Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode

A technology of p-nitrophenol and glassy carbon electrodes, which is applied in the direction of material electrochemical variables, etc., can solve the problems of time-consuming equipment, high operating costs, restrictions on rapid and accurate measurement, and complicated operations, and achieve excellent specific surface area, simple operation, and detection The effect of high sensitivity

Inactive Publication Date: 2014-05-21
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the methods for the determination of p-nitrophenol in environmental samples include liquid chromatography, spectrophotometry, flow injection and capillary electrophoresis...

Method used

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  • Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode
  • Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode
  • Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode

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Experimental program
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Effect test

Embodiment 1

[0040] Preparation method of PDDA functionalized graphene (PDDA-G)

[0041] Graphene oxide (GO) is firstly prepared for later use: it is prepared by the Hummer method.

[0042] 2.5 g K at room temperature 2 S 2 o 8 and 2.5 g P 2 o 5 Add to 12mL of concentrated sulfuric acid, stir well. Then add 1 gram of graphite powder and stir for 30 minutes to make the mixture uniform. Then the temperature was slowly raised to 80° C. for 4 hours. Then cool down to room temperature, wash repeatedly with secondary water until neutral, filter and dry at 60°C for 24 hours to obtain the preoxidized product. Then weigh 1 gram of the pre-oxidized product and add it to 36 mL of concentrated sulfuric acid that had been cooled to 0°C in advance, and stir for 30 minutes to make it evenly mixed. Then slowly add 5 g KMnO 4 Keep the temperature below 10°C. Stir for 30 minutes to mix well. The temperature was raised to 35°C, and the reaction was carried out for 8 hours. Then add 360mL of sec...

Embodiment 2

[0046] Method for modifying glassy carbon electrodes with PDDA functionalized graphene

[0047] 1) Take 50 mL of 1mg·mL -1 Graphene oxide solution, sonicated for 4h. Add 1 mL of 20% PDDA solution into 50 mL of secondary water, mix well, then add the graphene oxide solution into the PDDA solution under magnetic stirring, continue stirring for 30 min, add 1.5 mL of hydrazine hydrate (80%), and stir well Then put it in a hydrothermal kettle and react at 100°C for 3h, after cooling, centrifuge and wash with secondary water, and vacuum dry at 60°C to obtain PDDA functionalized graphene. The PDDA-functionalized graphene was dispersed in water to form a 1 mg / ml PDDA-functionalized graphene suspension.

[0048] 2) The glassy carbon electrode was polished to a mirror surface with 0.3 μm and 0.05 μm Al2O3 suspension in turn, and then ultrasonically cleaned with 95% ethanol and double distilled water in turn to obtain the treated glassy carbon electrode ;

[0049] 3) Dry the glassy...

Embodiment 3

[0051] A method for detecting p-nitrophenol

[0052] 1) The PDDA-functionalized graphene-modified electrode was placed in a phosphate buffer solution containing p-nitrophenol at pH 7, with a platinum wire electrode as the counter electrode and an Ag / AgCl electrode as the reference electrode, and PDDA functionalized The graphene-modified electrode and the bare electrode were used as working electrodes. from figure 2 It can be seen that compared with the bare electrode (a), the PDDA-functionalized graphene-modified electrode (b) has a good catalytic effect on the detection of p-nitrophenol, greatly improving The reduction potential of p-nitrophenol was determined.

[0053] 2) The graphene-modified electrode functionalized by PDDA contained 1×10 -4 mol L -1 0.2mol L of p-nitrophenol -1 Cyclic voltammetry curves of different scan rates in phosphate buffer at pH 7 ( image 3 ) and the linear relationship between scan rate and peak current ( Figure 4 ) It can be seen th...

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Abstract

The invention discloses a new method for detecting p-nitrophenol by using a PDDA functionalized graphene modified glassy carbon electrode. The method comprises the following steps: taking 50mL of 1mg*mL<-1> graphene oxide solution, and performing an ultrasonic treatment for 4 hours; adding 1mL of 20% PDDA solution into 50mL of secondary water, uniformly mixing, then adding the graphene oxide solution into the PDDA solution in a magnetic stirring manner, keeping on stirring for 30 minutes, adding 1.5mL of hydrazine hydrate (80%), uniformly stirring, putting into a hydrothermal synthesis reactor and reacting for 3 hours at 100 degrees centigrade, cooling, centrifuging and washing by using the secondary water, and performing vacuum drying at 60 degrees centigrade to obtain the PDDA functionalized graphene. Not only is the dispersibility of the PDDA functionalized graphene in the water increased, but also the graphene has positive electricity, a good matrix is provided for preparation of a graphene-based composite material, and the application of the graphene in electro-analytical chemistry is widened.

Description

technical field [0001] The invention relates to a new method for detecting p-nitrophenol. Background technique [0002] Nitrophenol compounds are one of the refractory organic pollutants, especially nitrophenols are widely used in organic synthesis, dyes and explosives production, so the analysis and detection of nitrophenols in the environment is particularly important. So far, the methods for the determination of p-nitrophenol in environmental samples include liquid chromatography, spectrophotometry, flow injection and capillary electrophoresis, etc., which have limited their rapid and accurate determination due to the disadvantages of complex operation, time-consuming and high operating costs. Applications. The electrochemical method has the characteristics of simple electrode preparation, rapid response and high sensitivity. Therefore, it is of great significance to use a chemically modified electrode method for the quantitative determination of p-nitrophenol. Conten...

Claims

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Application Information

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IPC IPC(8): G01N27/30G01N27/48
Inventor 卢小泉彭丹张婧譞王永兰郭旭东
Owner NORTHWEST NORMAL UNIVERSITY
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