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Pretreatment method of polybrominated diphenyl ethers in environment solid matrix

A polybrominated diphenyl ether and solid matrix technology, which is applied to measuring devices, instruments, scientific instruments, etc., can solve the problems of long extraction time, cumbersome extraction method steps, high energy consumption, etc. less consumption

Active Publication Date: 2015-06-17
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, today's PBDEs sample pretreatment methods have defects or deficiencies such as cumbersome extraction steps, long extraction time, and high energy consumption to varying degrees.

Method used

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  • Pretreatment method of polybrominated diphenyl ethers in environment solid matrix
  • Pretreatment method of polybrominated diphenyl ethers in environment solid matrix

Examples

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Embodiment 1

[0037] like figure 1 As shown, the microwave-assisted extraction of the present invention coupled with solid-phase purification technology analyzes the method for PBDEs in soil, comprising the following steps:

[0038] Step 1. Samples are air-dried and pulverized: the samples are wrapped in tinfoil, and the soil samples to be treated are freeze-dried using a vacuum freeze dryer, and then ground to a smaller particle size with a glass mortar; the freeze-drying temperature is -40 to -60 ℃, the drying time is 24±1h, and the minimum particle size is less than 2mm.

[0039] In this embodiment, the soil sample to be treated is specifically Taizhou farmland soil. During actual operation, the freeze-drying temperature is -50°C, and the drying time is 24 hours. After being air-dried and ground, pass through a 2mm sieve for later use.

[0040] Step 2, microwave-assisted extraction of the sample to be processed, the extraction process is as follows:

[0041] 201. Weigh the soil sampl...

Embodiment 2

[0061] The difference between this example and Example 1 is that the sediment sample to be treated in Step 1 is specifically Taihu Lake bottom mud.

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Abstract

The invention relates to a pretreatment method of polybrominated diphenyl ethers in an environment solid matrix, which is characterized in that a combined technology of microwave auxiliary extraction and solid phase extraction is used for processing solid matrix PBDEs such as soil and deposits. The method comprises the following steps: 1)drying and crushing a sample; 2)performing microwave auxiliary extraction: weighing a soil deposit sample to be processed, weighing a certain amount of extraction solvent, using a microwave digestion / extraction instrument for microwave auxiliary extraction; 3)performing solid-liquid separation; 4)solid phase purification and purification by a small column: performing rotary evaporation on the extract to about 1ml, through solid phase extraction and purification by the small column; and 5)subsequent processing: performing nitrogen blowing on an eluate to a dry state, metering volume on the solvent, after membrane filtration, and using GC-NCI-MS for analysis. According to the invention, pre-treatment time of the sample is short, decomposition of unstable substances such as PBDEs can be avoided, multiple samples can be simultaneously processed, by comparing with a traditional soxhlet extraction method, organic solvent consumption is less, secondary pollution on environment can be avoided, and good extraction effect is reached.

Description

【Technical field】 [0001] The invention belongs to the field of pretreatment methods of PBDEs in environmental samples, and in particular relates to a method for treating PBDEs in soil sediments by microwave-assisted extraction combined with solid-phase extraction technology. 【Background technique】 [0002] Polybrominated diphenyl ethers (PBDEs), as a new type of persistent organic pollutants, are ubiquitous in the environment and organisms, and the pollution level is increasing, causing potential harm to animals, plants and human health. PBDEs have the characteristics of low vapor pressure, hydrophobicity and lipophilicity at room temperature, so they are easy to accumulate in soil or sediment and exist for a long time. Through animal experiments to study the toxicity of PBDEs, it is found that PBDEs have endocrine disrupting toxicity, carcinogenicity and developmental toxicity, etc. Therefore, the risk assessment of PBDEs in aquatic and terrestrial environments has become a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 朱瑞利黄波涛李辉孙志远韩耀宗廖水文向霄
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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