through food in daily life. Sulfur dioxide exceeding the standard can produce toxicity, and its toxicity is mainly man...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/26G01N27/333
Inventor 王丽许磊
Owner ZHEJIANG GONGSHANG UNIVERSITY
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