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Detection method for the purity of fluorosulfonic acid
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A detection method, the technology of fluorosulfonic acid, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that the detection method of fluorosulfonic acid purity is susceptible to interference, cumbersome steps, and not intuitive, and achieves comprehensive expression of impurities and high degree of separation High, short-term and high-efficiency effects
Active Publication Date: 2022-07-15
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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[0005] In view of the above-mentioned shortcomings and deficiencies of the prior art, the present invention provides a detection method for the purity of fluorosulfonic acid, which creates suitable detection conditions and adopts ion chromatography to solve the problems of being susceptible to interference, complicated steps and problems in the existing detection method for the purity of fluorosulfonic acid. unintuitive question
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Embodiment 1
[0029] (1) Pretreatment: add 2g of standard fluorosulfonic acid to 40ml of 1 mol / L sodium hydroxide solution (0-5°C) with an excess of 1.5-2 times, add 100ml of pure water, and then adjust pH with 0.1mol / L hydrochloric acid The value is 7-9, properly diluted with eluent, filtered and set aside.
[0030] (2) Add sulfate to treat standard solution: prepare 5 parts of fluorosulfonate standard solution (20.0 μg / mL) with the same concentration, add sulfate ions of 0, 1, 2, 3, and 4 times the mass respectively (with The mass of fluorosulfonic acid in the standard solution is the calculation standard), and prepared into different (with different sulfate concentration) fluorosulfonic acid standard solutions No. 1, 2, 3, 4, and 5.
[0031] Ion chromatography detection conditions are: equipped with a conductivity detector and a corresponding anion chromatography column (Dianan anion chromatography column: AS-22), set the flow rate: 0.8 mL / min; column temperature: 35 °C; cell temperature...
Embodiment 2
[0037] (1) Pretreatment (for the standard product and the sample to be tested): add 2 g of the standard fluorosulfonic acid and 2 g of the sample to be tested to 40 ml of 1 mol / L sodium hydroxide solution (0-5°C) with an excess of 1.5-2 times, Add 100ml of pure water, adjust the pH value to 7-9 with 0.1mol / L hydrochloric acid, dilute properly with eluent, and filter it for later use.
[0038] (2) Add sulfate to treat the standard solution: prepare a fluorosulfonate standard solution (20.0 μg / mL) of the same concentration, add 3 times the mass of sulfate ions (take the fluorosulfonate mass in the standard solution as the calculation standard) , and then processed into gradient concentration (sulfate-containing) fluorosulfonic acid standard solutions A, B, C, D, E.
[0039] Ion chromatography detection conditions are: equipped with a conductivity detector and a corresponding anion chromatography column (Dianan anion chromatography column: AS-22), set the flow rate: 0.8 mL / min; c...
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Abstract
The invention relates to a method for detecting the purity of fluorosulfonic acid, comprising: S1: pretreatment: adding a certain volume of excess sodium hydroxide / potassium solution to a fluorosulfonic acid standard product and a sample to be tested respectively, and adjusting the pH value with hydrochloric acid after the reaction 7-9, the eluent is diluted and filtered for use; S2: draw the standard curve: measure the standard product processed by S1, add the sulfate ion of 2-4 times the quality of the fluorosulfonic acid standard product, and prepare the fluorosulfonic acid standard of gradient concentration The product solution is detected by ion chromatography, and a standard curve is drawn with the concentration of fluorosulfonic acid standard substance and peak area; S3: sample injection detection: measure the sample to be tested processed by S1, and add 2-4 times of sulfuric acid of the mass of the sample to be tested. Root ions, prepare the solution to be tested, detect by ion chromatography, fit the peak area and standard curve, and calculate the content of fluorosulfonic acid in the sample to be tested. Compared with the fluorine determination method, the method of the invention has better linearity, more accurate determination of fluorosulfonic acid, less interference by hydrofluoric acid, comprehensive expression of impurities, high separation degree, short time and high efficiency, and high stability, and has the advantages Low requirements.
Description
technical field [0001] The present invention relates to a method for detecting compounds, in particular to a method for detecting the purity of fluorosulfonic acid. Background technique [0002] Fluorosulfonic acid is a strong acid containing fluorine, which can be regarded as the anhydride of sulfuric acid and hydrofluoric acid. Soluble in polar organic solvents (such as nitrobenzene, acetic acid and ethyl acetate), but insoluble in non-polar solvents (such as alkanes). Reflecting its strong acidity, it dissolves almost all organic matter including weak proton acceptors. Fluorosulfonate is easily hydrolyzed to produce H when it is exposed to water or moisture in the air. 2 SO 4 with HF (FSO 3- +H 2 O→F-+SO 4 2- +2H + ). This super acid is also used in the alkylation of branched alkanes and aromatic compounds, and can also catalyze the polymerization of mono-enes to produce useful polymers. Its uses include: polymerization, degradation, and alienation of inactive a...
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