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Detection method for twelve poly brominated diphenyl ethers in soil

A polybrominated diphenyl ether and detection method technology, which is applied in the field of detection of twelve kinds of polybrominated diphenyl ethers in soil, can solve the problems of ineffective detection of polybrominated diphenyl ether content in soil and many impurities in the extract

Active Publication Date: 2019-07-30
EAST CHINA NORMAL UNIV
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Problems solved by technology

For example, accelerated solvent extraction (ASE) has been applied to the detection of PBDEs. Compared with traditional extraction techniques (such as Soxhlet extraction and microwave extraction), it has the advantages of short detection period and high extraction efficiency, but the impurities in the extract obtained by using ASE method are less However, it is still unable to effectively detect the content of PBDEs in soil

Method used

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  • Detection method for twelve poly brominated diphenyl ethers in soil
  • Detection method for twelve poly brominated diphenyl ethers in soil
  • Detection method for twelve poly brominated diphenyl ethers in soil

Examples

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Embodiment 1

[0046] 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.

[0047] Weigh 4g of the soil to be tested, add 0.5g of copper powder and 1g of diatomaceous earth, mix well and put it into a 34mL stainless steel extraction cell for ASE extraction. The filling volume should 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, and 3 cycles. The default pressure was 1500 psi, heating for 10 min, and nitrogen purging for 60 s.

[0048] After the extraction, transfer the extract (about 40 mL) to a 120 mL round-bottomed flask with a pipette, rinse the inner wall of the ASE collection bottle with n-hexane at least three times, and transfer all the washings to the round-bottomed flask. Add 20 μL of the recovery...

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Abstract

The invention provides a detection method for twelve poly brominated diphenyl ethers in soil, and belongs to the technical field of environment monitoring. The detection method comprises the followingsteps of after the soil to be detected, copper powder and kieselguhr are mixed, extraction is performed by using an accelerated solvent extraction method to acquire extract liquor; organic solvent replacement is performed after the extract liquor is concentrated to acquire purified liquor; purifying the purified liquor by using a gel permeation chromatography to acquire liquid to be detected; anddetecting the liquid to be detected by using a mass coupled chromatograph. The method provided by the invention is short in time, good in separation and extraction effect of poly brominated diphenylethers in samples, small in impurity interference, high in recovery rate and good in repeatability, and particularly has good application value for the analysis and detection of massive soil samples.

Description

technical field [0001] The invention relates to the technical field of environmental monitoring, in particular to a method for detecting twelve kinds of polybrominated diphenyl ethers in soil. Background technique [0002] Polybrominated diphenyl ethers (PBDEs) are a typical class of brominated flame retardants, which are widely used in electronics due to their high flame retardant efficiency, good thermal stability, small amount of addition, little effect on material properties and low price. , electrical, chemical, transportation, building materials, textiles, petroleum, mining and other fields. According to the number and position of bromine atoms on the benzene ring, there are 209 homologues of PBDEs, the common ones are tetrabromodiphenyl ether, pentabromodiphenyl ether, hexabromodiphenyl ether, octabromodiphenyl ether and decabromodiphenyl ether. Phenyl ether etc. [0003] Due to the characteristics of PBDEs such as environmental persistence, long-distance migration,...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/062
Inventor 杨静赵丹丹李月孙沛罗冬梅刘敏
Owner EAST CHINA NORMAL UNIV
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