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Preparation and Mass Spectrometry Application of a Diheteroatom-doped Graphene/Porous Carbon Composite

A technology of graphene and composites, applied in the field of analytical chemistry, to achieve the effects of good conductivity, good ultraviolet absorption capacity, and simple preparation methods

Active Publication Date: 2021-04-02
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although carbon materials with single doped atoms have been successfully applied to the analysis of MALDI-TOF MS, carbon materials based on double heteroatom doping have not been reported for MALDI-TOF MS so far.

Method used

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  • Preparation and Mass Spectrometry Application of a Diheteroatom-doped Graphene/Porous Carbon Composite

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Experimental program
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Embodiment 1

[0052] (1) Under stirring and ice bath conditions, 0.921 mL of 50% phytic acid solution was continuously added dropwise to 2 mL of graphene solution with a mass concentration of 6 mg / mL, and then 0.458 mL of aniline solution was added dropwise , and set aside after mixing evenly. (2) In the above mixed solution, quickly add 1.25 mmol of ammonium persulfate solution under stirring conditions, and continue to keep it under ice bath conditions for 12 hours. After the graphene / polyaniline gel is initially formed, further use The dialysis bag with MW~14,000 MW dialyzes the unreacted aniline and phytic acid solution to obtain a pure graphene / polyaniline gel, which is finally freeze-dried under liquid nitrogen to obtain a solid powder of graphene / polyaniline. (3) The obtained graphene / polyaniline composite was heated to 900 °C for 2 h at a heating rate of 5 °C / min in an argon atmosphere, and then lowered to room temperature to obtain a three-dimensional co-doped nitrogen and phosphor...

Embodiment 2

[0055] (1) Under the condition of stirring and ice bath, 0.460 mL of 50% phytic acid solution was continuously added dropwise to 2 mL of graphene solution with a mass concentration of 6 mg / mL, and then 0.458 mL of aniline solution was added dropwise , and set aside after mixing evenly. (2) In the above mixed solution, quickly add 1.25 mmol of ammonium persulfate solution under stirring conditions, and continue to keep it under ice bath conditions for 12 hours. After the graphene / polyaniline gel is initially formed, further use The dialysis bag with MW~14,000 MW dialyzes the unreacted aniline and phytic acid solution to obtain a pure graphene / polyaniline gel, which is finally freeze-dried under liquid nitrogen to obtain a solid powder of graphene / polyaniline. (3) The obtained graphene / polyaniline composite was heated to 900 °C for 2 h at a heating rate of 5 °C / min in an argon atmosphere, and then lowered to room temperature to obtain a three-dimensional co-doped nitrogen and ph...

Embodiment 3

[0057] (1) Under stirring and ice bath conditions, 0.460 mL of 50% phytic acid solution was continuously added dropwise to 2 mL of graphene solution with a mass concentration of 6 mg / mL, and then 0.916 mL of aniline solution was added dropwise , and set aside after mixing evenly. (2) In the above mixed solution, quickly add 1.25 mmol of ammonium persulfate solution under stirring conditions, and continue to keep it under ice bath conditions for 12 hours. After the graphene / polyaniline gel is initially formed, further use The dialysis bag with MW~14,000 MW dialyzes the unreacted aniline and phytic acid solution to obtain a pure graphene / polyaniline gel, which is finally freeze-dried under liquid nitrogen to obtain a solid powder of graphene / polyaniline. (3) The obtained graphene / polyaniline composite was heated to 900 °C for 2 h at a heating rate of 5 °C / min in an argon atmosphere, and then lowered to room temperature to obtain a three-dimensional co-doped nitrogen and phosphor...

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Abstract

The invention discloses preparation of double-heteroatom-doped graphene / porous carbon complexes and application of the double-heteroatom-doped graphene / porous carbon complexes to analyzing mass spectra. Double heteroatoms in each double-heteroatom-doped graphene / porous carbon complex refer to a nitrogen atom and a phosphorus atom. The double-heteroatom-doped graphene / porous carbon complexes comprise, by weight, 75-92.0 wt% of graphene / porous carbon, 3-10.0 wt% of nitrogen atoms, 1-5.0 wt% of phosphorus atoms and 4-10.0 wt% of oxygen atoms. The preparation includes preparing graphene / polyaniline gel complexes by the aid of improved polymer gel methods; carbonizing the graphene / polyaniline gel complexes at the high temperatures to generate the nitrogen and phosphorus co-doped three-dimensional graphene / porous carbon complexes in an in-situ manner at one step. The double-heteroatom-doped graphene / porous carbon complexes can be used as MALDI-TOF MS (matrix-assisted laser desorption ionization-time of flight mass spectrometry) novel carbon material matrixes for analyzing the mass spectra of compounds with low molecular weights. The preparation and the application have the advantages that the double-heteroatom-doped graphene / porous carbon complexes can be used as the novel matrixes for detecting small-molecule compounds and are extremely low in background interference peak, high in sensitivity and excellent in reproducibility, and the like.

Description

technical field [0001] The present invention relates to the preparation and application of mass spectrometry of a double heteroatom-doped graphene / porous carbon composite, in particular to the preparation of a nitrogen-phosphorus double-doped graphene / porous carbon composite and its use in matrix-assisted Applications of Laser Desorption Ionization Time-of-Flight Mass Spectrometry for Small Molecule Compound Detection. belongs to the field of analytical chemistry. Background technique [0002] Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is a new type of soft ionization biological mass spectrometry, which is mainly composed of matrix-assisted laser desorption (MALDI) ionization source and time-of-flight (TOF) mass analyzer. Among them, MALDI technology was first proposed by Tanaka. It is a co-crystallized film formed by irradiating the analyte and matrix molecules with laser light. Since the matrix molecules absorb energy throu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/64
CPCG01N27/64
Inventor 王俊中赵慧芳
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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