Analytical test method of perfluorosulfonyl fluoride alkene ether
The technology of perfluorosulfonyl fluoroalkenyl ether and fluorosulfonyl fluoroalkenyl ether is applied in the field of analysis and testing of perfluorosulfonyl fluoroalkenyl ether, which can solve the problems of quantitative analysis of impurities and products, and achieve reliable results and simple operation. Effect
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Embodiment 1
[0045] Add 2ml of carbon tetrachloride and 1mmol of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride to a 10mL reaction test tube with magnetic stirring and heating bath (high-resolution NMR purity calibration concentration 98.50%), drop 1.1 mmol of liquid bromine, control the reaction temperature to 40 ° C, react for 0.2 hours, add 1 mmol of sodium bicarbonate aqueous solution to wash, separate layers, take the lower layer of liquid, and inject Agilent's 7890 chromatographic, chromatographic The column is DB-5, and the analytical purity is 98.49%.
Embodiment 2
[0047] Add 1ml of carbon tetrachloride and 1mmol of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride to a 10mL reaction tube with magnetic stirring and heating bath (high-resolution NMR purity calibration concentration 99.90%), 1.05mmol of liquid bromine was added dropwise, the reaction temperature was controlled to 40°C, and the reaction was carried out for 0.1 hour, adding 0.5mmol of sodium bicarbonate aqueous solution for washing, layering, taking the lower layer of liquid, and injecting Agilent's 7890 chromatogram, The chromatographic column is DB-5, and the analytical purity is 99.88%.
Embodiment 3
[0049] Add 1ml of carbon tetrachloride and 1mmol of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride to a 10mL reaction tube with magnetic stirring and heating bath (high-resolution NMR purity calibration concentration 99.95%), 1.05 mmol of liquid bromine was added dropwise, the reaction temperature was controlled to 40° C., and the reaction was carried out for 0.1 hour, adding 0.5 mmol of sodium bicarbonate aqueous solution for washing, layering, taking the lower layer of liquid, and injecting Agilent 7890 chromatogram, The chromatographic column is DB-5, and the analytical purity is 99.92%.
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