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A method for detecting organic phosphate flame retardants in abs plastics

A technology of ABS plastic and organic phosphoric acid, applied in the field of detection, can solve problems such as unsatisfactory detection results, human health, and environmental safety hazards

Active Publication Date: 2019-12-17
上海微谱检测科技集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, recent studies have shown that excessive use of organophosphate flame retardants (OPFRs) may cause harm to human health and environmental safety; for this reason, many countries and regions have issued laws / regulations to limit the use of OPFRs in various products
[0004] At present, the commonly used detection method is to detect with conventional detection instruments after solid phase extraction, but the detection effect of this detection method for reactive organophosphate flame retardants is not ideal, and there are technical difficulties

Method used

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  • A method for detecting organic phosphate flame retardants in abs plastics
  • A method for detecting organic phosphate flame retardants in abs plastics
  • A method for detecting organic phosphate flame retardants in abs plastics

Examples

Experimental program
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preparation example Construction

[0086] Preparation of chitosan cerium (Ⅳ) complex:

[0087] Add 0.5g of ammonium cerium nitrate and 100ml of 0.5% acetic acid solution into a 250ml three-neck flask, stir well, add 0.5g of chitosan, stir, after it is completely dissolved, continue stirring and adjust the pH to 5.0, continue stirring for 5h, and the reaction is over Afterwards, filter, rinse with 20ml of ethanol, and dry under reduced pressure at 40° C. to obtain chitosan cerium (IV) complex.

[0088] In one embodiment, the hydrolyzing agent can also be an amino acid alkaline earth metal complex.

[0089] The hydrolysis of the phosphate bond is also a nucleophilic substitution process. First, the nucleophilic species hydroxide ion (produced by the dissociation of the water molecule after the activation of the metal ion) attacks the phosphorus atom to form a five-coordinated intermediate. This step is Reversible; in the second step, the P-O bond is broken and the product is generated. The study found that the ...

Embodiment 1

[0124] A detection method for detecting organic phosphate flame retardants in ABS plastics, comprising the following steps:

[0125] (1) Sample pretreatment: Accurately weigh 1.0 g of the sample to be tested, pulverize it, and then dissolve it in tetrahydrofuran (10 ml), add the hydrolysis agent magnesium aminotriacetate complex acetic acid solution (0.18 g / ml, 5 ml) dropwise, shake at room temperature 1h, then the oscillation is terminated, and filtered with a 0.5 μm microporous polytetrafluoroethylene fiber membrane to obtain the sample solution to be tested;

[0126](2) Sample detection: use gas chromatography-mass spectrometer to detect the organophosphate flame retardant in the solution to be tested; wherein the chromatographic conditions are:

[0127] Gas chromatographic column: HP-701 14% Cyanopropyl Phenyl Methyl Capillary30.0m×320μm×0.25μm; carrier gas: high-purity nitrogen; sampling method: splitless injection; injection volume: 1 μl, qualitative by retention time, ...

Embodiment 2

[0133] A detection method for detecting organic phosphate flame retardants in ABS plastics, comprising the following steps:

[0134] (1) Sample pretreatment: Accurately weigh 1.0 g of the sample to be tested, pulverize it, and then dissolve it in tetrahydrofuran (10 ml), add the hydrolysis agent magnesium aminotriacetate complex acetic acid solution (0.18 g / ml, 5 ml) dropwise, shake at room temperature 1h, then the oscillation is terminated, and filtered with a 0.5 μm microporous polytetrafluoroethylene fiber membrane to obtain the sample solution to be tested;

[0135] (2) Sample detection: Utilize gas chromatography-mass spectrometer to detect the organophosphate flame retardant in the solution to be tested, and then analyze the qualitative and quantitative analysis of the organophosphate flame retardant according to the test results; wherein the chromatographic conditions are :

[0136] Gas chromatographic column: HP-701 14% Cyanopropyl Phenyl Methyl Capillary30.0m×320μm×0...

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Abstract

The invention discloses a detection method for detecting organophosphate flame retardants in ABS plastic. The detection method at least comprises the following steps of 1 sample pretreating, wherein a to-be-detected sample is accurately weighed, crushed and dissolved, a hydrolytic agent-acetate solution is added, oscillating is conducted for 0.5 h to 2 h at room temperature, filtering is conducted, a to-be-detected sample solution is obtained, and a chitosan-cerium (IV) complex is adopted as the hydrolytic agent; 2 sample detecting, wherein the to-be-detected solution is detected with a gas chromatography-mass spectrometer, and qualitative and quantitative preliminary analysis is conducted on the to-be-detected solution; 3 sample re-detecting, wherein the to-be-detected solution is detected with 31P-NMP, and further qualitative and quantitative analysis is conducted on a result by combining an analysis result obtained in the step 2. According to the method, the organophosphate flame retardants in the ABS plastic can be quickly, conveniently and accurately detected.

Description

technical field [0001] The invention relates to a detection method, in particular to a detection method for detecting organic phosphate flame retardants in ABS plastics. Background technique [0002] Today's flame retardants and flame retardant materials are facing double challenges from increasingly stringent fire safety standards and environmental protection laws. On the one hand, fire protection standards provide a broad development space for flame retardant materials and promote the continuous development of flame retardant technology; on the other hand, the introduction of environmental protection laws restricts the application of certain halogenated flame retardants. Complying with the requirements of safety and environmental protection development is the principle that all plastic additive developers and applicators must always follow. The product structure of flame retardants has been adjusted at home and abroad, and it is expected to develop high-performance safety ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 宁飞飞孙福胜赵彬希贾梦虹杨玲玲
Owner 上海微谱检测科技集团股份有限公司
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