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Extraction purifying measuring method of polycyclic aromatic hydrocarbons in soil

A polycyclic aromatic hydrocarbons and determination method technology, applied in the field of extraction and purification of polycyclic aromatic hydrocarbons in soil, can solve the problems of large quantitative error, long extraction time, poor stability, etc., and achieve fast analysis speed, short extraction time and low consumption small effect

Inactive Publication Date: 2009-06-24
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most classic method for extracting organic matter in solid samples is to use a Soxhlet extractor for continuous solvent extraction, but the extraction time is longer and the amount of solvent used is larger
Other methods have improved in extraction time and solvent usage, but there are their own shortcomings: such as ultrasonic extraction, which easily decomposes organic substances with poor stability (such as phenanthrene in polycyclic aromatic hydrocarbons); weak polarity during microwave-assisted extraction Or the non-polar extractant used in the extraction of non-polar organics (such as polycyclic aromatic hydrocarbons) does not have a high utilization rate of microwave energy; the equipment used for accelerated solvent extraction is expensive, etc.
However, when HPLC analysis is used, the chromatographic peak retention time is commonly used for qualitative determination, and 254nm is selected as the quantitative wavelength. When this method is qualitative, the reproducibility of the target retention time is high. In addition, the presence of a large number of interfering substances will also lead to large quantitative errors.
Gas chromatography-mass spectrometry (GC-MS) is a method often used in the determination of polycyclic aromatic hydrocarbons in recent years, but mass spectrometry cannot distinguish isomers, and can only be characterized by retention time, so the accurate determination of isomer compounds in PAHs (such as Benzo[b]fluoranthene and benzo[k]fluoranthene) have always been difficult for the determination of trace PAHs in environmental samples

Method used

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  • Extraction purifying measuring method of polycyclic aromatic hydrocarbons in soil
  • Extraction purifying measuring method of polycyclic aromatic hydrocarbons in soil
  • Extraction purifying measuring method of polycyclic aromatic hydrocarbons in soil

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The invention is used to sample and analyze polycyclic aromatic hydrocarbons in the wasteland surface soil near a thermal power plant in Shanghai.

[0027] The obtained soil samples were placed in a dark place to dry naturally. Weigh 200 g of the air-dried soil sample, grind it, and pass through a 200-mesh sieve. Accurately weigh 5.0 g of the sieved sample with an electronic balance, mix it with 5.0 g of anhydrous sodium sulfate, measure 25 mL each of chromatographically pure acetone and n-hexane with a graduated cylinder, and mix it evenly to make an extractant. An automatic Soxhlet apparatus was used for extraction, the temperature of the heating plate was 200°C, hot leaching for 40 minutes, rinsing for 40 minutes, and solvent recovery for 3 minutes. The solvent of the extract was replaced with cyclohexane, and concentrated to 1-2 mL.

[0028] Prepare 5.0g of activated silica gel and 20mL of dichloromethane to make a silica gel slurry, place it in a chromatographic ...

Embodiment 2

[0031] The invention is used to sample and analyze the polycyclic aromatic hydrocarbons in the surface soil of the green belt in the urban area of ​​Shanghai.

[0032] The obtained soil samples were placed in a dark place to dry naturally. Weigh 400 g of the air-dried soil sample, grind it, and pass through a 200-mesh sieve. Accurately weigh 20.0g of the sieved sample with an electronic balance, mix it with 20.0g of anhydrous sodium sulfate, measure 50mL each of chromatographically pure acetone and n-hexane with a graduated cylinder, and mix it evenly to make an extractant. An automatic Soxhlet apparatus was used for extraction, the temperature of the heating plate was 200°C, hot leaching for 70 minutes, rinsing for 70 minutes, and solvent recovery for 5 minutes. The solvent of the extract was replaced with cyclohexane, and concentrated to 1-2 mL.

[0033] Make a slurry of 10.0g of activated silica gel and 30mL of dichloromethane, place it in a chromatographic column (400mm×...

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Abstract

The extraction and purification determination method of polycyclic aromatic hydrocarbons in soil involves the analysis and determination methods of 18 kinds of trace polycyclic aromatic hydrocarbons in soil. The polycyclic aromatic hydrocarbons in soil samples were extracted by an automatic Soxhlet extractor, and then the extract was purified by a silica gel chromatography column to remove polar and non-polar interference substances brought about during the extraction. Finally, high performance liquid chromatography (including diodes) Array detector) for qualitative and quantitative analysis of 18 kinds of polycyclic aromatic hydrocarbons. The extraction solvent consumption of the present invention is small, can be used for the extraction of large-volume samples, the sample analysis speed is fast, and the sample pretreatment cost is low. For 13 kinds of isomers in 5 groups of 18 kinds of polycyclic aromatic hydrocarbons, it can not only accurately identify but also It can be accurately quantified, with low detection limit and high sensitivity. Except for fluorene and perylene, the detection limits of other 16 polycyclic aromatic hydrocarbons are all lower than 10ng / g-dw. It is suitable for rapid, sensitive and accurate analysis of trace polycyclic aromatic hydrocarbons in various soils such as farmland, wasteland and urban green belts.

Description

technical field [0001] The invention discloses an extraction and purification determination method for polycyclic aromatic hydrocarbons in soil, and relates to an analysis and determination method for 18 kinds of trace polycyclic aromatic hydrocarbons in soil. Specifically, technologies such as automatic Soxhlet extraction, silica gel chromatography column purification and high-performance liquid chromatography are used to realize the extraction, purification, analysis and determination of polycyclic aromatic hydrocarbons in the soil environment. It belongs to the comprehensive technology for the diagnosis of polycyclic aromatic hydrocarbon trace organic pollutants in soil. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic, teratogenic and mutagenic, and 16 of them have been included in the list of priority pollutants by the US Environmental Protection Agency. PAHs are mainly produced by the incomplete combustion of organic matter at hig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08G01N1/34
Inventor 赵建夫刘颖陈玲郜洪文黄清辉仇雁翎
Owner TONGJI UNIV