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Electrochemical sensor electrode capable of simultaneously detecting heavy metal lead and cadmium ions in grains

A sensor electrode and electrochemical technology, which is applied in the field of electrochemical sensor electrodes and their preparation, can solve the problems of cumbersome preparation of bismuth-coated film electrodes, insufficient reproducibility, etc., and achieves improved optimal condition control, detection reproducibility, and low cost. , the effect of the consistency of test results

Active Publication Date: 2021-02-12
FUZHOU UNIV
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Problems solved by technology

In order to solve the problems of cumbersome preparation and insufficient reproducibility of traditional bismuth-coated film electrodes, the present invention uses carbon nitride nanosheets to load bismuth sphere composite nanomaterials to modify the electrode interface, effectively increasing the specific surface area, adsorption and coordination of the sensing electrode. And electrical conductivity, improve the detection sensitivity, reproducibility and selectivity of the sensor, low cost, can be used for simultaneous rapid detection of lead and cadmium in grain samples

Method used

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  • Electrochemical sensor electrode capable of simultaneously detecting heavy metal lead and cadmium ions in grains
  • Electrochemical sensor electrode capable of simultaneously detecting heavy metal lead and cadmium ions in grains
  • Electrochemical sensor electrode capable of simultaneously detecting heavy metal lead and cadmium ions in grains

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Embodiment 1

[0027] This embodiment provides a method for preparing a carbon nitride nanosheet-loaded bismuth sphere composite nanomaterial, and the specific steps are as follows:

[0028] (1) Preparation of carbon nitride nanosheets by acid exfoliation method: 60.0 mL 0.2 M HNO 3Add 1.0 g melamine in 20.0 mL ethanol solution, stir for 10 min, wash with ethanol and dry at 60 °C for 12 h. After the obtained white solid was ground, it was calcined at 450 °C for 2 h in an air atmosphere with a heating rate of 10 °C / min. Finally, a light yellow solid is obtained, which is carbon nitride nanosheets.

[0029] (2) Bi / g-C 3 N 4 Preparation of composite nanomaterials: 0.364 g bismuth nitrate pentahydrate solid was completely dissolved in 10 mL1 M HNO 3 , stirred vigorously in a stainless steel reactor. After dissolving, add 55 mL of ethylene glycol, stir at room temperature for 10 min, then add 0.6 g of PVP, and continue stirring for 30 min. After the solid was completely dissolved, different...

Embodiment 2

[0032] This embodiment also provides a method for constructing heavy metal lead and cadmium electrochemical sensor electrodes using carbon nitride nanosheets loaded with bismuth ball composite nanomaterials and applying them to electrochemical detection. The specific construction and detection steps are as follows:

[0033] (1) Bi / g-C 3 N 4 Preparation of composite nanomaterial dispersion: weigh 1.0 mg of Bi / g-C prepared in Example 1 3 N 4 Composite nanomaterials (Bi / CN 200), dispersed with 1.0 mL of secondary water, sonicated for 30 min, then allowed to stand for 10 min; the supernatant was diluted 10 times to obtain 0.1 mg / mL Bi / g-C 3 N 4 Composite nanomaterial dispersion.

[0034] (2) Bi / g-C 3 N 4 / GCE sensor electrode preparation: Glassy carbon electrodes (GCE, φ=3 mm) were prepared with α-Al 2 o 3 Powder (0.05 μm, 0.3 μm) was polished to a mirror surface, then cleaned with ethanol and secondary water in turn, and dried with nitrogen. Take 10 μL of the composite n...

Embodiment 3

[0040] According to the national food safety standards for lead and cadmium (GB 5009.12-2017, GBT 5009.15-2014), the microwave digestion instrument was used to digest and pretreat grain samples such as rice, millet and corn; after filtering the obtained grain digestion solution, add 1M NaOH was adjusted to pH 4.7, then with 0.1 mol L -1 Acetic acid-sodium acetate buffer solution (pH 4.7) was diluted to 50 mL, and the carbon nitride nanosheet-loaded bismuth sphere composite nanomaterial electrochemical sensor prepared in Example 1 was used for square wave anodic stripping voltammetry under optimal conditions. .

[0041] As a method control for the determination of lead and cadmium, the obtained grain digestion solution was filtered, adjusted to pH 7.0 by adding 1 M NaOH, and then diluted to 50 mL with secondary water, and then subjected to ICP-MS (national food safety standard GB 5009.268-2016 ) detection.

[0042] The experimental results showed that lead and cadmium ion con...

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Abstract

The invention discloses an electrochemical sensor electrode capable of simultaneously detecting heavy metal lead and cadmium ions as well as a preparation method and application of the electrochemicalsensor electrode. A glassy carbon electrode is modified by a carbon nitride nanosheet loaded bismuth sphere composite nano material synthesized by hydrothermal reaction through a drop-coating methodto construct a sensor electrode sensitive interface; and simultaneous square wave anodic stripping voltammetry detection of trace lead and cadmium ions is realized. The defects of traditional mercury-plated film and bismuth film electrodes in the aspect of preparation or detection reproducibility are overcome, the specific surface area and the adsorption capacity of the electrode are increased through the sensing interface modified carbon nitride nanosheet, the good electro-catalytic performance is achieved, and meanwhile by means of the combination effect of bismuth balls and heavy metal ions, the lead ion and cadmium ion selective enrichment capacity of the sensor is improved, the response sensitivity to lead ions and cadmium ions is high, the selectivity is good, the detection linear range is wide, and the sensor is suitable for simultaneous, rapid and quantitative detection of heavy metal lead and cadmium ions in grain samples.

Description

technical field [0001] The invention belongs to the technical field of electrochemical sensors, in particular to an electrochemical sensor electrode capable of simultaneously detecting heavy metal ions of lead and cadmium and a preparation method thereof. The sensor is suitable for rapid detection of heavy metal ions in food safety and environmental fields. Background technique [0002] With the rapid development of urbanization and industrialization, food and food pollution problems caused by excessive heavy metal emissions are emerging in an endless stream. Lead and cadmium, as the two most toxic heavy metals to the human body announced by the Food and Agriculture Organization of the United Nations (FAO) and the World Health Organization (WHO), are currently the most common food heavy metal pollutants. The pollution and toxic effects of the two are often synergistic, and accumulation in the human body through the food chain can cause chronic poisoning and many diseases. W...

Claims

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Application Information

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IPC IPC(8): G01N27/30G01N27/48
CPCG01N27/308G01N27/48
Inventor 吴晓苹满苏宁张翼
Owner FUZHOU UNIV
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