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Method of electrochemically measuring permanganate index by virtue of stannic oxide nanometer electrode

A permanganate index, nano-electrode technology, applied in the direction of electrochemical variables of materials, can solve the problems of cumbersome operation, depend on accuracy and reproducibility, and lack of sensitivity, and achieve high measurement accuracy and high current efficiency. , the effect of easy operation

Active Publication Date: 2011-10-12
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

This method has the following problems: (1) analysis time (comprising boiling water bath time and titration time) reaches more than half an hour; (2) consumes chemicals and energy; (3) operation is more loaded down with trivial details, and the accuracy of experimental result and reproduction Depending on the skill level of the operator
This method can quickly and accurately measure the chemical oxygen demand (COD) in simulated samples and actual wastewater. Cr ), but its sensitivity does not meet the requirements for the determination of permanganate index, and the electrode used is based on PbO 2 As the main active component, it will cause secondary pollution

Method used

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  • Method of electrochemically measuring permanganate index by virtue of stannic oxide nanometer electrode
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  • Method of electrochemically measuring permanganate index by virtue of stannic oxide nanometer electrode

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Effect test

Embodiment 1

[0026] Embodiment 1, measure the permanganate index of different concentration glucose solution

[0027] Ti / SnO 2 The nanorod array electrode is the working electrode, and the working electrode area is 3.0cm 2 , the preparation parameters are: SnCl 4 Concentration is 0.12mol / L, solid mass ratio SnCl 4 .5H 2 The ratio of O: NaOH was 1 / 1, and the reaction time was 18 hours; with the platinum plate as the counter electrode and the saturated calomel electrode as the reference electrode, the applied potential was 1.95V, and under the condition of magnetic stirring, the sulfuric acid of 15mL and 0.1mol / L Standard test solutions with different permanganate indices were added to the sodium solution, and the generated current signals were recorded, measured in parallel three times, and a calibration curve of the response current value and the permanganate index of the standard sample was obtained by fitting, with a correlation coefficient of 0.99. Under the same test conditions, gl...

Embodiment 2

[0028] Embodiment 2, measure the permanganate index of certain reservoir water sample

[0029] Ti / SnO 2The nanorod array electrode is the working electrode, and the working electrode area is 1.5cm 2 , the preparation parameters are: SnCl 4 Concentration is 0.06mol / L, solid mass ratio SnCl 4 .5H 2 O: NaOH is 4 / 5, and the reaction time is 16 hours; with platinum sheet as the counter electrode and silver / silver chloride electrode as the reference electrode, under the condition of applying potential 1.7V and magnetic stirring, to 10mL, 0.08mol / L Standard test solutions with different permanganate indices were added to the sodium sulfate solution, and the current signals generated were recorded. Each sample was measured in parallel three times, and the calibration curve of the response current value and the permanganate index of the standard sample was obtained by fitting. The correlation coefficient is 0.975. Under the same test conditions, the average permanganate index of t...

Embodiment 3

[0030] Embodiment 3, measure the permanganate index of certain reservoir water sample

[0031] The working electrode area is 3.0cm 2 , the preparation parameters are: SnCl 4 Concentration is 0.12mol / L, solid mass ratio SnCl 4 .5H 2 O:NaOH is 1 / 1, and the reaction time is 18h; the platinum plate is used as the counter electrode, the saturated calomel electrode is used as the reference electrode, and the applied potential is 1.95V. Standard test solutions with different permanganate indices were added to the sodium solution, and the generated current signals were recorded, measured in parallel three times, and a calibration curve of the response current value and the permanganate index of the standard sample was obtained by fitting, with a correlation coefficient of 0.993. Under the same test conditions, the average permanganate index of the reservoir water sample was measured to be 5.2mg / L, and the relative standard deviation was 3.9%. Compared with the standard potassium pe...

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Abstract

The invention belongs to the technical field of environmental monitoring and relates to a method of measuring a permanganate index of a cleaner water body by utilizing an electrochemical method, wherein the method is characterized in that a stannic oxide nanometer electrode which utilizes metal titanium as a substrate and has a surface in a nanometer stick array structure is utilized as working electrode, the stannic oxide nanometer electrode is prepared by utilizing a hydrothemal method to cause SnCl4.5 H2O and NaOH which are utilized as precursors to react on the metal titanium substrate at180-200 DEG C for 16-24 hours; a working voltage when in electrochemical measurement is respectively 1.7-2.2 V when a saturated silver / chlorinated silver electrode is utilized as a reference electrode and 1.65-2.15 V when a saturated calomel electrode is utilized as a reference electrode, the concentration of sodium sulfate or sodium nitrate in the electrolyte solution is 0.08-0.4 mol / L. According to the invention, no toxic materials can be generated when in measurement, and the method provided by the invention has the advantages of high measurement accuracy, low detection limit, permanganateindex detection lower limit up to 0.2 mg / L (S / N=3), simplicity and convenience in operation and short single measurement time less than 5 minutes.

Description

technical field [0001] The invention belongs to the technical field of environmental monitoring, and relates to a method for measuring the index of organic matter pollution in relatively clean water bodies—permanganate index—by an electrochemical method. Background technique [0002] Permanganate index is a commonly used indicator to reflect the degree of organic pollution in clean or relatively clean water, and has become one of the must-test indicators in water environment monitoring. In recent years, my country's seven major water systems and three major lakes have been polluted to varying degrees, resulting in a shortage of drinking water resources and deterioration of water quality. Therefore, it is very important to establish a simple, rapid, cheap and non-toxic method for the determination of permanganate index in order to grasp the changing law of permanganate index in time, understand the pollution of surface water quality, and find abnormalities as soon as possible...

Claims

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Application Information

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IPC IPC(8): G01N27/26G01N27/30
Inventor 全燮刘艳明赵慧敏陈硕
Owner DALIAN UNIV OF TECH
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