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Method for separating and purifying sixteen polycyclic aromatic hydrocarbons in soil

A technology for separation and purification of polycyclic aromatic hydrocarbons, applied in the direction of material separation, measuring devices, and analysis materials, etc., to achieve the effect of less co-spillage, good effect, and less background interference

Inactive Publication Date: 2020-06-12
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the diversity of environmental media and the complexity of PAHs sources, the traditional analysis methods for the sources of PAHs in various environmental media are still insufficient

Method used

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  • Method for separating and purifying sixteen polycyclic aromatic hydrocarbons in soil
  • Method for separating and purifying sixteen polycyclic aromatic hydrocarbons in soil
  • Method for separating and purifying sixteen polycyclic aromatic hydrocarbons in soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] After vacuum freeze-drying the soil sample, grind it evenly, pass through a 200-mesh (0.074mm) nylon sieve, obtain the sample and store it at -20°C to obtain the soil to be tested.

[0059] Accurately weigh 4g of the soil to be tested (according to the concentration of polycyclic aromatic hydrocarbons in the sample, it can be appropriately increased), add 0.5g of copper powder and 1g of diatomaceous earth, mix well and put them into a 34mL stainless steel extraction pool with a glass fiber filter membrane pre-installed at the bottom, and carry out Accelerated solvent extraction (ASE), the filling volume does not exceed 3 / 4 of the cell body. The extraction solvent was a mixed solvent of dichloromethane and acetone with a volume ratio of 1:1. The ASE extraction conditions were static extraction at 100°C for 5 min, 3 cycles, the default pressure was 1500 psi, heating for 5 min, and nitrogen purge for 100 s. If the sample volume is too large and the filling volume exceeds 3...

Embodiment 2

[0070] Embodiment 2: concentration gradient test

[0071] According to the stable carbon isotope properties, PAH monomer δ at different target concentrations 13 The C value will not change with the concentration, and the mixed standard substances of polycyclic aromatic hydrocarbons with concentrations of 0.1mg / L, 0.5mg / L, 1mg / L, 2.5mg / L, 5mg / L and 10mg / L were prepared respectively, according to the implementation The detection method of gas chromatography-isotope ratio mass spectrometer in Example 1 carried out a concentration gradient experiment to observe the lowest signal value under the condition that all 16 PAHs peaked, and based on this, estimated the minimum sample amount of the actual sample in the follow-up test. The experimental results are shown in Table 1:

[0072] Table 1 Mixed standards of PAHs with different concentrations δ 13 C value

[0073]

[0074]

[0075] Note: nd means that the instrument has not detected

[0076] It can be seen from Table 1 th...

Embodiment 3

[0077] Embodiment 3: Matrix spike test

[0078] A soil sample of about 5 g was randomly selected, and 5 μL of 2000 mg / L 16 kinds of PAHs mixed standard solutions were added to its ASE extract (extraction conditions were consistent with Example 1), and the matrix addition test was carried out according to the method of Example 1 , the test results are as Figure 4 shown. Depend on Figure 4 It can be seen from the test results that the co-elution of samples and the co-distillation of target compounds in the method provided by the present invention have a low degree of interference.

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Abstract

The invention relates to the technical field of environment monitoring and provides a method for separating and purifying sixteen polycyclic aromatic hydrocarbons in soil. The method comprises the following steps of using rapid solvent extraction, gel permeation chromatography and a silica gel-aluminum oxide chromatographic column for carrying out combined treatment on the to-be-detected soil; firstly, transferring polycyclic aromatic hydrocarbon in to-be-detected soil into an extracting solution by utilizing accelerated solvent extraction; then, using gel permeation chromatography to remove impurities such as fats and oils from large molecules; and using silica gel-alumina chromatography column to remove alkanes. The method provided by the invention has the advantages that the separationand purification effect is good, the impurities in the finally obtained purification liquid are few, and the phenomena of background interference and co-overflow during detection are few; the invention further provides a method for detecting the stable carbon isotopes of the sixteen polycyclic aromatic hydrocarbon monomers in the soil, the method is good in repeatability, and the ratio of the stable carbon isotopes of the sixteen polycyclic aromatic hydrocarbon monomers in the soil can be rapidly and accurately detected.

Description

technical field [0001] The invention relates to the technical field of environmental monitoring, in particular to a method for separating and purifying sixteen kinds of polycyclic aromatic hydrocarbons in soil and a method for detecting stable carbon isotopes of monomers. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) refer to hydrocarbons containing two or more benzene rings in their molecules. PAHs in the environment can be divided into natural sources and man-made sources. Natural sources are mainly synthesized by microorganisms and some higher plants. Volcanic activities, forest or grassland fires can also produce PAHs; artificial sources are the main sources of PAHs in the environment. The source is mainly the product of incomplete combustion of organic polymer compounds such as coal, petroleum, and wood. [0003] Due to the characteristics of environmental persistence, long-distance migration, bioaccumulation and carcinogenic mutagenicity of PAH...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/062G01N2030/065
Inventor 杨静孙沛刘霞魏昕怡刘敏
Owner EAST CHINA NORMAL UNIV
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