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Method for determining chlorine ions in vanadium electrolyte

An electrolyte and chloride ion technology, applied in measuring devices, material analysis through optical means, instruments, etc., can solve the problems of easy to cause errors, harsh experimental conditions, and low accuracy of measurement results, so as to reduce errors and absorb small Effect

Pending Publication Date: 2018-05-08
湖南汇锋高新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The molar method is more accurate for the determination of substances with higher chloride ion content, but it will cause large analysis errors for samples with low chloride ion content, and the color resolution of the titration end point is not obvious and easy to cause errors; the mercury method will produce after the experiment. Toxic mercury-containing waste liquid has a great impact on environmental pollution and the health of operators, and the color judgment of the end point of the mercury method is inaccurate
Because the potentiometric titration method uses silver nitrate standard solution for titration, the resulting silver chloride precipitate is unstable, so the measurement accuracy of this method is not high, and the silver nitrate reagent is costly and toxic, and is easy to pollute the environment; the volumetric method can be divided into nitric acid Silver volumetric method and mercury nitrate volumetric method, the silver nitrate volumetric method is a precipitation titration method, the end point color change is not sensitive, the mercury nitrate volumetric method titration end point color change is very sensitive, but the pH value of the test solution must be strictly controlled within a certain range, and the experimental conditions are harsh
These methods are not suitable for the determination of chloride ion content in vanadium electrolyte
At present, there is no literature report on the detection method of trace chloride ion content in the vanadium battery electrolyte

Method used

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  • Method for determining chlorine ions in vanadium electrolyte
  • Method for determining chlorine ions in vanadium electrolyte
  • Method for determining chlorine ions in vanadium electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] ① Oxidize the electrolyte sample into an electrolyte containing pentavalent vanadium, and dilute it 25 times at the same time

[0028] Pipette 4ml of vanadium battery electrolyte in a 100ml beaker, add 8ml of sulfur-phosphorus mixed acid (sulfuric acid: phosphoric acid: water volume ratio 1:1:2), then add 5mol / L potassium permanganate dropwise to oxidize until the solution is reddish, static Set aside for 5 minutes, add 5ml of urea (20wt%), dropwise add 4 to 6 drops of sodium nitrite (1wt%) to make the solution yellow, transfer it to a 100ml volumetric flask, shake well, add water to make up to 100ml.

[0029] ②Drawing of working curve

[0030] Take 25ml of pure pentavalent vanadium solution in six 50ml volumetric flasks, respectively add 0mL, 1mL, 2mL, 3mL, 4mL, 5mL chlorine standard solution, then add 2ml of nitric acid (1:1 nitric acid aqueous solution), 2ml of silver nitrate ( 0.1mol / L), add water to dilute to the scale 50ml, after standing for 20min, take the samp...

Embodiment 2

[0040] Except for the following differences, all the others were measured by the same method as that of Example 1 to measure the electrolyte sample of Example 2.

[0041] ① Drawing of working curve

[0042] Pipette 4ml of the prepared trivalent and tetravalent vanadium electrolytes into a 100ml beaker, add a certain amount of sulfur-phosphorus mixed acid, then add potassium permanganate dropwise to oxidize until the solution is reddish, let it stand for 5min, add 5ml of urea, drop 4 ~6 drops of sodium nitrite make the solution yellow, transfer it to a 100ml volumetric flask, shake well, add water to make the solution 100ml.

[0043] Take 25ml of oxidized pentavalent vanadium solution in six 50ml volumetric flasks, add 0mL, 1mL, 2mL, 3mL, 4mL, 5mL of chlorine standard solution, add 2ml of nitric acid, 2ml of silver nitrate, dilute with water to 50ml , after standing still for 20min, take the sample without chlorine standard solution as blank, measure the absorbance of the othe...

Embodiment 3

[0045] Except for the following differences, the same method as that of Example 1 was used to measure the electrolyte sample of Example 3.

[0046] ① Drawing of working curve

[0047] Take 5ml of pure pentavalent vanadium solution in eight 25ml volumetric flasks, add 0mL, 0.5mL, 1mL, 2mL, 3mL, 4mL, 6mL, 8mL chlorine standard solution, add 2ml of nitric acid, 2ml of silver nitrate, dilute with water to the scale, after standing still for 20 minutes, take the sample without chlorine standard solution as blank, measure the absorbance of other 7 samples at the wavelength of 460nm, take the chloride ion concentration as the abscissa, and the corresponding absorbance as the ordinate, draw the work curve, working curve such as figure 2 shown.

[0048] ②Use a spectrophotometer to measure the absorbance of the sample

[0049] Use a pipette to accurately pipette 5mL of pentavalent vanadium electrolyte solution into a 25mL volumetric flask, add 2mL of nitric acid in turn and shake we...

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Abstract

The invention relates to a method for determining trace chlorine ions in a vanadium electrolyte. The method comprises (A) oxidizing a vanadium electrolyte sample into pentavalent vanadium and simultaneously diluting the sample by a certain factor to obtain a pentavalent vanadium ion electrolyte, (B) putting the pentavalent vanadium ion electrolyte as a substrate solution into a colorimetric tube,adding nitric acid into the electrolyte, carrying out acidification, and adding a silver nitrate solution into the electrolyte, adding water to dilute the mixed solution and carrying out volume metering to obtain a test solution, or directly adding water to dilute the acidified electrolyte and carrying out volume metering to obtain a test solution, (C) drawing a working curve and checking a linearcorrelation coefficient of the working curve at the same time, and (D) determining the absorbance of the test solution with the silver nitrate solution obtained in step the (B), calculating the corresponding chlorine concentration through the blank test solution without the silver nitrate solution based on the absorbance according to the linear equation, and multiplying the chlorine concentrationby the dilution factor to obtain the chloride ion concentration of the vanadium electrolyte. The method can fast and accurately detect the trace chlorine ion content of the vanadium electrolyte, is easy to operate and needs unharsh experimental conditions.

Description

technical field [0001] The invention relates to a method for determining chloride ions in a vanadium electrolyte. Background technique [0002] The vanadium redox flow battery system consists of stacks, electrolyte solutions, electrolyte solution storage and supply systems, system control systems, charge and discharge systems and other parts. The core part of the system is the electrolyte and the stack. The electrolyte is composed of vanadium ions in different valence states and a certain concentration of sulfuric acid. The electrolyte circulates in the stack and flows on the porous electrodes on both sides of the ion exchange membrane. Reduction and oxidation reactions occur separately. The presence of certain impurity ions in the electrolyte will seriously affect the stability of the electrolyte, the charge and discharge efficiency of the battery, the rate of capacity decay and the life of the stack. Chloride ions are an important impurity element in the vanadium electro...

Claims

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Application Information

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IPC IPC(8): G01N21/3577
CPCG01N21/3577
Inventor 王远望官清
Owner 湖南汇锋高新能源有限公司
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