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Analysis measuring method for brominated flame-retardant in plastic component of deserted household electrical appliance

A technology for brominated flame retardants and plastic parts is applied in the field of analysis and determination of brominated flame retardants in plastic parts of waste household appliances, which can solve the problems of incomplete purification of impurities, poor repeatability and accuracy of analysis results, and large amount of solvent used. problems, to reduce the cost of sample analysis, simplify the sample cleanup process, and improve the effect of solubility limitation

Inactive Publication Date: 2009-11-18
TONGJI UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Among them, the traditional Soxhlet extraction method continuously extracts the sample, the extraction time is more than 72 hours, the solvent usage is large, and the manpower consumption is large; the extraction efficiency of brominated flame retardants in household appliances by ultrasonic extraction and microwave-assisted extraction It is not high, and it is not easy to quantify accurately; the equipment required for supercritical fluid extraction is expensive, and it is difficult for general laboratories to have
In terms of sample purification, silica gel / alumina chromatography column purification method is often used, which takes a long time (accounting for 20-40% of the entire analysis process), consumes a lot of reagents, and does not purify impurities thoroughly
In terms of the detection of brominated flame retardants in samples, gas chromatography / mass spectrometry (GC / MS) and gas chromatography / electron capture detector (GC / ECD) are mainly used at home and abroad to determine brominated flame retardants in electrical and electronic products. However, because high-brominated flame retardants are prone to thermal decomposition at high temperatures, the repeatability and accuracy of the analysis results of gas chromatography are poor; although high-brominated flame retardants are determined by high-performance liquid chromatography (HPLC) This shortcoming can be overcome, but due to the low solubility of high-brominated flame retardants in organic solvents, the detection range of the concentration of brominated flame retardants in electrical and electronic products by liquid chromatography is limited, which has become a current issue. A technical difficulty that needs to be overcome in this field

Method used

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  • Analysis measuring method for brominated flame-retardant in plastic component of deserted household electrical appliance
  • Analysis measuring method for brominated flame-retardant in plastic component of deserted household electrical appliance
  • Analysis measuring method for brominated flame-retardant in plastic component of deserted household electrical appliance

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Effect test

Embodiment 1

[0026] The invention is used to analyze the casing of a certain domestic brand TV set and the casing of a certain domestic brand water dispenser, and determine the type and content of brominated flame retardants therein.

[0027] The casing of the TV set and the casing of the water dispenser were collected as samples. After the two samples are coarsely crushed into a diameter of 1cm, the coarsely crushed samples are further finely crushed with a hammer mill. By connecting the screening device to the discharge port of the pulverizer, the online connection of fine crushing and screening is realized. Use, carry out online combined screening, collect 18 mesh sieves and sieve.

[0028] Use an electronic balance to weigh 1 g of the TV casing and water dispenser casing samples processed in the previous step and place them in a 50mL glass beaker; use a graduated cylinder to measure 25mL of tetrahydrofuran (purity: chromatographic grade) and mix them with the plastic sample evenly, and...

Embodiment 2

[0032] The present invention is used to analyze a computer case of a certain brand in the United States.

[0033] Take several representative samples of the computer case. Coarsely pulverize the sample into a size of 1 cm in diameter, use a hammer mill to further pulverize the coarsely pulverized sample, and collect and sieve through a 18-mesh sieve through online joint screening. Accurately weigh 2g of the computer case sample processed in the previous step into a 100mL glass beaker; use a graduated cylinder to measure 30mL of dichloromethane (purity: chromatographic grade) and mix it with the plastic sample evenly, stir to dissolve the sample in the solvent; weigh 20g of silica gel particles (60-100 mesh) mixed with the above solution evenly, and continue to stir to make the solution mix more evenly, and at the same time, completely volatilize the solvent in the sample at a temperature of 25°C to obtain a plastic sample that forms a uniformly distributed plastic film on the ...

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Abstract

The invention provides an analysis measuring method for brominated flame-retardant in a plastic component of a deserted household electrical appliance, relating to the technology for fast identifying and analyzing the brominated flame-retardant in the plastic component of the deserted household electrical appliance. A collected sample of the plastic component of the deserted household electrical appliance is processed by coarse and fine grinding and screen separation and then is dissolved in the dissolvent and uniformly dispersed on the surface of a colloidal silica particle; an automatic Soxhelt's extractor is used for extracting the brominated flame-retardant in the sample; and finally, a high efficiency liquid chromatography (matched with a diode array detector) is used for qualitative / quantitative analysis. The method has the advantages of simple operation of extraction and purification, low consumption of dissolvent, high speed of analysis, accurate qualitative and quantitative determination, low limit of detection and wide range of concentration of detection, solves the technical problem that the solubility is limited during the detection of the brominated flame-retardant by the high efficiency liquid chromatography, and is suitable for the safe identification and the accurate detection of two kinds of brominated flame-retardants, namely polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) in the plastic components of various deserted household electrical appliances, such as a television, an electric refrigerator, a washing machine, a computer, a water drinking machine, etc.

Description

technical field [0001] The method for analyzing and measuring brominated flame retardants in plastic parts of discarded household appliances relates to a rapid identification and analysis technology for brominated flame retardants in discarded household appliances. Specifically, it is an analysis and detection technology for two types of toxic and harmful brominated flame retardants-polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) in plastic parts of discarded household appliances. Background technique [0002] Brominated flame retardants mainly include polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs), which are widely used in various home appliances because of their excellent flame retardant properties. During the use, disposal and recycling of home appliances, large amounts of PBDEs and PBBs will be released into the surrounding environment, posing potential hazards to the ecosystem and human health. At present, they hav...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/89G01N1/28G01N1/34
Inventor 陈玲黄帆孟祥周刘颖潘兆宇向楠李光明
Owner TONGJI UNIV
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