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Method for measuring content of decabromodiphenyl oxide in plastics by liquid phase chromatography

A technology of decabromodiphenyl ether and liquid chromatography, which is applied in the field of rapid detection of typical brominated flame retardants, can solve the problems of poor spectrum quality, long solvent extraction time, and difficult to quantify accurately, achieving high applicability, Effect of shortening sample processing time and avoiding yield problems

Inactive Publication Date: 2010-10-20
SOUTH CHINA UNIV OF TECH
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Problems solved by technology

[0005] The biggest disadvantage of the existing liquid chromatography is that the solvent extraction takes a long time (at least two hours or more), and if supercritical fluid extraction and other enhanced extraction methods are used, expensive equipment is required, and the quality of the spectrum of the HPLC analysis results is poor, and it is difficult to be accurate. Quantitative

Method used

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  • Method for measuring content of decabromodiphenyl oxide in plastics by liquid phase chromatography
  • Method for measuring content of decabromodiphenyl oxide in plastics by liquid phase chromatography
  • Method for measuring content of decabromodiphenyl oxide in plastics by liquid phase chromatography

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Embodiment 1

[0030] Embodiment 1: Decabromodiphenyl ether content determination in high impact polystyrene

[0031] Such as figure 1 Shown, the present invention measures the flow process of the content of decabromodiphenyl ether in high-impact polystyrene plastics. The solid sample is made of a high-impact polystyrene plastic masterbatch of a domestic brand PS-I and a decabromodiphenyl ether industrial product, which is mixed evenly by banburying, and the mass content of decabromodiphenyl ether is 10.3%. After the above solid sample was crushed into a solid powder with an average size of 0.5 mm by a blade type solid crusher, 0.5821 g of the solid powder was weighed with an analytical balance and placed in a 150 mL Erlenmeyer flask, and then about 50 mL of analytically pure tetrahydrofuran solvent was added. The above solvent and solid sample powder were magnetically stirred for 10 minutes to completely dissolve the solid sample in the tetrahydrofuran solvent. Transfer the above liquid i...

Embodiment 2

[0035] Embodiment 2: Decabromodiphenyl ether content determination in waste TV casings

[0036] The invention is used to determine the content of decabromodiphenyl ether in an imported waste TV casing. After the solid sample is washed and dried, it is crushed into solid powder with an average size of 0.5 mm by a blade-type solid crusher, and 0.6522 g of the solid powder is weighed with an analytical balance and placed in a 150 mL conical flask, and then about 50 mL of analytically pure tetrahydrofuran solvent is added. . The above solvent and solid sample powder were magnetically stirred for 10 minutes to completely dissolve the solid sample in the tetrahydrofuran solvent. Transfer the above liquid into a 100mL volumetric flask and dilute with tetrahydrofuran to obtain a sample solution.

[0037] Take about 3mL of the sample solution and place it in a 5mL glass centrifuge tube, and centrifuge at a speed of 3000rpm for 15 minutes to separate the sample solution into a superna...

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Abstract

The invention discloses a method for measuring the content of decabromodiphenyl oxide in plastics by liquid phase chromatography. The method of the invention comprises the following steps: dissolving plastics into tetrahydrofuran for forming solution; carrying out centrifugal separation on the solution; taking supernatant liquor for carrying out micro-filtration to obtain filter liquid of chromatography solution to be measured; and adopting high-efficiency liquid phase chromatography to measure the content of decabromodiphenyl oxide in the chromatography solution to be measured. Thereby, the total analysis time of the decabromodiphenyl oxide is reduced from at least two hours to half an hour. The method of the invention realizes the goal of fast detecting the content of decabromodiphenyl oxide in the plastics by the efficient liquid phase chromatography method. The invention is applicable to the measurement of content of the polybrominated diphenyl ether in various plastics (such as polystyrene, high impact polystyrene and the like) capable of being dissolved in tetrahydrofuran, particularly the measurement of the content of decabromodiphenyl oxide in the plastics of various electronic and electric appliance products with the inflaming retarding performance requirements.

Description

technical field [0001] The invention relates to a rapid detection technology of typical brominated flame retardants mixed in plastics. Specifically, it is a rapid quantitative analysis method for decabromodiphenyl ether in various plastics soluble in tetrahydrofuran. The invention can be applied to the content detection of decabromodiphenyl ether in new and old electronic and electric appliance plastic products. Background technique [0002] Plastic materials in electronic and electrical products need to add flame retardants because of their special requirements for fire resistance. Decabromodiphenyl ether is one of the most widely used flame retardants. In 2006, the global demand for decabromodiphenyl ether was 56,000 tons, of which more than 7,500 tons were imported by EU countries. An important reason for the current huge demand for decabromodiphenyl ether is that decabromodiphenyl ether is safer for the environment than its low-brominated counterparts. On July 1, 2006...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
Inventor 关国强陈列强解东来谢明权
Owner SOUTH CHINA UNIV OF TECH
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