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Detection method of hexabromocyclododecane content in rubber parts of electronic and electrical products

A hexabromocyclododecane, electronic and electrical technology is applied in the field of detection of hexabromocyclododecane content in rubber parts of electronic and electrical products, and can solve problems such as high price, difficult qualitative and quantitative analysis, and no reports, etc., Achieving the effect of method sensitivity and low detection limit

Inactive Publication Date: 2011-12-14
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the detection of hexabromocyclododecane focuses on soil and water environment, organisms, plastics, textiles and other substances, and these detection methods are mostly liquid chromatography-mass spectrometry. To obtain trace levels of hexabromocyclododecane The detection results of dodecane require the use of expensive isotopic markers to separately measure the α-, β-, and γ- isomers of hexabromocyclododecane, and then add them up to obtain the total content; for the determination method of hexabromocyclododecane in rubber materials, there is no report at all, because rubber is difficult to dissolve with organic solvents, and it contains many interfering substances, it is difficult to carry out accurate qualitative and quantitative analysis

Method used

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  • Detection method of hexabromocyclododecane content in rubber parts of electronic and electrical products
  • Detection method of hexabromocyclododecane content in rubber parts of electronic and electrical products
  • Detection method of hexabromocyclododecane content in rubber parts of electronic and electrical products

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The detection method of hexabromocyclododecane in the rubber button of the circuit board provided by this embodiment, as attached figure 1 As shown, it mainly includes the following steps:

[0034] (1) Sample preparation

[0035] The rubber button rubber sample of the circuit board is frozen and crushed until the maximum particle size is less than 0.5mm, and mixed to obtain a uniform sample.

[0036] (2) Extraction of HBCD

[0037] Put 0.5g of anhydrous sodium sulfate at the bottom of the extraction tank. Weigh about 1g of crushed rubber sample (accurate to 0.1mg), add 0.5g of activated copper powder, the activation process of copper powder is: put 5g of copper powder in a dry 100mL conical flask, add Acetone-concentrated hydrochloric acid (volume ratio 1:1, concentrated hydrochloric acid is commercially available, with a mass percentage of about 37%) mixed solution 30mL, started the magnetic stirrer to stir vigorously for 10 min, and then filtered it with sand core ...

Embodiment 2

[0059] The detection method of hexabromocyclododecane in the butyl rubber insulating sheet provided by this embodiment, as attached figure 1 As shown, it mainly includes the following steps:

[0060] (1) Sample preparation

[0061] Freeze and crush the butyl rubber insulation sheet until the maximum particle size is less than 0.5 mm, and mix well to obtain a uniform sample.

[0062] (2) Extraction of HBCD

[0063] Put 0.3g of anhydrous sodium sulfate at the bottom of the extraction tank, weigh about 1g of the crushed rubber sample (accurate to 0.1mg), add 0.8g of activated silver powder, the activation process of silver powder is: put 5g of silver powder in 100ml Add 30mL of the mixed solution of acetone and (1+1) nitric acid (the volume ratio of acetone and 1+1 nitric acid is 1:1) into a dry ground-mouth Erlenmeyer flask, start the magnetic stirrer to stir vigorously for 5min, and then use a sand core to Filter through the funnel. Repeat this again, and then wash with wat...

Embodiment 3

[0086] The detection method of hexabromocyclododecane in the nitrile rubber sealing ring that present embodiment provides, as attached figure 1 As shown, it mainly includes the following steps:

[0087] (1) Sample preparation

[0088] Freeze and crush the nitrile rubber sealing ring until the maximum particle size is less than 0.5 mm, and mix well to obtain a uniform sample.

[0089] (2) Extraction of HBCD

[0090] Put 0.1g of anhydrous sodium sulfate at the bottom of the extraction pool. Weigh about 1g of crushed rubber sample (accurate to 0.1mg), add 1.0g of activated lead powder, the activation process of lead powder is: put 5g of lead powder in a dry 100ml conical flask, add The mixed solution of acetone and (1+1) nitric acid (the volume ratio of acetone and 1+1 nitric acid is 1:1) was 30mL, and the magnetic stirrer was started to stir vigorously for 5min, and then suction filtered with a sand core funnel. Repeat this again, and then wash with water until the washing s...

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Abstract

A method for detecting the content of hexabromocyclododecane in electrical and electronic rubber parts, comprising the following steps: (1) sample preparation; (2) extraction of hexabromocyclododecane: adding heavy metal powder to the pulverized sample, mixing Then put it into the accelerated solvent extraction pool and use the organic solvent to carry out accelerated solvent extraction on the sample to obtain the extract; (3) Purification of the extract: transfer the extract to the solid phase extraction column, and then use the mixed solvent for elution, collect the washed Deliquoring and concentrating to obtain purified extract; (4) Determination of hexabromocyclododecane: measure the purified extract and hexabromocyclododecane mixed standard solution with gas chromatography-mass spectrometer, After data processing and quantitative analysis, the content of trace HBCD in electronic and electrical rubber components was obtained. The method can effectively remove interfering impurities in the rubber, and the hexabromocyclododecane can be fully extracted, the purification degree is high, the detection sensitivity is high, and the sample testing cost is low.

Description

technical field [0001] The invention relates to a method for detecting the content of hexabromocyclododecane, in particular to a method for detecting the content of hexabromocyclododecane in rubber parts of electronic and electrical products. Background technique [0002] As countries pay more and more attention to various safety, health and environmental protection issues caused by toxic and harmful substances in industrial and consumer products, Western developed countries have proposed more and more strict control measures. Export trade has formed a strong green trade barrier. Hexabromocyclododecane is one of the environmental control substances. It is an alicyclic additive type high-efficiency flame retardant with high bromine content. It is widely used in plastics, textiles, coatings and adhesives. It has become the third largest flame retardant in the world after decabromodiphenyl ether and tetrabromobisphenol A. However, more and more studies have found that HBCD ha...

Claims

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Application Information

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IPC IPC(8): G01N30/72G01N30/06
Inventor 李丹郑建国周明辉李全忠翟翠萍刘莹峰赵泉
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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