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Method for determining phthalate ester in soil

A medium phthalate and soil technology, applied in the field of trace pollutant analysis in the environment, can solve problems such as low resolution and overlapping retention times of isomer groups, achieve high sensitivity, reduce matrix interference, and reduce the possibility of Effect

Inactive Publication Date: 2010-10-20
NANKAI UNIV
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  • Claims
  • Application Information

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Problems solved by technology

Liquid chromatography (HPLC) is also one of the main methods for analyzing phthalates. Liquid chromatography solves the problem of low resolution and overlapping retention times between isomer groups when the GC-MS method separates isomer mixtures. question

Method used

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  • Method for determining phthalate ester in soil
  • Method for determining phthalate ester in soil
  • Method for determining phthalate ester in soil

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Embodiment

[0027] The invention uses dichloromethane as the extracting liquid, extracts by ultrasonic extraction, concentrates by nitrogen blowing, and finally analyzes and measures by gas chromatography tandem mass spectrometry (GC / MS), so as to accurately and quickly analyze the phthalate in soil.

[0028] 84 agricultural soils of 21 different land use types in Tianjin were selected as the analysis objects. The analysis methods and results are as follows:

[0029] Extraction process: Take a certain amount of naturally air-dried soil in an Erlenmeyer flask, add 15mL of dichloromethane according to the optimized conditions, ultrasonically extract for 5 minutes, collect the extract after filtering, and repeat the above steps twice;

[0030] Concentration process: blow off the dichloromethane solvent from the combined extract with nitrogen, blow to 5mL, transfer to the concentrator tube and continue to blow to below 2mL, add internal standard, and dichloromethane to volume;

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Abstract

The invention relates to a method for determining phthalate ester in soil, belonging to the filed of analysis of trace contaminants in the environment. The method comprises the following steps: taking dichloromethane as an extract, and extracting by an ultrasonic extraction method; carrying out nitrogen blowing concentration; and finally analyzing and determining by gas chromatography tandem mass spectrometry (GC / MS) so as to accurately and quickly analyze phthalate ester in the soil. The specific analytical determination method comprises the following steps: taking a certain amount of naturally air-dried soil in a conical flask, and adding 10-30mL of dichloromethane; ultrasonically extracting for 5-30min, and collecting the extract after filtering; repeating the steps twice, and combining the extract; nitrogen-blowing to 3-6mL, and transferring to a concentration tube and then continuing to blow to below 2mL; adding internal standard, fixing volume with the dichloromethane, and transferring to an automatic sample bottle; and finally, accurately determining with debugged GC-MS. The determination method developed by the invention is simple and fast, and has the characteristics of high recovery rate, low detection limit, high sensitivity, matrix interference resistance and the like.

Description

【Technical field】 [0001] The invention belongs to the field of analysis of trace pollutants in the environment, in particular to a method for accurately and quickly measuring phthalates in soil. 【Background technique】 [0002] Phthalates (phthalates) are important plasticizers that have attracted attention due to their important effects on reproductive health. The U.S. Environmental Protection Agency (US EPA) classified bis(2-ethylhexyl) phthalate (DEHP), dioctyl phthalate (DOP), benzyl butyl phthalate (BBP) , dibutyl phthalate (DBP), dimethyl phthalate (DMP) and diethyl phthalate (DEP) and other 6 kinds of phthalates are listed as priority control toxic pollutants. my country will DMP , DBP, and DOP are listed as priority monitoring pollutants. Phthalates enter the natural environment, undergo processes such as leaching, volatilization, sedimentation and degradation, migrate and transform in environmental media such as soil, water and the atmosphere, and accumulate in soil ...

Claims

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Application Information

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IPC IPC(8): G01N30/72G01N1/34
Inventor 姬亚芹刘玲玲赵雪艳
Owner NANKAI UNIV
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