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Method for measuring hexafluorophosphoric acid radical ion by amperometric titration

A technology of hexafluorophosphate and amperometric titration, applied in the direction of electrochemical variables of materials, etc., can solve the problems of affecting the accuracy of measurement results, long operation time of gravimetric method, interference measurement, etc.

Inactive Publication Date: 2009-06-24
NORTHWEST RES INST OF MINING & METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because permanganate, perrhenate, perchlorate, bromide, iodide iodate, and thiocyanate will all form precipitates with tetraphenylarsenic chloride, these ions interfere with the determination and affect the accuracy of the measurement results
In addition, the ions most likely to coexist with hexafluorophosphate are orthophosphate and monofluorophosphate. Although these ions do not produce precipitation, the gravimetric method takes a long time to operate and the reproducibility of the results is not very good.

Method used

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  • Method for measuring hexafluorophosphoric acid radical ion by amperometric titration
  • Method for measuring hexafluorophosphoric acid radical ion by amperometric titration
  • Method for measuring hexafluorophosphoric acid radical ion by amperometric titration

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Embodiment 1

[0016] Embodiment 1 A method for measuring the hexafluorophosphate ion of lithium hexafluorophosphate by amperometric titration, the steps are:

[0017] (1) Prepare the standard solution of tetraphenylarsenic chloride: accurately measure 8.00ml and dilute it to 100ml with saturated NaCl solution, and use 0.02055mol / l standard KI 3 The solution was calibrated, and the potential change of the tetraphenyl arsenic chloride solution was measured with a PXS-215 ion activity meter. The titration reaction equation is:

[0018] (C 6 h 5 ) 4 As + +I 2 +I→(C 6 h 5 ) 4 AsI 3

[0019] Calculate the end point of the titration, the volume of the standard potassium triiodide solution consumed and the concentration of the calibrated tetraphenyl arsenic chloride solution by using the second-order differential quotient method.

[0020] Calibrate the concentration of tetraphenylarsenic chloride solution.

[0021] The concentration titration data of tetraphenyl arsenic chloride solutio...

Embodiment 2

[0051] Select a newly-purchased commercial-grade lithium hexafluorophosphate sample (content 99.8%), adopt current polarography and gravimetric method to carry out comparative determination respectively, use tetraphenyl arsenic chloride as titrant to carry out current titration to hexafluorophosphate ion, the determined The results are shown in Table 2. Tetraphenylarsenic chloride was used as a precipitating agent to carry out gravimetric determination of hexafluorophosphate ions, and the results are shown in Table 3.

[0052] The results showed that the sample PF determined by the two methods - 6 The average value of the content is consistent, which shows that the current titration method of hexafluorophosphate ion using tetraphenylarsenic chloride as a titrant is a fast, accurate and economical analysis method.

[0053] Table 2 Amperometric titration of hexafluorophosphate ion with tetraphenylarsenic chloride as titrant

[0054]

[0055] Table 3 uses tetraphenylarsenic ...

Embodiment 3

[0059] In the research of preparing lithium hexafluorophosphate by solvent method, carry out 6 parallel determinations for the same sample of the lithium hexafluorophosphate product synthesized by oneself, calculate the standard deviation and relative standard deviation (R SD value), the test shows that the precision of the method can meet the requirements of analysis and determination. The measurement results are shown in Table 4.

[0060] Table 4 precision test results

[0061]

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Abstract

The invention relates to a method for analyzing and measuring hexafluorophosphoric acid ions, in particular to a method for measuring hexafluorophosphoric acid ions through the amperometric titration. The method comprises the following steps: (1), preparing a standard tetraphenylarsonium chloride solution, and calibrating the concentration of the tetraphenylarsonium chloride solution; (2), preparing a hexafluorophosphoric acid ion solution to be tested; (3), setting conditions for polarographic analysis: the initial potential ranges from minus 1.25 to minus 1.78; the sensitivity I is 8; the differentiation is 2.0; the scanning is carried out once; the step length is 5; the hexafluorophosphoric acid ions are subjected to the amperometric titration, with tetraphenylarsinium chloride taken as a titrant; and (4), reducing excess tetraphenylarsonium ions on mercury drops after (C6H5)4AsPF6 is produced, and calculating the concentration of a lithium-ion battery electrolyte sample to be tested on the basis of the concentration of lithium salt in a diluted sample and the dilution multiple. The invention provides the quick, accurate and economical method for measuring the hexafluorophosphoric acid ions. Tetraphenylarsonium chloride can remain in a stable state in a solution, tetraphenylarsonium chloride and hexafluorophosphoric acid salt form complex compound sediment, and the hexafluorophosphoric acid ions are unlikely to be oxidized or reduced by the mercury drops, so that the reducibility of the tetraphenylarsonium ions facilitates the analysis of the hexafluorophosphoric acid ions.

Description

Technical field: [0001] The invention relates to a method for analyzing and measuring hexafluorophosphate ion. Background technique: [0002] Hexafluorophosphate includes lithium hexafluorophosphate, sodium hexafluorophosphate, potassium hexafluorophosphate, ammonium hexafluorophosphate, etc., and is widely used in lithium-ion batteries, catalytic reactions and electropolishing of metals. Lithium hexafluorophosphate is an important electrolyte in the electrolyte of the latest generation of green high-energy rechargeable batteries. It has been developed rapidly in the past 10 years and has been used in mobile electronic terminals such as notebook computers, mobile phones, camcorders, and weapons and equipment with its excellent performance and price advantages. Secondary lithium-ion batteries in the field of equipment occupy a dominant position, and are considered to be high-tech products that are of great significance to the national economy and people's lives in the 21st ce...

Claims

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Application Information

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IPC IPC(8): G01N27/44
Inventor 张析吴国振吴斌王进龙李冠军黄建芬王永斌
Owner NORTHWEST RES INST OF MINING & METALLURGY INST
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