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Method for simultaneous detection of hydroquinone and pyrocatechol, and preparation method for applied nitrogen-doped graphene-modified glassy carbon electrode

A technology of nitrogen-doped graphene and glassy carbon electrodes, applied in the direction of material electrochemical variables, etc., can solve the problems of poor reagent stability, high instrument operating costs, and complicated operations, and achieve simple operation, low cost, and high detection sensitivity. Effect

Inactive Publication Date: 2013-08-28
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the disadvantages of complex operation, time-consuming, high instrument operation cost and poor reagent stability, these methods limit the application of rapid and accurate determination. method is important

Method used

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  • Method for simultaneous detection of hydroquinone and pyrocatechol, and preparation method for applied nitrogen-doped graphene-modified glassy carbon electrode
  • Method for simultaneous detection of hydroquinone and pyrocatechol, and preparation method for applied nitrogen-doped graphene-modified glassy carbon electrode
  • Method for simultaneous detection of hydroquinone and pyrocatechol, and preparation method for applied nitrogen-doped graphene-modified glassy carbon electrode

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation method of nitrogen-doped graphene (NG)

[0043] Graphene oxide (GO) is firstly prepared for later use: it is prepared by the Hummer method.

[0044] Assemble a 250 mL reaction flask in an ice-water bath, add an appropriate amount of concentrated sulfuric acid, add a solid mixture of 2 g of graphite powder and 1 g of sodium nitrate under stirring, and then add 6 g of potassium permanganate in portions, and control the reaction temperature not to exceed Stir at 20°C for a period of time, then raise the temperature to about 35°C, continue stirring for 30 minutes, then slowly add a certain amount of deionized water, continue stirring for 20 minutes, and add an appropriate amount of hydrogen peroxide to reduce the residual oxidant, making the solution bright yellow. Filter while hot and wash with 5% HCl solution and deionized water until no sulfate is detected in the filtrate. The filtrate was then dispersed under ultrasonic conditions for 2 h to obtain a bro...

Embodiment 2

[0047] Preparation method of nitrogen-doped graphene (NG)

[0048] Ultrasonic disperse 150mg GO in 30ml water, add a certain amount of concentrated HCl to form 1mol L -1 The solution. Then 100mg of pyrrole was added to the above solution, followed by 3ml containing 0.15g (NH 4 ) 2 S 2 o 8 1mol L -1 HCl solution was added to the above solution (graphene oxide solution: containing (NH 4 ) 2 S 2 o 8 1mol L -1 The volume ratio of HCl solution was 10:1), and after reacting at room temperature for 24 hours, the formed GO-ppy complex was filtered, washed, and dried under vacuum at 55 °C overnight. Finally, GO-ppy was thermally decomposed at 800 °C for 30 min in an argon atmosphere to obtain nitrogen-doped graphene.

Embodiment 3

[0050] Preparation method of nitrogen-doped graphene (NG)

[0051] Ultrasonic disperse 180mg GO in 36ml water, add a certain amount of concentrated HCl to form 1mol L -1 The solution. Then 100mg of pyrrole was added to the above solution, followed by 3.6ml containing 0.2g (NH 4 ) 2 S 2 o 8 1mol L -1 HCl solution was added to the above solution (graphene oxide solution: containing (NH 4 ) 2 S 2 o 8 1mol L -1 The volume ratio of HCl solution was 10:1), and after reacting at room temperature for 24 hours, the formed GO-ppy complex was filtered, washed, and dried under vacuum at 55 °C overnight. Finally, GO-ppy was thermally decomposed at 1000 °C for 30 min in an argon atmosphere to obtain nitrogen-doped graphene.

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Abstract

The invention discloses a novel method for simultaneous detection of hydroquinone and pyrocatechol by using a nitrogen-doped graphene-modified electrode. The method comprises the following steps: 1) placing the nitrogen-doped graphene-modified electrode in a sodium phosphate buffer solution which has a concentration of 0.1 mol / L and a pH value of 7 and contains hydroquinone and pyrocatechol with a total concentration of 1* 10<-4> mol / L and carrying out cyclic voltammetric scanning of different scanning speeds with a platinum wire electrode used as a counter electrode and a saturated calomel electrode used as a reference electrode; 2) placing the nitrogen-doped graphene-modified electrode in a sodium phosphate buffer solution which has a concentration of 0.1 mol / L and a pH value of 7 and contains pyrocatechol with a concentration of 1* 10<-5> mol / L and hydroquinone with different concentrations and carrying out differential pulse voltammetric scanning with the platinum wire electrode used as the counter electrode and the saturated calomel electrode used as the reference electrode; and 3) placing the nitrogen-doped graphene-modified electrode in a sodium phosphate buffer solution which has a concentration of 0.1 mol / L and a pH value of 7 and contains hydroquinone with a concentration of 1* 10<-5> mol / L and pyrocatechol with different concentrations and carrying out differential pulse voltammetric scanning with the platinum wire electrode used as the counter electrode and the saturated calomel electrode used as the reference electrode.

Description

technical field [0001] The invention relates to a new method for simultaneously detecting hydroquinone and catechol. Background technique [0002] Hydroquinone, as a kind of phenolic compound, is widely used in many industrial fields such as medicine, plastics, pesticides, dyes, etc., but because it is toxic and difficult to degrade, it becomes an important source of water pollution in the environment and endangers human health; On the one hand, the two isomers of hydroquinone (hydroquinone and catechol) have similar structures and properties at low concentrations, which makes it difficult for people to distinguish between the two. Currently reported methods for distinguishing and detecting quinone mainly include spectrophotometry, high performance liquid chromatography, and electrochemiluminescence. Due to the disadvantages of complex operation, time-consuming, high instrument operation cost and poor reagent stability, these methods limit the application of rapid and accu...

Claims

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Application Information

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IPC IPC(8): G01N27/30G01N27/48
Inventor 卢小泉袁彩霞张村王永兰周喜斌杜娇
Owner NORTHWEST NORMAL UNIVERSITY
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