Quantitative analysis method for surface oxygenic functional groups of graphene materials

A surface oxygen-containing, quantitative analysis technology, which is applied in the direction of chemical analysis by titration, can solve the problems of inability to carry out quantitative analysis, affect application performance, and single conditions, and achieve low test cost, accurate and reliable results, and simple operation. Effect

Inactive Publication Date: 2016-10-12
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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Problems solved by technology

The oxygen-containing functional groups on the surface of graphene materials have a great influence on the surface hydrophilicity, acidity and alkalinity, electrochemical performance, dispersion performance, adsorption performance, etc. of graphene materials, thus affecting its application performance
[0003] Some existing analysis and characterization methods, such as XPS, FTIR, elemental analysis, etc., can only perform qualitative analysis or semi-quantitative analysis on oxygen-containing functional groups, and the error is large, so quantitative analysis cannot be performed.
Graphene materials are an emerging field. In 2014, our research team drafted the China Graphene Industry Technology Innovation Strategic Alliance Standard Q / LM03CGS001-2014: Chemical titration method for quantitative analysis of the content of oxygen-containing functional groups on the surface of graphene, but the standard method The conditions are relatively single, and it is difficult for all research institutions to satisfy them. Therefore, after two years of continuous practical experience on this basis, and on the basis of ensuring that the test results are accurate and reliable, the drying conditions of the samples to be tested, the acid-base titration method, Suspension reaction environment, standard solution concentration, blank test and calculation formula have been expanded and supplemented, so that general laboratories and analysis institutions can meet the test conditions required by the present invention, and the method has been fully improved

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  • Quantitative analysis method for surface oxygenic functional groups of graphene materials
  • Quantitative analysis method for surface oxygenic functional groups of graphene materials
  • Quantitative analysis method for surface oxygenic functional groups of graphene materials

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Experimental program
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Effect test

Embodiment 1

[0066] (1) According to the instructions in GBT 601-2002, prepare 0.05M NaOH and NaHCO with deionized water with a resistivity of 10MΩ 3 、Na 2 CO 3 and HCl aqueous solution, and prepare 0.1M EtONa solution with absolute ethanol. Weigh the working standard reagent potassium hydrogen phthalate, which was dried to constant weight in an electric oven at 105°C, dissolve it in carbon dioxide-free water, and titrate it with the prepared NaOH solution on the potentiometric titrator, and obtain the titration according to the entire titration curve. At the end point, the concentration of NaOH was calculated. Use the calibrated NaOH standard solution to calibrate the concentration of the HCl solution. Use the calibrated HCl standard solution to titrate NaHCO directly on the potentiometric titrator 3 、Na 2 CO 3 Aqueous solution and EtONa ethanol solution;

[0067] (2) Dry the graphene sample 1 to be tested in a vacuum drying oven at 80°C for 12 hours, then cool it to room temperatu...

Embodiment 2

[0080] (1) According to the instructions in GBT 601-2002, prepare 0.05M NaOH and NaHCO with deionized water with a resistivity of 15MΩ 3 、Na 2 CO 3 and HCl aqueous solution, and prepare 0.1M EtONa solution with absolute ethanol. Weigh the working standard reagent potassium hydrogen phthalate, which was dried to constant weight in an electric oven at 107°C, dissolve it in carbon dioxide-free water, add 2 drops of phenolphthalein indicator, and titrate with the prepared NaOH solution, the color of the solution turns pink When the color remains unchanged for 30s, it is the end point of the titration, and the concentration of NaOH is calculated. Use the calibrated NaOH standard to calibrate and titrate the concentration of the HCl solution. Direct titration of NaHCO with calibrated HCl standard solution 3 、Na 2 CO 3 aqueous solution and EtONa ethanolic solution, titrate NaHCO 3 、Na 2 CO 3 Add 10 drops of bromocresol green-methyl red indicator solution every now and then, ...

Embodiment 3

[0094] (1) According to the instructions in GBT 601-2002, prepare 0.08M NaOH and NaHCO with deionized water with a resistivity of 15MΩ 3 、Na 2 CO 3 and HCl aqueous solution, and prepare 0.1M EtONa solution with absolute ethanol. Weigh the working standard reagent potassium hydrogen phthalate, which was dried to constant weight in an electric oven at 103°C, dissolve it in carbon dioxide-free water, add 2 drops of phenolphthalein indicator, and titrate with the prepared NaOH solution, the color of the solution turns pink When the color remains unchanged for 30s, it is the end point of the titration, and the concentration of NaOH is calculated. Use the calibrated NaOH standard solution to calibrate the HCl solution concentration, and use the calibrated HCl standard solution and NaOH standard solution to back-titrate NaHCO 3 、Na 2 CO 3 aqueous solution and EtONa ethanol solution.

[0095] (2) Dry the graphene sample 1 to be tested in a vacuum drying oven at 100°C for 8 hours...

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Abstract

The invention discloses a quantitative analysis method for surface oxygenic functional groups of graphene materials. The method includes that alkalis different in alkalinity and graphene surface oxygenic functional groups different in acidity are in specific acid-alkali neutralization reaction, dilute solutions of sodium hydroxide, sodium carbonate, sodium bicarbonate and sodium ethoxide are adopted for neutralizing the surface oxygenic functional groups of the graphene materials, and quantitative information of single oxygenic functional groups is obtained according to difference values of consumption of the alkalis, wherein the NaHCO3 solution neutralizes carboxyl groups, the Na2CO3 solution neutralizes carboxyl groups and lactonic groups, the NaOH solution neutralizes carboxyl groups, lactonic groups and phenolic hydroxyl groups, and the EtONa solution neutralizes carboxyl groups, lactonic groups, phenolic hydroxyl groups and carbonyl groups. The quantitative analysis method has advantages of accuracy in determination and low test cost.

Description

technical field [0001] The invention relates to a performance characterization method of graphene materials, in particular to a quantitative analysis method for oxygen-containing functional groups on the surface of graphene materials. Background technique [0002] Graphene materials have excellent electrical, mechanical, thermal properties and ultra-high specific surface area, and are widely used in the fields of electronics, aerospace, chemical engineering, biology, and medicine. They are strategic new materials that are being developed by countries all over the world. The oxygen-containing functional groups on the surface of graphene materials have a great influence on the surface hydrophilicity and hydrophobicity, acidity and alkalinity, electrochemical performance, dispersion performance, adsorption performance, etc. of graphene materials, thus affecting its application performance. [0003] Some existing analysis and characterization methods, such as XPS, FTIR, elementa...

Claims

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Application Information

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IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 陈成猛谢莉婧黄显虹孔庆强
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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