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Determination method for content of tricresyl phosphate flame retardants in rubber parts of electronic and electrical products

A kind of trimethyl phosphate, electronic and electrical technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of many rubber interferences, insoluble rubber, difficult qualitative and quantitative analysis, etc., to achieve high sensitivity, low detection limit, convenient Accurately Measured Effects

Active Publication Date: 2011-12-14
广东德威检验认证有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the detection of tricresyl phosphate mainly focuses on plastics, textiles, soil and water environment, organisms and other substances, but there is no report on the determination method of tricresyl phosphate in rubber materials, because rubber It is difficult to dissolve in organic solvents, and it is difficult to extract tricresyl phosphates in it by general methods, and there are many interference substances in rubber, so it is difficult to carry out accurate qualitative and quantitative analysis

Method used

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  • Determination method for content of tricresyl phosphate flame retardants in rubber parts of electronic and electrical products
  • Determination method for content of tricresyl phosphate flame retardants in rubber parts of electronic and electrical products
  • Determination method for content of tricresyl phosphate flame retardants in rubber parts of electronic and electrical products

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Embodiment 1

[0032] The detection method of the tricresyl phosphate flame retardant in the antistatic styrene-butadiene rubber mat provided by this embodiment, as attached figure 1 As shown, it mainly includes the following steps:

[0033] (1) Sample preparation

[0034] Freeze and crush the antistatic styrene-butadiene rubber mat until the maximum particle size is less than 0.5 mm, and mix well to obtain a uniform sample.

[0035] (2) Extraction of tricresyl phosphate flame retardants

[0036]Put 0.5g of anhydrous sodium sulfate at the bottom of the extraction tank, weigh about 1g of the pulverized rubber sample (accurate to 0.1mg), add 0.5g of activated copper powder, and the activation process is: put 5g of copper powder in Add 30mL of acetone-concentrated hydrochloric acid (the volume ratio of the two is 1:1, the concentrated hydrochloric acid is commercially available, its mass fraction is about 37%, the same below) mixed solution into 100mL dry ground Erlenmeyer flask, and turn on ...

Embodiment 2

[0057] The detection method of the tricresyl phosphate flame retardant in the EPDM rubber hose of the hydraulic press provided in this embodiment, as attached figure 1 As shown, it mainly includes the following steps:

[0058] (1) Sample preparation

[0059] Freeze and crush the EPDM rubber tube of the hydraulic press until the maximum particle size is less than 0.5mm, and mix well to obtain a uniform sample.

[0060] (2) Extraction of tricresyl phosphate flame retardants

[0061] Put 0.3g of anhydrous sodium sulfate at the bottom of the extraction tank, weigh about 1g of crushed rubber sample (accurate to 0.1mg), add 1.0g 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 the two is 1:1) into the dry ground-mouth Erlenmeyer flask, start the magnetic stirrer to stir vigorously for 5min, and then use the sand core funnel to suction filter....

Embodiment 3

[0083] The detection method of the tricresyl phosphate flame retardant in the temperature-resistant neoprene rubber ring provided by this embodiment, as attached figure 1 As shown, it mainly includes the following steps:

[0084] (1) Sample preparation

[0085] Freeze and crush the temperature-resistant neoprene ring until the maximum particle size is less than 0.5 mm, and mix well to obtain a uniform sample.

[0086] (2) Extraction of tricresyl phosphate flame retardants

[0087] Put 0.2g of anhydrous sodium sulfate at the bottom of the extraction tank, weigh about 1g of the pulverized rubber sample (accurate to 0.1mg), add 0.2g of activated copper powder, the activation process of copper powder is as follows: 5g of copper powder Place in a 100mL dry ground-mouth Erlenmeyer flask, add 30mL of acetone-concentrated hydrochloric acid (1:1) mixed solution, start the magnetic stirrer to stir vigorously for 10 min, and then use a sand core funnel to suction filter. Repeat this twi...

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Abstract

The invention discloses a method for detecting the content of a triocresyl phosphate fire retardant of a rubber part of an electrical or electronic product. The method comprises the following steps of: (1) sample preparation; (2) extraction of the triocresyl phosphate fire retardant: adding heavy metal powder into the sample, uniformly mixing and performing accelerated solvent extraction so as to obtain extract; (3) extract purification: uniformly mixing the extract and an interior label, transferring to a small solid phase extraction column, eluting by using a mixed solvent, collecting and concentrating eluent so as to obtain the purified extract; and (4) measurment of the triocresyl phosphate fire retardant: measuring the purified extract and the triocresyl phosphate mixed standard solution containing the interior label by using a gas chromatography-mass spectrometer, and performing data processing and quantitative analysis to obtain the content of the triocresyl phosphate fire retardant. By the method, interference impurities in the rubber can be eliminated effectively, triocresyl phosphate can be extracted fully, the purification degree is high, the detection sensitivity is high and the sample measurement cost is low.

Description

technical field [0001] The invention relates to a method for detecting the content of tricresyl phosphate flame retardants, in particular to a method for detecting the content of tricresyl phosphate flame retardants 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. With the promulgation and implementation of the widely influential EU RoHS Directive, REACH Directive, and Norwegian PoHS Directive, the use of traditional brominated flame retardants such as polybrominated diphenyl ethers has been gradually reduced, but triphenyl phosphate is the representative The use of phosphorus-containing flame retardants is increasing. In additio...

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岳大磊
Owner 广东德威检验认证有限公司
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