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GC-MS detection method for phosphate ester flame retardant plasticizers in textiles

A technology of flame retardant plasticizer and phosphate ester, which is applied in the field of gas chromatography-mass spectrometry combined detection to achieve the effects of high sensitivity, easy operation and little interference of impurities

Inactive Publication Date: 2012-09-12
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the European Union has issued the relevant decree EN71-9:2005, requiring the detection of phosphate compounds such as tributyl phosphate, triphenyl phosphate, and tricresyl phosphate in toys, but there is no related phosphate plasticizer in China. Research Report on Detection Methods in Textiles

Method used

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  • GC-MS detection method for phosphate ester flame retardant plasticizers in textiles
  • GC-MS detection method for phosphate ester flame retardant plasticizers in textiles
  • GC-MS detection method for phosphate ester flame retardant plasticizers in textiles

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Embodiment 1

[0089] Embodiment 1, a kind of gas chromatography-mass spectrometry detection method of phosphate flame retardant plasticizer in textiles, comprises the following steps:

[0090] 1), prepare the sample solution to be tested:

[0091] ①Take 5.0g of the sample to be tested, cut it to 0.5cm×0.5cm, and mix well.

[0092] ②Take 1.0 g (accurate to 0.01 g) of the above-mentioned chopped sample to be tested and place it in a conical flask, add 20 mL of extractant-ethyl acetate to fully immerse the sample, and then place it in an ultrasonic wave with a frequency of 40 kHz at the temperature of a water bath. Ultrasonic extraction at 50°C for 30 minutes; respectively obtain the extract and sample residue after extraction; transfer the extract into a flat-bottomed flask.

[0093] ③ After extraction, add 10 mL of extractant to the sample residue for washing to obtain a washing solution;

[0094] ④ The extract obtained in step ② and the washing solution obtained in step ③ are combined, co...

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Abstract

The invention discloses a GC-MS detection method for phosphate ester flame retardant plasticizers in textiles, comprising the following steps: 1) preparing a sample solution to be tested; 2) preparing standard solutions: dissolving the phosphate ester flame retardant plasticizers with a solvent, thus preparing gradient standard working solutions; 3) injecting the gradient standard working solutions to GC-MS, selecting an ion monitoring mode to assay, determining peak positions of the phosphate ester flame retardant plasticizers, recording peak areas of quantitative ions, making a standard curvilinear equation with concentration for x-axis and peak area for y-axis; 4) replacing the gradient standard work-solutions in the step 3) with the sample solution obtained in the step 1), determining the phosphate ester flame retardant plasticizers in the sample solution and peak areas thereof with the method in step 3), calculating with the standard curvilinear equation obtained in the step 3) so as to obtain the contents of the phosphate ester flame retardant plasticizers in the sample solution.

Description

technical field [0001] The invention relates to a gas chromatography-mass spectrometry detection method suitable for eight types of phosphate ester flame-retardant plasticizers in textiles. Background technique [0002] Phosphate plasticizers are one of the main types of plasticizers. Phosphate plasticizers have dual functions of flame retardancy and plasticization. They can be used as flame retardants and plasticizers. They can be used in polyvinyl chloride , rubber, polyurethane and other synthetic materials are used in PVC products to make the products have excellent resistance to brittleness and discoloration under sunlight exposure, good flame retardancy, and good low-temperature performance. Products using it as a plasticizer can be improved in wear resistance, water resistance and electrical properties. It also has excellent wear-resistant and antibacterial functions, and has good compatibility with polyvinyl chloride, acetic acid, nitrocellulose, polystyrene, polyet...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 吴刚赵珊红吴俭俭郭方龙王力君刘婷张明誉
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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