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Sensitive electrode for direct electrochemical detection of ammonia nitrogen in water and preparation method of sensitive electrode

A sensitive electrode and electrochemical technology, applied in the field of electrochemical sensing, can solve the problems of inability to appear oxidation peaks, cumbersome process, high ammonia oxidation potential, etc., and achieve complex detection process, uniform particle size, and high anti-interference Effect

Inactive Publication Date: 2019-11-29
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the shortcomings are also obvious. The detection product contains mercury, which is toxic. If it is not handled properly, it will cause secondary pollution to the water body.
The salicylic acid method avoids the secondary pollution of the water body and has high detection sensitivity. However, due to the complicated detection steps and cumbersome process, and the need to transport water samples to laboratories and other places for detection, it is difficult to ensure Consistency, it is difficult to achieve fast and accurate detection of ammonia nitrogen
[0005] Existing detection methods also include electrochemical detection. Among them, the electrode for electrochemical detection of ammonia nitrogen designed based on the ammonia gas-sensing electrode method has a wide range of applications. The ammonia-gas-sensing electrode method is simple to operate and has high accuracy, but the electrolysis in the electrode The liquid and semipermeable membrane need to be replaced frequently. In addition, the ammonia gas sensitive electrode method belongs to the secondary detection of ammonia, rather than direct detection. The root cause is that the oxidation potential of ammonia is too high, and the oxidation peak cannot appear in the conventional potential window, making it difficult to direct detection

Method used

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  • Sensitive electrode for direct electrochemical detection of ammonia nitrogen in water and preparation method of sensitive electrode
  • Sensitive electrode for direct electrochemical detection of ammonia nitrogen in water and preparation method of sensitive electrode
  • Sensitive electrode for direct electrochemical detection of ammonia nitrogen in water and preparation method of sensitive electrode

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The preparation method of the sensitive material suitable for direct electrochemical ammonia nitrogen detection in water body is as follows:

[0034] a) Cut the carbon cloth into 0.5cm×1cm, ultrasonically clean it with toluene, acetone, ethanol, deionized water, and hydrochloric acid for 10 minutes, and finally clean it with deionized water for use;

[0035] b) Prepare 3.5mM H 2 PtCl 4 and 0.5mM NiSO 4 The mixed aqueous solution is used as the electrolyte;

[0036] c) Electrochemical deposition is carried out using a three-electrode system. The carbon cloth obtained in step a) is used as the working electrode, the platinum sheet electrode is used as the counter electrode, and the Ag / AgCl electrode is used as the reference electrode. Cyclic voltammetry is used, and the potential interval is -0.8 ~0.6V, the number of scanning cycles is 15, and the scanning speed is 10mv / s to obtain the Pt-Ni / carbon cloth electrode material. Dry in a 40°C oven for 2 hours.

[0037] d)...

Embodiment 2

[0039] A) the cleaning process of carbon cloth is as embodiment 1;

[0040] b) other conditions remain unchanged, 3mM H 2 PtCl 4 and 1mM NiSO 4 mixed aqueous solution as electrolyte;

[0041] c) Electrochemical deposition was carried out using a three-electrode system, with carbon cloth as the working electrode, platinum sheet electrode as the counter electrode, and Ag / AgCl electrode as the reference electrode. Cyclic voltammetry was used with the potential range of -0.8 to 0.6V. The number of laps is 15 laps, and the scanning speed is 10mv / s to obtain the Pt-Ni / carbon cloth electrode material, and the electrode is placed in a 40°C oven to dry for 2 hours before use.

[0042]d) The test process is the same as in Example 1, and the test results show that the sensitivity of the electrode prepared by the inventive method to ammonia nitrogen detection is 11.435mA cm -2 mM -1 .

Embodiment 3

[0044] A) the cleaning process of carbon cloth is as embodiment 1;

[0045] b) Other conditions remain unchanged, 2.5mM H 2 PtCl 4 and 1.5mM NiSO 4 mixed aqueous solution as electrolyte;

[0046] c) A three-electrode system is used for electrochemical deposition, with carbon cloth as the working electrode, platinum sheet electrode as the counter electrode, and Ag / AgCl electrode as the reference electrode. Cyclic voltammetry is used with the potential range of -0.8 to 0.6, and the scanning circle The number is 15 cycles, and the sweep speed is 10mv / s to obtain the Pt-Ni / carbon cloth electrode material, and the electrode is placed in a 40°C oven to dry for 2 hours before use.

[0047] d) The test process is the same as in Example 1, and the test results show that the sensitivity of the electrode prepared by the method of the present invention to the detection of ammonia nitrogen is 12.72mA cm -2 mM -1 .

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Abstract

The invention discloses a sensitive electrode for direct electrochemical detection of ammonia nitrogen in water and a preparation method of the sensitive electrode and belongs to the field of electrochemical sensing technologies. According to the preparation method, a carbon material is used as a supporting electrode, and the carbon material is subject to ultrasonic cleaning in a cleaning solutionafter being cut; then, a mixed aqueous solution of a fourth-period transition metal compound and a sixth-period transition metal compound is used as an electrolytic solution to deposit bimetal on thesurface of the carbon material through an electrochemical deposition method; next, drying is performed for 1.5-3.0h under the condition of 30-50 DEG C to obtain the sensitive electrode; and last, thesensitive electrode is used for detecting the ammonia nitrogen in the water under a three-electrode system. Through the preparation method, the sensitive electrode capable of realizing rapid and direct detection of the ammonia nitrogen is successfully prepared, the defects of detection process complexity, poor detection timeliness and the like are relieved to some extent, and the sensitive electrode has the advantages of high sensitivity, high anti-interference, environment-friendliness and the like.

Description

technical field [0001] The invention belongs to the technical field of electrochemical sensing, in particular to a sensitive electrode for direct electrochemical detection of ammonia nitrogen in water and a preparation method thereof. Background technique [0002] With the rapid development of my country's economy, industry and agriculture, the unreasonable use of a large number of chemical fertilizers and pesticides, as well as the large discharge of industrial wastewater and domestic sewage, have made rivers, lakes and other water bodies more and more polluted. Among them, ammonia nitrogen and phosphorus are the main pollutants leading to eutrophication of water bodies, which are highly toxic to aquatic organisms, especially aquatic fish larvae. Therefore, it is necessary to directly and quickly detect ammonia nitrogen in water bodies. [0003] Ammonia nitrogen in water is represented by free ammonia (NH 3 ) or ammonium salt (NH 4+ ) form, which is one of the total contr...

Claims

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Application Information

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IPC IPC(8): G01N27/48G01N27/30
CPCG01N27/308G01N27/48
Inventor 索辉彭晓雷张良孙邦宁赵纯
Owner JILIN UNIV
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