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Method for enriching phthalate in air through graphene/ionic liquid composite material

A phthalate ester and ionic liquid technology, which is applied in material separation, material analysis, sampling, etc., can solve problems such as cross-contamination and solvent volatilization, and achieve high sensitivity, avoid solvent volatilization, and good selectivity

Active Publication Date: 2016-11-16
CANGNAN BAOFENG PRINTING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a method for enriching phthalates in the air, which does not require the use of a large amount of organic solvents, avoids problems such as solvent volatilization and cross-contamination, and has simple operation steps. Good selectivity and high sensitivity for phthalates, the adsorbent can be reused, and can simultaneously enrich gaseous and granular phthalates

Method used

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  • Method for enriching phthalate in air through graphene/ionic liquid composite material

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preparation example Construction

[0027] Preparation of activated graphene A

[0028] 1) Preparation of graphene oxide A: Weigh 10 g of graphite oxide into a ball mill jar, add 1 g of DMF, add 6 g of ammonium bicarbonate, mill for 13 hours, add the product in the ball mill jar to ethanol, and perform ultrasonication for 28 hours at 20 ° C to obtain The colloidal solution of graphene oxide A is centrifuged, washed successively with deionized water and ethanol, centrifuged, and dried;

[0029] 2) Activation of Graphene Oxide A: Weigh the dried Graphene Oxide A and place it in a tube furnace, inject 65mL min -1 N 2 40min; set the furnace at 10°C min -1 The heating rate was raised to 800 °C; then the gas was changed to CO 2 , flow 20mL min -1 , keep warm for 3h; change the gas to N 2 , flow 60mL min -1 , the tube furnace is cooled to room temperature to obtain activated graphene A;

[0030] Preparation of activated graphene B

[0031] 1) Preparation of graphene oxide B: Weigh 10g of graphite oxide B into ...

Embodiment 1

[0038] Draw 1uL of standard solutions with concentrations of 0.1μg / mL, 0.5μg / mL, 2μg / mL, 5μg / mL, 10μg / mL, 30μg / mL, and 50μg / mL with a micro-sampler, inject them into sampling tube A, and Under the conditions of thermal desorption-gas chromatography-mass spectrometry, the determination is carried out, and the working curve is drawn with the peak area as the ordinate and the concentration as the abscissa.

[0039] Table 2 standard curve detection limit and limit of quantification

[0040] serial number

Embodiment 2

[0042] Draw 1uL of 0.1μg / mL, 0.5μg / mL, 2μg / mL, 5μg / mL, 10μg / mL, 30μg / mL, and 50μg / mL standard solutions with a micro-sampler, inject them into sampling tube B, and Under the conditions of thermal desorption-gas chromatography-mass spectrometry, the determination is carried out, and the working curve is drawn with the peak area as the ordinate and the concentration as the abscissa.

[0043] Table 3 standard curve detection limit and limit of quantification

[0044] serial number

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Abstract

The present invention discloses a method for enriching phthalate in air through a graphene / ionic liquid composite material. According to the present invention, the material obtained by compounding graphene and a poly-1-allyl-3-ethylbenzimidazole hexafluorophosphate ion liquid is adopted as an adsorbent, phthalate in air is analyzed by a thermal desorption-gas chromatography-mass spectrometry combined detection means, and graphene oxide prepared by using a ball milling method is activated with CO2 to obtain the carbon material with characteristics of high specific surface and more pore channels so as to increase the enrichment efficiency; and the method has the following advantages that the use of a large number of the organic solvent is not required, the problems of solvent evaporation, cross-contamination and the like are avoided, the operation steps are simple, the selectivity on phthalate is good, the sensitivity is high, the adsorbent can be recycled, and the gas-state phthalate and the granular phthalate can be simultaneously enriched.

Description

technical field [0001] The invention relates to a method for enriching and detecting phthalates, and more specifically relates to a method using graphene / ionic liquid composite material as an adsorption material combined with thermal desorption-gas chromatography-mass spectrometry Detection means to analyze the method of phthalates in the air. Background technique [0002] Indoor organic pollutants can be divided into volatile and semi-volatile. Semi-volatile organic pollutants refer to a type of organic pollutants with low saturated vapor pressure, low volatility and strong adsorption, mainly including pesticides, plasticizers, flame retardant etc. Phthalates can interact with the secondary molecules of the polymer chain, thereby improving the elasticity of the polymer material, and increasing the ductility and softness of the polymer material. It is an ideal plasticizer, but Phthalates can affect the human endocrine system, leading to reproductive, developmental and beha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/22G01N30/02
CPCG01N1/2214G01N30/02G01N2030/025
Inventor 林福亮
Owner CANGNAN BAOFENG PRINTING
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