A method for detecting fluoride ion content in perfluoroalkylsulfonylimide salts

A technology of perfluoroalkylsulfonylimide salts and fluoride ions, which is applied in the field of analytical chemistry and can solve problems such as the inability to measure fluoride ion content and the interference of fluoride ion electrodes

Active Publication Date: 2019-07-23
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, perfluoroalkylsulfonylimide salts have a greater interference effect on the fluoride ion electrode, so the formula (1) cannot be used to measure the fluoride ion content

Method used

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  • A method for detecting fluoride ion content in perfluoroalkylsulfonylimide salts
  • A method for detecting fluoride ion content in perfluoroalkylsulfonylimide salts
  • A method for detecting fluoride ion content in perfluoroalkylsulfonylimide salts

Examples

Experimental program
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Effect test

Embodiment 1

[0056] (1) Prepare total ionic strength adjustment buffer solution TISAB solution: prepare potassium nitrate-trisodium citrate mixed solution, wherein potassium nitrate 1mol / L, trisodium citrate 1mol / L, and adjust pH with glacial acetic acid to be 6~7;

[0057] (2) Preparation of fluoride ion standard stock solution (concentration: 1000mg / kg): Accurately weigh 0.2210g of the reference reagent NaF (dried at 105-110°C for 2 hours, and cooled to room temperature in a drying oven), and dilute it with deionized water to 100g;

[0058] (3) Preparation of fluoride ion standard test solution:

[0059] Preparation of fluoride ion standard test solution 1 (concentration is 1mg / kg): Accurately weigh 0.0500g of fluoride ion standard stock solution, add 10mL total ionic strength adjustment buffer solution, then add 3.5g potassium nitrate, and finally dilute to 50g, dissolve and mix well;

[0060] Preparation of fluoride ion standard test solution 2 (concentration is 100mg / kg): Accurately w...

Embodiment 2

[0067] (1) prepare total ionic strength adjustment buffer solution TISAB solution: with example 1;

[0068] (2) preparation of fluoride ion standard stock solution (concentration is 1000mg / kg): same as example 1;

[0069] (3) preparation of fluoride ion standard test solution: with example 1;

[0070] (4) Sample analysis

[0071] Fluoride ion standard solution 1 and fluoride ion standard solution 2 were tested with a fluoride ion meter, and the electrode constant S was obtained as 58.57 according to their respective concentrations and potential values;

[0072] Weigh 12.2993gNa + [N(CF 3 SO 2 )(C 2 f 5 SO 2 )] - Sodium perfluoroalkylsulfonylimide was added to a beaker, and 10mL of total ionic strength adjustment buffer solution was added, then diluted to 50.3565g with distilled water, and mixed evenly to obtain a sample solution. The mass of the solution was m s , the solution potential E was measured with a fluoride ion meter 1 is 100.2mV;

[0073] Then add fluorid...

Embodiment 3

[0076] (1) prepare total ionic strength adjustment buffer solution TISAB solution: same as example 1;

[0077] (2) preparation of fluoride ion standard stock solution (concentration is 1000mg / kg): same as example 1;

[0078] (3) preparation of fluoride ion standard test solution: with example 1;

[0079] (4) Sample analysis

[0080] Fluoride ion standard solution 1 and fluoride ion standard solution 2 were tested with a fluoride ion meter, and the electrode constant S was obtained as 59.57 according to their respective concentrations and potential values;

[0081] Weigh 6.5290g lithium bisfluorosulfonyl imide into a beaker, add 10mL total ionic strength adjustment buffer solution, then dilute to 50.0625g with distilled water, mix well to obtain a sample solution, the mass of the solution is m s , the solution potential E was measured with a fluoride ion meter 1 is 40.8mV;

[0082] Then add fluoride ion standard stock solution 0.1507g (m i ), after mixing evenly, measure t...

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Abstract

The invention provides a method for detecting the content of fluorine ions in perfluoroalkyl sulfonyl imine salts. The method comprises the following steps: preparing at least two fluorine ion standard test solutions with different fluorine ion concentrations, measuring the potential values of the standard test solutions, according to the Nernst equation, calculating the electrode constants (S); adding a total ion strength adjusting and buffering solution into perfluoroalkyl sulfonyl imine salts, diluting the solution by water, evenly mixing, measuring the potential value of the sample solution; then adding a fluorine ion standard stock solution into the sample solution, evenly mixing, measuring the potential value of the mixed solution; according to the Nernst equation, calculating the fluorine ion concentration of the sample solution, and finally calculating out the fluorine ion concentration of perfluoroalkyl sulfonyl imine salts. The provided method reduces the dependency of detection of fluorine ions in perfluoroalkyl sulfonyl imine salts on the ion chromatography, is capable of directly, accurately, and rapidly measuring the content of fluorine ions in perfluoroalkyl sulfonyl imine salts, and has the advantages of simple measurement process, high result precision, and wide measuring range.

Description

technical field [0001] The invention relates to a method for detecting fluoride ion content in perfluoroalkylsulfonylimide salts, belonging to the field of analytical chemistry. Background technique [0002] Perfluoroalkylsulfonylimide salts have outstanding applications in many fields due to their anionic chemical structures. For example, lithium perfluoromethylsulfonylimide is used in lithium-ion batteries, lithium-sulfur batteries and gel lithium batteries due to its high solubility, high stability and insensitivity to water; perfluoromethylsulfonyl Potassium imide and sodium salt are used as antistatic agents on liquid crystal panels. Although perfluoromethanesulfonylimide salt has received considerable attention, there has not been a relatively simple and accurate test method for the determination of the fluoride ion content in it. At present, it is common to determine the content of fluoride ion in samples containing a large number of other anions, mainly using the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/00
CPCG01N27/00
Inventor 曹敏香何永刚钱晓兵陈剑李建中
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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