Method for detecting polybrominated diphenyl ether content in sludge composting sample by using accelerated solvent extraction online purification method

A polybrominated diphenyl ether and accelerated solvent technology, applied in the field of environmental chemical analysis, can solve the problems of long operation time, cumbersome operation, consumption of organic solvents, etc., and achieves the effects of high degree of automation, reduced matrix effect, and easy operation.

Inactive Publication Date: 2018-10-19
CHINA UNIV OF GEOSCIENCES (BEIJING) +1
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Problems solved by technology

Step (1) adopts accelerated solvent extraction technology to extract the sample. Although compared with traditional extraction technology (Soxhlet extraction, etc.), it takes less time, consumes less solvent, and improves extraction efficiency, but the extra...

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  • Method for detecting polybrominated diphenyl ether content in sludge composting sample by using accelerated solvent extraction online purification method
  • Method for detecting polybrominated diphenyl ether content in sludge composting sample by using accelerated solvent extraction online purification method
  • Method for detecting polybrominated diphenyl ether content in sludge composting sample by using accelerated solvent extraction online purification method

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Embodiment 1

[0029] The invention provides a method for analyzing polybrominated diphenyl ethers in sludge compost samples by using an accelerated solvent extraction on-line purification method, which can be used to analyze the contents of 14 kinds of polybrominated diphenyl ethers in sludge compost samples, using the following instruments and reagents:

[0030] Instruments: ASE350 Accelerated Solvent Extractor (Dionex, Germany); Gas Chromatography and Mass Spectrometry (Agilent, USA); Rotary Evaporator; Nitrogen Blowing Apparatus; Low Temperature Freeze Dryer.

[0031] Reagents: graphitized carbon black (120-400 mesh); Florisil (100-200 mesh); acidic silica gel (40-43 mesh); chromatographically pure organic solvents such as dichloromethane and n-hexane. 14 kinds of PBDEs mixed standard: BDE-17, BDE-28, BDE-47, BDE-66, BDE-71, BDE-85, BDE-99, BDE-100, BDE-138, BDE-153, BDE-154, BDE-183, BDE-190, BDE-209 (AccuStandard, BDE COC).

[0032] A method of detecting polybrominated diphenyl ether ...

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Abstract

The invention discloses a method for detecting the polybrominated diphenyl ether content in a sludge composting sample by using an accelerated solvent extraction online purification method. The methodcomprises: treating a sludge composting sample; filling the extraction pool of an accelerated solvent extraction instrument; setting extraction conditions; and after concentrating the extraction liquid, detecting by using a gas chromatograph-mass spectrometer. According to the present invention, according to the characteristics of the sludge composting sample and the characteristics of the targetsubstance polybrominated diphenyl ether, the graphitized carbon black as the key filling material, magnesium silicate, an acidic silica gel and other materials are mixed, and the extraction pool of the accelerated solvent extraction instrument is filled with the obtained mixture, such that the accelerated solvent extraction instrument can extract 14 kinds of polybrominated diphenyl ethers in thesludge composting sample, and can further perform online purification on the sample, wherein the concentrated extraction liquid can be directly subjected to analysis detection by the gas chromatograph-mass spectrometer (NCI mode); and the method has advantages of high recovery rate, greatly-shortened sample pretreatment time, reduced organic solvent consumption and sample treatment cost reducing.

Description

technical field [0001] The invention belongs to the technical field of environmental chemical analysis, and specifically relates to a method for detecting the content of polybrominated diphenyl ethers in sludge compost samples by using an accelerated solvent extraction on-line purification method. Background technique [0002] Polybrominated diphenyl ethers (Polybrominated diphenyl ethers, PBDEs) are a class of compounds in brominated flame retardants, which are widely used in textiles, electronic products, construction and other industrial products and daily products. The surface of the product falls off and enters the environment, and finally enters the urban sewage treatment plant through the urban wastewater and waste transportation pipe network. Municipal sludge is a sedimentary substance produced in the process of urban sewage treatment. The matrix composition of urban sludge is complex and contains various refractory organic substances. If it is discharged arbitrarily...

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 张倩韩贵琳梁涛
Owner CHINA UNIV OF GEOSCIENCES (BEIJING)
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