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Electrochemical method of detecting trace heavy metal by using walnut shell-based carbon material modified glassy carbon electrode

A technology of trace heavy metals and glassy carbon electrodes, which is applied in the electrochemical field of heavy metal ion detection, can solve the problems that the performance of heavy metal ions has not been significantly improved, real-time online detection cannot be applied, and the preparation of samples takes a long time to achieve stable pores. structure, saving manpower and material resources, and low cost

Active Publication Date: 2019-06-14
SHIHEZI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Problems and defects of the prior art: Although the existing methods have good selectivity and high sensitivity, the equipment required by these methods is expensive, the equipment is large in size, unfavorable for carrying, and the preparation of samples takes a long time. The operation is complex, requires professional detection and cannot be applied to real-time online detection of heavy metal ions
At present, the commonly used modified electrode materials include graphene, multi-walled carbon nanotubes, metal nano-ions, metal oxides, etc. However, the performance of the sensors prepared based on the above-mentioned materials has not been significantly improved for the detection of heavy metal ions, and the material synthesis Complexity and high cost limit their practical application

Method used

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  • Electrochemical method of detecting trace heavy metal by using walnut shell-based carbon material modified glassy carbon electrode
  • Electrochemical method of detecting trace heavy metal by using walnut shell-based carbon material modified glassy carbon electrode
  • Electrochemical method of detecting trace heavy metal by using walnut shell-based carbon material modified glassy carbon electrode

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Experimental program
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Effect test

Embodiment 1

[0027] Preparation of carbon materials by carbonization activation method:

[0028] a. After walnut shells are simply pulverized, soak them in hydrochloric acid with a concentration of 1mol / L for 24 hours to remove cellulose impurities in the biomass, then pulverize them with a pulverizer, and pass through an 80-mesh sieve for sieving and grinding;

[0029] b. Put the material obtained in step a in the ark, and under the protection of nitrogen, heat it in a tube furnace at 3°C / min to 300°C, keep it warm for 2 hours, and take it out after cooling;

[0030] c. Mix and grind the material obtained in step b with the activator potassium hydroxide at a mass ratio of 1:6, place the sample in a high-temperature tube furnace, and raise the temperature to 500°C at a rate of 3°C / min under the protection of nitrogen , keep warm for 3 hours, then cool down to room temperature at the same rate;

[0031] d. The sample obtained in step c is successively washed with deionized water and ethano...

Embodiment 2

[0038] Preparation of carbon materials by carbonization activation method:

[0039] a. After walnut shells are simply pulverized, soak in hydrochloric acid with a concentration of 5mol / L for 24 hours to remove impurities such as cellulose in the biomass, then pulverize with a pulverizer, and pass through a 200-mesh sieve for sieving and grinding;

[0040] b. Place the material obtained in step a in the ark, and under the protection of argon, heat it in a tube furnace at 10°C / min to 900°C, keep it warm for 2 hours, and take it out after cooling;

[0041] c. Mix and grind the material obtained in step b with the zinc chloride activator at a mass ratio of 1:2, place the sample in a high-temperature tube furnace, and raise the temperature to 900 °C at a rate of 10 °C / min under the protection of argon. ℃, keep warm for 1 hour, then cool down to room temperature at the same rate;

[0042] d. The sample obtained in step c is successively washed with deionized water and ethanol by su...

Embodiment 3

[0049] Preparation of carbon materials by carbonization activation method:

[0050] a. After the walnut shells are simply pulverized, soak in hydrochloric acid with a concentration of 3mol / L for 24 hours to remove impurities such as cellulose in the biomass, then pulverize with a pulverizer, and pass through a 100-mesh sieve for sieving and grinding;

[0051] b. Put the material obtained in step a in the ark, and under the protection of nitrogen or argon, heat it in a tube furnace at 5°C / min to 400°C, keep it warm for 2 hours, and take it out after cooling;

[0052] c. Mix and grind the material obtained in step b with the calcium chloride activator at a mass ratio of 1:5, place the sample in a high-temperature tube furnace, and raise the temperature to 600°C at a heating rate of 5°C / min under the protection of nitrogen , keep warm for 2 hours, then cool down to room temperature at the same rate;

[0053] d. The sample obtained in step c is successively washed with deionized ...

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Abstract

The invention discloses an electrochemical method of detecting trace heavy metal by using walnut shell-based carbon material modified glassy carbon electrode. The method comprises steps of preparing biomass porous carbon with walnut shell as a raw material through high temperature carbonization and activation by an activator, modifying the walnut shell-based carbon material on the surface of the glassy carbon electrode, and performing trace detection on heavy metal ions like Cu<2+>, Hg<2+>, Pb<2+> and Cd<2+> by using an electrochemical differential pulse anodic stripping voltammetry method. The biomass porous carbon prepared by the method has advantages of large specific surface area, rich pores, and more surface defects. The method can highly selectively detect heavy metal ions like Cu<2+>, Hg<2+>, Pb<2+> and Cd<2+>, and has advantages of high detection flexibility, high stability, high anti-interference, and wide detection linear range, thereby meeting actual industrial requirements.

Description

technical field [0001] The invention relates to the field of preparation of electrochemical sensors for heavy metal ion detection, and specifically discloses an electrochemical method for heavy metal ion detection using walnut shells as raw materials, carbonization and activation. Background technique [0002] At present, the traditional methods used to detect heavy metal ions mainly include atomic fluorescence spectrometry, atomic absorption spectrometry, inductively coupled plasma emission spectrometry, inductively coupled plasma mass spectrometry, high performance liquid chromatography, ultraviolet-visible spectrometry and other methods. Problems and defects of the prior art: Although the existing methods have good selectivity and high sensitivity, the equipment required by these methods is expensive, the equipment is large in size, unfavorable for carrying, and the preparation of samples takes a long time. The operation is complicated, professional personnel are required...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N27/48
Inventor 陈龙赵泽玉郭旭虹付海海史玉琳范长春李昊泉杨建昊
Owner SHIHEZI UNIVERSITY
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