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Qualitative screening method for hexabromocyclododecane in polymer materials for electrical and electronic products

A technology of hexabromocyclododecane and polymer materials, applied in the field of analytical chemistry, can solve the problems of complex processing process, long time-consuming, large organic solvent, etc., and achieve the effects of less sample consumption, simple and rapid method, and high sensitivity

Active Publication Date: 2020-06-23
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, research reports mainly focus on biological, environmental and food samples, and there are relatively few studies on electrical and electronic products.
Moreover, the pretreatment process of the existing detection methods is complex, and most of them use solvent extraction, which not only consumes a large amount of organic solvents, but also takes a long time and is expensive.

Method used

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  • Qualitative screening method for hexabromocyclododecane in polymer materials for electrical and electronic products
  • Qualitative screening method for hexabromocyclododecane in polymer materials for electrical and electronic products
  • Qualitative screening method for hexabromocyclododecane in polymer materials for electrical and electronic products

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A qualitative screening method for hexabromocyclododecane in polymer materials of electrical and electronic products, using tweezers or a micro spoon to take 0.5 mg of a small piece or powder sample and put it into a sample cup, accurate to 0.01 mg. The weighed sample is put into the thermal cracker for thermal analysis, and the hexabromocyclododecane released by thermal analysis directly enters the inlet of the gas chromatography-mass spectrometer through the outlet of the thermal cracker, and then Subsequent analysis was carried out by gas chromatography-mass spectrometry.

[0037] The thermal analysis temperature of the pyrolyzer is 300°C for instant cracking, that is, when the sample to be tested is heated to 300°C in the pyrolyzer, the HBCCD is released completely, and the work of the pyrolyzer can be ended.

[0038] The conditions of the gas chromatography in the gas chromatography-mass spectrometry instrument are as follows: VF-5MS capillary column is used; the t...

Embodiment 2

[0044] Experimental condition optimization in embodiment 1 determines experiment:

[0045] 1.1 Instruments and reagents

[0046] Gas chromatography-mass spectrometry (5890N / 5975C model produced by Agilent Corporation of the United States), thermal cracker (EGA / PY-3030D model produced by Frontier Corporation of Japan);

[0047] Analytical balance, the sensitivity is 0.01mg;

[0048] CNC ultrasonic cleaner (KQ-300E, Kunshan Ultrasonic Instrument Co., Ltd.): working frequency 40kHz;

[0049] Sample preparation tools: scissors, pliers, cryo-grinder, and similar.

[0050] microinjector;

[0051] Acetone, tetrahydrofuran, dichloromethane (chromatographically pure, Baker company);

[0052] HBCDD standard product (CAS: 3194-55-6, purity 95%), Shanghai Macklin Biochemical Technology Co., Ltd.

[0053] HBCDD standard product (CAS: 25637-99-4, purity 97%), Mobibe (Shanghai) Biotechnology Co., Ltd.

[0054] 1.2 Preparation of standard solution

[0055] HBCDD standard stock solution...

Embodiment 3

[0087]Adopt the method that embodiment 1 establishes to 1# computer display screen shell (black), 2# toner cartridge shell (gray), 3# printer shell (white), 4# mouse shell (black), 5# mouse line shell ( Black), 6# mouse cable inner shell (orange), 7# mouse cable interface rubber cover (green), 8# plug-in shell (white), 9# plug-in switch (red), 10# plug-in display case ( Transparent color), 11# plug-in cable shell (white), 12# plug-in cable inner shell (blue), 13# plug-in plug shell (white) 13 actual samples and self-made PC and PS samples were tested. The test results are shown in Table 5. The chromatograms of positive samples PC and PS are as follows: Figure 15 and Figure 16 shown.

[0088] Table 5: Test results of actual samples

[0089]

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Abstract

The invention belongs to the field of analytical chemistry, and relates to a qualitative screening method for hexabrocyclododecane in polymer materials of electrical and electronic products. A sampleto be detected is directly introduced into a pyrolyzer after being smashed or sheared, the hexabromocyclododecane is analyzed from the polymer material in an instant cracking manner at 300 DEG C, andthen enters into a gas chromatograph-mass spectrometer, and then is separated by a VF-5MS capillary column ( 15m, 0.25 mm, 0.1 [mu]m), and is qualified by retention time and compound characteristic ions. The detection limit of the qualitative screening method can reach 100 mg / kg. The qualitative screening method for hexabrocyclododecane in polymer materials of electrical and electronic products issimple and rapid, a complex pretreatment process is not needed, the solid sample is directly introduced, theusage amount of the sample is small, the sensitivity is high, and the requirement for rapidscreening of the hexabrocyclododecane in the actual electrical and electronic products can be met.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a qualitative screening method for hexabromocyclododecane in polymer materials of electronic and electrical products, in particular to a thermal cracking-gas phase method of hexabromocyclododecane in polymer materials of electrical and electronic products Chromatography-mass spectrometry qualitative screening method. Background technique [0002] As early as 1997, the European Union began to conduct risk assessment work on Hexabromocyclododecane (HBCDD), and classified HBCDD as a key controlled substance. Since then, the United States, Australia, Canada and other countries have also carried out assessment work one after another, and Norway has listed HBCDD as a national banned chemical substance. In 2013, the United Nations "Stockholm Convention on Persistent Organic Pollutants" announced a global ban on the production and use of HBCDD. In recent years, countries around the wo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/125
Inventor 叶曦雯牛增元张甜甜刘坤罗忻李岸锦张清智
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU