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
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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 Friede
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-Cra
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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