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Electronic material hexabromocyclododecane content determination method

A technology for measuring hexabromocyclododecane and its method, which is applied in the field of flame retardant content determination, and achieves the effects of easy implementation, convenient method, and reliable implementation

Active Publication Date: 2008-07-09
谱尼测试集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is currently no method for the determination of HBCD in electronic materials using a GC-MSEI source

Method used

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  • Electronic material hexabromocyclododecane content determination method
  • Electronic material hexabromocyclododecane content determination method
  • Electronic material hexabromocyclododecane content determination method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1, the detection of hexabromocyclododecane content in the plastic shell:

[0022] Take 1.0006g of the solid sample to be tested (accurately weighed to 0.0001g), place it in a conical flask, add 60mL of 1:1 n-hexane and acetone, and reflux at 70°C for 4 hours; take it out and cool it to room temperature, and transfer the extraction solution into 250ml In a pear-shaped bottle, use a K-D concentrator to concentrate at 40°C to nearly dryness, and add 2ml of n-hexane.

[0023] Prepare a glass tube (20mm×350mm), one end of which is plugged with solvent-cleaned glass wool, and a 250ml receiver is connected below; add 1g of dehydrated sodium sulfate, 1g of silica gel, 4g of acid-modified silica gel and 1g of dehydrated Sodium sulfate, the column was rinsed with 30 ml of hexane, and the rinsed hexane was discarded. Add the previously concentrated sample, elute the column with 130 mL of hexane and save the entire eluate. The volume of the solution was rotary evaporat...

Embodiment 2

[0048] Embodiment 2, hexabromocyclododecane content determination in PCB board:

[0049] Take 1.0006g of the solid sample to be tested (accurately weighed to 0.0001g), place it in a conical flask, add 60mL of 1:1 n-hexane and acetone, and reflux at 70°C for 4 hours; take it out and cool it to room temperature, and transfer the extraction solution into 250ml In a pear-shaped bottle, use a K-D concentrator to concentrate at 40°C to nearly dryness, and add 2ml of n-hexane.

[0050] Prepare a glass tube (20mm×350mm), one end of which is plugged with solvent-cleaned glass wool, and a 250ml receiver is connected below; add 1g of dehydrated sodium sulfate, 1g of silica gel, 4g of acid-modified silica gel and 1g of dehydrated sodium sulfate. The column was washed with 30 ml of n-hexane, and the washed n-hexane was discarded. Add the previously concentrated sample, elute the column with 130 mL of hexane and save the entire eluate. The volume of the solution was rotary evaporated to ...

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Abstract

The invention relates to a method for determining content of hexabromocyclododecane in electronic material by gas chromatography-mass spectrometry. The method comprises the following steps of: adding n-hexane and acetone with a ratio of 1:(0.5-2) in a sample to be detected, refluxing at 60 to 90 DEG C for 2 to 16 h to extract hexabromocyclododecane, filtering, and purifying to obtain the sample; weighting hexabromocyclododecane standard substance, dissolving with methanol, adding distilled water to fixed volume to obtain a stock solution, and further diluting with methanol to obtain standard solutions with concentration gradient; detecting the sample processed solution by gas chromatography-mass spectrometry; and calculating the result. The inventive method for determining content of hexabromocyclododecane in electronic material has high speed, high efficiency and less error rate not larger than 10%. Accordingly, the invention provides a reliable and easily-implemented method for determining hexabromocyclododecane in electronic material and can meet the requirement of study and production.

Description

technical field [0001] The invention relates to a method for determining the content of flame retardants in electronic materials, in particular to a method for determining the content of hexabromocyclododecane in electronic materials by gas chromatography. Background technique [0002] Brominated flame retardants are a series of aromatic, alicyclic and cycloaliphatic compounds with different bromine contents, which are widely added to plastics, textiles, synthetic fibers and other combustibles to increase their fire resistance. Currently the most widely used flame retardant. Hexabromocyclododecane is one of the most widely used brominated flame retardants. Hexabromocyclododecane, not only refractory, has been shown to bioaccumulate. In the United Kingdom, HBCD has been listed as a priority control compound, and Japan has recently included HBCD in the list of chemicals for attention. However, there is currently no method for the determination of HBCD in electronic material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/34G01N30/86
Inventor 宋薇
Owner 谱尼测试集团股份有限公司
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