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Analysis method of fluorination surfactant

A technology for surfactants and analysis methods, applied in the field of analysis methods and recovery of fluorine-containing surfactants, can solve problems such as complex extraction process, difficult implementation, and unsmooth separation

Inactive Publication Date: 2017-04-26
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

[0005] However, in the investigation and research on the pollution of fluorine-containing surfactants in biological samples, ion-pair extraction and LC-MS / MS method are used for detection. The extraction process is complicated, the detection limit is high and the sensitivity is poor. If it is detected by LC-MS, the fluorine-containing surfactant will block the column of the liquid chromatograph, and the separation of each component in the fluorine-containing surfactant by the liquid chromatograph becomes not smooth, and the concentration of each measurement appears relatively large. Large discrepancies, resulting in problems such as difficult implementation of the measurement itself
[0006] Therefore, there is an urgent need for an analytical method for fluorosurfactants to solve the detection and recovery problems of fluorosurfactants

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] The sample is a polyester sample containing 0.1% PFOA.

[0088] Weigh 10.0g sample and cut it into pieces, add 200ml organic solvent dichloromethane and 2ml concentrated hydrochloric acid to stir for 2h (room temperature), filter, separate soluble and insoluble components, collect soluble components and concentrate to dryness under reduced pressure , add 50ml of dichloromethane to dissolve the solid, blow nitrogen and heat up to 25°C, start to add sulfuryl chloride / dichloromethane (0.042g / 1ml) dropwise, after the dropwise addition, react at 25-30°C for 2h, and the reaction ends Finally, the reaction solution was concentrated to dryness under reduced pressure, 50ml of acetonitrile was added, nitrogen was introduced, 0.02g of resorcinol and 0.01g of sodium methoxide were added, the temperature was raised to 75-80°C, and the reaction was carried out for 5h. After the reaction was completed, the reaction solution was concentrated under reduced pressure Dry to obtain Friedel...

Embodiment 2

[0091] The sample is a polyester sample containing 0.1% PFOS.

[0092] Weigh 10.0g sample and cut it into pieces, add 200ml organic solvent dichloromethane and 2ml concentrated hydrochloric acid to stir for 2h (room temperature), filter, separate soluble and insoluble components, collect soluble components and concentrate to dryness under reduced pressure , add 50ml of dichloromethane to dissolve the solid, pass nitrogen and heat up to 25°C, start to drop oxalyl chloride / dichloromethane (0.042g / 1ml), after the dropwise addition, react at 25-30°C for 2h, and the reaction ends Finally, the reaction solution was concentrated to dryness under reduced pressure, 50ml of acetonitrile was added, nitrogen gas was introduced, 0.025g of resorcinol and 0.01g of sodium methoxide were added, the temperature was raised to 75-80°C, and the reaction was carried out for 5h. After the reaction was completed, the reaction solution was concentrated under reduced pressure Dry to obtain Friedel-Craf...

Embodiment 3

[0095] The samples were cotton textile samples containing 0.1% PFOA.

[0096] Weigh 10.0g sample and cut it into pieces, add 200ml organic solvent dichloromethane and 2ml concentrated hydrochloric acid to stir for 2h (room temperature), filter, separate soluble and insoluble components, collect soluble components and concentrate to dryness under reduced pressure , add 50ml of dichloromethane to dissolve the solid, blow nitrogen and heat up to 25°C, start to add sulfuryl chloride / dichloromethane (0.042g / 1ml) dropwise, after the dropwise addition, react at 25-30°C for 2h, and the reaction ends Finally, the reaction solution was concentrated to dryness under reduced pressure, 50ml of acetonitrile was added, nitrogen was introduced, 0.02g of resorcinol and 0.01g of sodium methoxide were added, the temperature was raised to 75-80°C, and the reaction was carried out for 5h. After the reaction was completed, the reaction solution was concentrated under reduced pressure Dry to obtain ...

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PUM

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Abstract

The invention provides an analysis method of a fluorine-containing surfactant. The method comprises the following steps: 1, extracting: adding a sample containing the fluorine-containing surfactant to a first solvent and concentrated hydrochloric acid, stirring the sample, the first solvent and the concentrated hydrochloric acid, separating soluble components and insoluble components, collecting the soluble components, and carrying out reduced pressure concentration on the collected soluble components until the soluble components are dry; 2, carrying out a halogenation reaction: adding a halogenation agent to the soluble components obtained in step 1, and carrying out the halogenation reaction; 3, carrying out electrophilic substitution: carrying out reduced pressure concentration on a reaction product obtained in step 2, adding a second solvent and sodium methoxide, heating the reaction product, the second solvent and sodium methoxide, adding resorcinol, carrying out an electrophilic substitution reaction, and carrying out reduced pressure concentration after the reaction is completed in order to obtain a reaction product A; and 4, carrying out LC-MS detection on the reaction product A in step 3, wherein the first solvent is one or more of chlorohydrocarbon, acetonitrile and toluene, and the second solvent is one or more of acetonitrile and toluene.

Description

technical field [0001] The invention relates to an analysis method of a fluorine-containing surfactant, in particular to an analysis method and a recovery method of a fluorine-containing surfactant. Background technique [0002] In recent years, perfluorooctane sulfonate (PFOS for short) and perfluorooctanoic acid (PFOA for short) have been used as the main activity of waterproof, oil-proof and stain-resistant finishing agents for textiles, leather and interior decoration products. Components are added to various special clothing, textile and carpet coatings and microwave popcorn packaging bags as well as non-stick pan coatings and other food contact materials, widely used in industrial and consumer product production, these substances are chemically stable, It is difficult to degrade in the environment, has the characteristics of persistence, bioaccumulation, and long-distance environmental migration, and has an impact on human health and the living environment. The extens...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 孙福胜张娟娟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