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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AI-Extracted Technical Summary

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...
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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.

Application Domain

Component separationPreparing sample for investigation

Technology Topic

SolventBrominated flame retardant +15

Image

  • 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

Examples

  • Experimental program(2)

Example Embodiment

[0025] Example 1
[0026] The invention is used to analyze the housing of a certain domestic brand TV set and the housing of a certain domestic brand water dispenser, and determine the type and content of the brominated flame retardant therein.
[0027] The housing of the TV set and the housing of the water dispenser were collected as samples. After coarsely crushing the two samples into a size of 1cm in diameter, the coarsely crushed sample is further finely crushed by a hammer mill. By connecting the screening device to the outlet of the crusher, the online connection of fine crushing and screening is realized. Use, carry out on-line combined sieving, collect 18 meshes for sieving.
[0028] Use an electronic balance to weigh 1g each of the TV shell and water dispenser shell samples processed in the previous step and place them in a 50mL glass beaker; measure 25mL of tetrahydrofuran (purity: chromatographic grade) with a graduated cylinder and mix it with the plastic sample evenly, stir to make the plastic sample Thoroughly dissolve in the solvent; weigh 10g of silica gel particles (60-100 mesh) and mix the above solution evenly, and continue to stir to make the solution more evenly mixed, and at the same time, completely volatilize the solvent in the sample at a temperature of 30 ℃, and get on the surface of the silica gel particles. Form a plastic sample with a uniformly distributed plastic film.
[0029] Weigh the above-mentioned plastic sample with an electronic balance, weigh 1/20 of the total weight of the plastic sample for extraction, measure 80 mL of isopropanol as the extraction solvent; use FOSS Soxtec Avanti 2050 automatic Sox-type extraction instrument to extract, set the instrument temperature to 185 ℃, the sample was extracted by solvent hot extraction for 60 minutes, and then Soxhlet reflux extraction for 180 minutes to obtain the waste appliance extract, and the extract was fixed to 100 mL. Measure 10 mL of the extracted solution after constant volume in a glass centrifuge tube and centrifuge at a high speed of 4000 rpm for 20 minutes; take 5 mL of the supernatant and pass it through a 0.45 μm organic filter membrane to obtain the sample to be tested.
[0030] Place the sample to be tested in Shimadzu VP-ODS C 18After separation on the column (250mm×4.6mm ID, 5μm) chromatographic column, the measurement was carried out using Agilent 1200 high performance liquid chromatograph (equipped with Chemstation and diode array detector). The mobile phase is acetonitrile and high-purity water, and the gradient elution program is set to: 0-10 min, 90% acetonitrile and 10% water; 10-13 min, change the gradient of 90% acetonitrile and 10% water to 100% acetonitrile, and hold for 14 min; The elution flow rate is 1.0mL/min; the injection volume is 50μL; the column temperature is 25°C. The diode array detector collects UV spectrum data from 190 to 400 nm. Based on the chromatographic retention time of polybrominated diphenyl ethers and polybrominated biphenyl flame retardants, compare and analyze the acquired UV spectrum data with standard UV spectrum data to determine whether Contains this kind of flame retardant. Quantitative analysis of the content of brominated flame retardants in waste home appliances based on the chromatographic peak area at 225nm wavelength See the result figure 2 with 3. figure 2 The chromatographic peak with an absorbance value of about 15 in 25 to 26 minutes is decabromodiphenyl ether. image 3 The chromatographic peak with an absorbance value of about 35 in 25 to 26 minutes is decabromodiphenyl ether, and the peak that appears in 4 to 5 minutes is impurity peak; therefore, both samples contain decabromodiphenyl ether. The content of brominated diphenyl ether is 14.40 g/kg, and the content of decabromodiphenyl ether in the housing of the drinking fountain is 38.51 g/kg.

Example Embodiment

[0031] Example 2
[0032] The present invention is used to analyze the computer case of a certain American brand.
[0033] Take several representative samples in the computer case. The sample is coarsely crushed into a size of 1 cm in diameter, and the coarsely crushed sample is further finely crushed by a hammer mill, and combined with online sieving, collecting 18 meshes and sieving. Accurately weigh 2g of the computer case sample processed in the previous step into a 100mL glass beaker; measure 30mL of dichloromethane (purity: chromatographic grade) with a graduated cylinder and mix it with the plastic sample, stir to dissolve the sample in the solvent; weigh 20g of silica gel particles (60-100 mesh) mix with the above solution evenly, and continue to stir to make the solution more evenly mixed, and at the same time, completely volatilize the solvent in the sample at a temperature of 25°C to obtain a plastic sample with a uniformly distributed plastic film on the surface of the silica gel particles .
[0034] Weigh the above-mentioned plastic samples, then weigh 1/25 of the total weight for extraction, and measure 100 mL of isopropanol as the extraction solvent; use the FOSS Soxtec Avanti 2050 automatic Sox-type extraction instrument to extract, set the instrument temperature to 170°C, and remove the sample Solvent hot extraction for 50 minutes, and then Soxhlet reflux extraction for 150 minutes, to obtain the waste electrical appliance extract, and the volume of the extract is adjusted to 100 mL. Measure 10 mL of the extracted solution after constant volume in a glass centrifuge tube, and centrifuge at a high speed of 5000 rpm for 10 min; take 2 mL of the supernatant and pass it through a 0.45 μm organic filter membrane to obtain the sample to be tested.
[0035] Place the sample to be tested in Shimadzu VP-ODS C 18 After separation on the column (250mm×4.6mm ID, 5μm) chromatographic column, the measurement was carried out using Agilent 1200 high performance liquid chromatograph (equipped with Chemstation and diode array detector). The mobile phase is acetonitrile and high-purity water. The gradient elution program is set to: 0-10min, 90% acetonitrile and 10% water; 10-13min, 90% acetonitrile and 10% water gradient change to 100% acetonitrile, hold for 14min, total The running time is 27min; the elution flow rate is 1.0mL/min; the injection volume is 50μL; the column temperature is 25°C. The diode array detector collects UV spectrum data from 190 to 400 nm. Based on the chromatographic retention time of polybrominated diphenyl ethers and polybrominated biphenyl flame retardants, compare and analyze the acquired UV spectrum data with standard UV spectrum data to determine whether Contains this kind of flame retardant. Quantitative analysis of the content of brominated flame retardants in waste home appliances based on the chromatographic peak area at 225nm wavelength See the result Figure 4. Figure 4 The chromatographic peak with an absorbance of about 15 in 9-10 minutes is tribromodiphenyl ether, the chromatographic peak with an absorbance of about 34 in 11-12 minutes is tetrabromodiphenyl ether, and the chromatogram with an absorbance of about 8 in 14-15 minutes The peak is pentabromodiphenyl ether, and the chromatographic peak with an absorbance value of about 20 at 17-18 minutes is hexabromodiphenyl ether; therefore, tribromo, tetrabromo, pentabromo and hexabromodiphenyl ether are detected in the computer case sample The content of flame retardant is 3.42, 6.50, 1.50, 2.06g/kg, respectively.

PUM

PropertyMeasurementUnit
Diameter1.0 ~ 2.0cm

Description & Claims & Application Information

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