Extraction purifying measuring method of polycyclic aromatic hydrocarbons in soil

A technology for polycyclic aromatic hydrocarbons and a determination method, which is applied in the field of extraction, purification and determination of polycyclic aromatic hydrocarbons in soil, can solve the problems of long extraction time, large quantitative error, high cost, etc., and achieves short extraction time, fast analysis speed, and low detection limit. Effect

Inactive Publication Date: 2007-08-08
TONGJI UNIV
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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

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

Examples

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Effect test

Embodiment 1

[0027] The invention is used to sample and analyze polycyclic aromatic hydrocarbons in the wasteland surface soil near a thermal power plant in Shanghai.

[0028] 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.

[0029] Prepare 5.0g of activated silica gel and 20mL of dichloromethane to make a silica gel slurry, place it in a chromatographic ...

Embodiment 2

[0032] 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.

[0033] 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.

[0034] 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 PAHs extraction purification determination method in the soil relates to 18 trace PAHs analysis and determination method in the soil. Using automatic Soxhlet extraction instrument to extract PAHs organic in the soil samples, and then using silica gel column chromatography to purify the extracted liquid, remove the polar and non-polar interference during extraction, and finally, using HPLC (with diode array detector) to analyze qualitatively and quantitatively 18 PAHs. In this invention, the extraction solvent consumption is small, and it can be used for large volume sample extraction, with quick sample analysis speed, low-cost sample pretreatment, and for the 5 group 13 isomers in 18 PAHs, it can not only accurately qualitatively but also accurately quantitatively determine, with low detection limit, high sensitivity, and with the exception of fluorine and perylene, the detection limit of the other 16 PAHs all below 10ng/g-dw. It is a rapid, sensitive and accurate analytical method for the trace PAHs, applied to farmland, wasteland, urban green belt and other soil.

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 Applications(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
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