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A method for detecting polycyclic aromatic hydrocarbons in liquid phase

A polycyclic aromatic hydrocarbon and liquid phase technology, which is applied in the field of environmental chemical monitoring, can solve the problems of Raman spectrum sensitivity not meeting the detection requirements, low polycyclic aromatic hydrocarbon molecular content, complex substrate preparation process, etc., and achieve Raman signal enhancement ability, high sensitivity, and the effect of improving detection sensitivity

Active Publication Date: 2020-03-06
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the low content of polycyclic aromatic hydrocarbons in the liquid phase, the sensitivity of conventional Raman spectroscopy cannot meet the detection requirements, and surface-enhanced Raman scattering technology is required
The Chinese patent with the publication number CN 102608093A discloses a method for detecting polycyclic aromatic hydrocarbons using surface-enhanced Raman technology. The patent uses thiol-modified Fe 3 o 4 @Ag nanoparticles enrich polycyclic aromatic hydrocarbons and detect them as surface-enhanced Raman active substrates. The operation is simple, but the substrate preparation process is complicated and the dispersion in water is not ideal.

Method used

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  • A method for detecting polycyclic aromatic hydrocarbons in liquid phase
  • A method for detecting polycyclic aromatic hydrocarbons in liquid phase
  • A method for detecting polycyclic aromatic hydrocarbons in liquid phase

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Experimental program
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Embodiment 1

[0029] In this embodiment, the sample is a concentration of 10 -7 For the aqueous solution of pyrene of M, sample A and sample A are used to detect polycyclic aromatic hydrocarbons in the sample. Sample A is a metal-organic framework material MIL-101, and reagent B is a spherical Ag nanoparticle sol.

[0030] Sample A can be prepared by the following method:

[0031] 2.7g Cr(N0 3 ).9H 2 0, l.lg terephthalic acid, and 100mL HF were mixed in 30ml distilled water, and reacted at 220°C for 8 hours; after the reaction was complete, the reaction product was washed with water and ethanol under reflux at 70°C, and the washed product was baked at 150°C Dry to obtain sample A powder, its specific surface area is 2023m 2 / g, the pore size is 2.9nm and 3.4nm.

[0032] Reagent B can be prepared as follows:

[0033] 20mL concentration is 10 -2 M silver nitrate solution, 20mL trisodium citrate solution with a mass percentage of 1% and 80mL deionized water were mixed evenly, and 100mL ...

Embodiment 2

[0038] In this embodiment, the sample is a concentration of 10 -7 For the aqueous perylene solution of M, sample A and sample A are used to detect polycyclic aromatic hydrocarbons in the sample. Sample A is metal-organic framework material UIO-66, and reagent B is polyhedral Au nanoparticle sol.

[0039] Sample A can be prepared by the following method:

[0040] ZrCl 4 1.40g, 0.96g of terephthalic acid, 7.32g of benzoic acid, and 1.0mL of HCl with a concentration of 37% were ultrasonically dissolved in 108mL of DMF, and the mixed solution was transferred to a glass bottle, heated at 120°C for 48 hours, and then centrifuged in DMF Washing; soak the washed product in acetone for 24 hours to replace DMF, then centrifuge, and then vacuum dry at 80°C to obtain sample A powder with a specific surface area of ​​m 2 / g, the pore diameter is about 4.1nm.

[0041] Reagent B can be prepared as follows:

[0042] Heat 37.5mL of ascorbic acid aqueous solution to 60°C, add 0.03mL of a m...

Embodiment 3

[0047] In this embodiment, the sample is a concentration of 10 -4 Anthracene methanol solution of M, using sample A and sample A to detect polycyclic aromatic hydrocarbons in the sample. Sample A is a metal-organic framework material ZIF-8, and reagent B is a spherical Ag nanoparticle sol.

[0048] Sample A can be prepared by the following method:

[0049] 2.58g Zn(NO 3 ) 2 Dissolve in 200mL of methanol to obtain solution A; dissolve 2.63g of 2-methylimidazole in 200mL of methanol to obtain solution B. Solution A and solution B were mixed, stirred for 15 minutes, and then aged at room temperature for 24 hours. The obtained white precipitate was centrifuged, washed with methanol and dried at 100°C to obtain sample A powder with a specific surface area of ​​1430m 2 / g, the pore diameter is about 0.34nm. Weigh 100 mg of the sample A powder ZIF-8, sandwich it between two clean glass slides, and press it into a sample A thin slice.

[0050] The preparation method of reagent B...

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Abstract

The invention provides a detection method for polycyclic aromatic hydrocarbons in a liquid phase. The method includes: combining a metal organic framework material and a Raman reinforcing agent, immersing a metal organic framework material into a to-be-detected liquid phase sample, utilizing the porosity and high specific surface area of the metal organic framework material and the pi-pi conjugated effect between the metal organic framework material and the detected polycyclic aromatic hydrocarbons to adsorb polycyclic aromatic hydrocarbon molecules, and then adding the Raman reinforcing agent dropwise to conduct Raman detection. Compared with the prior art, the method has the advantages of low cost, simple and easy operation, and can realize high speed and high sensitivity detection of polycyclic aromatic hydrocarbons in the liquid phase, thus having good application prospects.

Description

technical field [0001] The invention relates to the technical field of environmental chemical monitoring, in particular to a detection method for polycyclic aromatic hydrocarbons in a liquid phase. Background technique [0002] Polycyclic aromatic hydrocarbons are a class of compounds composed of two or more aromatic rings (such as pyrene, perylene, anthracene, fluorene, benzoperylene, benzopyrene, etc.) etc.), has strong three-causing (carcinogenic, teratogenic, mutagenic) effects, and the severity and complexity of the pollution far exceeds that of conventional pollutants. It is an important environmental and food pollutant. Moreover, PAHs can be enriched and amplified in the food chain, and migrate globally through various transport pathways. Therefore, countries all over the world have paid close attention to the prevention and control of PAH pollution. Extensive monitoring of PAH and timely grasp of pollution status and evolution trends are important links in controlli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/65
Inventor 程昱川陈超刘雅娇鲍静静许高杰
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI