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Preparation method of glassy carbon electrode for detecting pyrocatechol and/or paradioxybenzene in water

A glassy carbon electrode and catechol technology, applied in the field of electrodes, can solve the problems of no improvement in sensitivity, stability and repeatability technical effects, rising and lowering of glassy carbon electrode costs, and achieve high sensitivity, low equipment requirements, good repeatability

Inactive Publication Date: 2015-01-14
GUANGZHOU INGSENS SENSOR TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the inventors' research results show that when the nitrogen doping amount in nitrogen-doped graphene oxide exceeds 8.35% (mass ratio), the prepared nitrogen-doped graphene oxide-modified glassy carbon electrode can be used to detect o-benzene in water. Diphenol or hydroquinone, the technical effects such as sensitivity, stability and repeatability will not be improved, but will be slightly reduced
At the same time, blindly pursuing high nitrogen doping will lead to a substantial increase in the cost of manufacturing glassy carbon electrodes

Method used

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  • Preparation method of glassy carbon electrode for detecting pyrocatechol and/or paradioxybenzene in water
  • Preparation method of glassy carbon electrode for detecting pyrocatechol and/or paradioxybenzene in water
  • Preparation method of glassy carbon electrode for detecting pyrocatechol and/or paradioxybenzene in water

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] Example 1 (preparation of glassy carbon electrode)

[0025] 1. Preparation of nitrogen-doped graphene oxide

[0026] (1) The graphite raw material is oxidized to graphite oxide by the improved Hummers method

[0027] 10g of potassium persulfate (K 2 S 2 o 8 ), 10g phosphorus pentoxide (P 2 o 5 ) and 12g of graphite powder were added to 50mL of 80°C concentrated sulfuric acid (H 2 SO 4 )middle. The above solution was kept at 80° C. and stirred for 4.5 h. After cooling to room temperature, it was diluted with 2 L of deionized water and allowed to stand overnight. The supernatant was decanted, and the pellet was washed several times with deionized water and centrifuged.

[0028] Add concentrated sulfuric acid to the precipitate to the concentration of the precipitate in the concentrated sulfuric acid is 40mg / mL, place in an ice-water bath, slowly add 7g of potassium permanganate (KMnO 4 ), and keep the solution temperature below 10°C. After the mixture was stirr...

example 2

[0046] Example 2 (inspection of main technical indicators of glassy carbon electrode)

[0047] (1) The nitrogen-doped graphene oxide-modified glassy carbon electrode prepared in Example 1 was used as the working electrode, the Ag / AgCl electrode was used as the reference electrode, and the platinum electrode was used as the counter electrode to establish a three-electrode system with an electrolytic cell.

[0048] (2) adding hydroquinone (abbreviated as HQ) and catechol (abbreviated as CC) standard substance respectively to pH 6.5, concentration is 0.1mol L -1 In the phosphate buffer solution, the concentrations were prepared to be 1×10 -6 mol / L, 10×10 -6 mol / L, 20×10 -6 mol / L, 40×10 -6 mol / L, 80×10 -6 mol / L, 120×10 -6 mol / L, 160×10 -6 mol / L and 200×10 -6 8 concentrations of hydroquinone standard solution and 8 concentrations of catechol standard solution of mol / L; because hydroquinone and catechol often exist in waste water at the same time, therefore, in 8 Concentrati...

example 3

[0052] Example 3 (the effect of the ratio of different graphene oxide and ammonium carbonate on the amount of nitrogen doping)

[0053] 1. Get 20 mg of single-layer graphene oxide obtained in the step (2) of the method for preparing nitrogen-doped graphene oxide in example 1, dissolve it in 10 ml distilled water, and ultrasonically disperse to obtain a graphene oxide solution of 2 mg / mL. Add 3.6g of ammonium carbonate to the liner of the tetrafluoroethylene hydrothermal reaction kettle and stir until dissolved. The hydrothermal reaction kettle was placed at 130° C. for 10 h to obtain a black solid precipitate. The precipitated product was continuously washed with deionized water to remove impurities, and the precipitate was dried in an oven at 35° C. for 10 h to obtain sample A of nitrogen-doped graphene oxide.

[0054] 2. Get 20 mg of single-layer graphene oxide obtained in step (2) of the method for preparing nitrogen-doped graphene oxide in example 1, dissolve it in 10 ml ...

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Abstract

The invention relates to a preparation method of a glassy carbon electrode for detecting pyrocatechol and / or paradioxybenzene in water. The method comprises the following steps: (1) adding deionized water into nitrogen doped graphene oxide until the concentration of the nitrogen doped graphene oxide in the deionized water is 2mg / mL, and carrying out ultrasonic dispersion for 2 hours to obtain dispersion liquid, wherein the nitrogen doped graphene oxide is synthesized from ammonium carbonate and monolayer graphene oxide as a precursor according to a weight ratio of (100 to 1) to (120 to 1) by virtue of a hydrothermal method; (2) polishing a bare glass carbon electrode with an effective diameter being 3mm to form a mirror surface, then sequentially carrying out ultrasonic treatment in absolute ethyl alcohol and deionized water for 5 minutes and drying; and (3) dropwise adding 10 microliter of dispersion liquid prepared by the step (1) on the surface of the bare glass carbon electrode treated by the step (2), and then drying to obtain the glassy carbon electrode. The glassy carbon electrode prepared by the method can be used for detecting pyrocatechol and / or paradioxybenzene in water, and is high in sensitivity, high in stability and high in repeatability.

Description

technical field [0001] The invention relates to an electrode composed of active materials, in particular to a preparation method of a glassy carbon electrode with a conductive layer on an insulating support. Background technique [0002] Several phenolic substances commonly found in the environment, such as hydroquinone, catechol, and nitrophenol, are important raw materials or intermediates in the fields of industry, agriculture, and medicine. Phenolic substances are primary poisons that are toxic to organisms and have been listed as priority pollutants by many countries. Phenols can enter the human body through the skin, mucous membranes, or digestive system, and react with proteins in the cytoplasm to induce inactivation of proteins that cannot be dissolved. Phenols have great affinity to the nervous system, and high concentrations of phenols can cause damage to the nervous system. In addition, phenols are difficult to degrade and are very harmful to the environment and...

Claims

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Application Information

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IPC IPC(8): G01N27/30
Inventor 叶建山黄奕莹李雪玲
Owner GUANGZHOU INGSENS SENSOR TECH
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