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Preparation method of electrochemical sensor for trace lead ion detection

A lead ion and electrochemical technology, applied in the field of preparation of electrochemical sensing, can solve the problems of complex preparation and low cost, and achieve the effect of simple preparation, low cost and controllable structure

Active Publication Date: 2018-12-11
普瑞丰环保科技(武汉)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This kind of working electrode modification material (microporous covalent organic framework) has high stability and repeatability, but the preparation is complicated and the cost is not low (T. Zhang et al., Talanta, 2018, Vol.188, p578-583)

Method used

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  • Preparation method of electrochemical sensor for trace lead ion detection
  • Preparation method of electrochemical sensor for trace lead ion detection
  • Preparation method of electrochemical sensor for trace lead ion detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A preparation method for electrochemical sensing of trace lead ion detection, the specific process is shown in figure 1 :

[0030] Gelatin-sodium carboxymethylcellulose-polysiloxane carboxylate prepared by the complex coacervation method (specifically refer to "Highblades spreadability of chlorpyrifos microcapsules prepared with polysiloxanesodium carboxylate / sodium carboxymethylcellulose / gelatin via complexcoacervation") after freeze-drying , see figure 2 a), from figure 2 In a, it can be seen that the uniform microporous structure of the microcapsules; under nitrogen protection, carbonization at 650°C for 8 hours, see figure 2 b, from figure 2 b It can be seen that the microcapsules shrink after carbonization, the pore size becomes smaller, and the specific surface area is larger. Take 2mg of carbonized microcapsule powder and ultrasonically disperse it in 2mL of 1mg / mL chitosan acetic acid solution, the mass fraction of acetic acid solution is 5%; take 5μL of...

Embodiment 2

[0032] The gelatin-carboxymethylcellulose sodium-sodium lauryl sulfate microcapsules prepared by the complex coacervation method were freeze-dried and carbonized at 600°C for 10 hours under the protection of nitrogen; 2 mg of the carbonized microcapsule powder was ultrasonically dispersed in In the chitosan acetic acid solution of 4mL 1mg / mL, the mass fraction of acetic acid solution is 1.0%; Take 5 μ L of carbonized microcapsule dispersion liquid as electrode material and modify the glassy carbon electrode after the surface is polished and ultrasonically cleaned, as the working electrode, The platinum sheet is used as the counter electrode, and the silver / silver chloride is used as the reference electrode to form a three-electrode system; Pb(CH 3 COO) 2The electrolyte solution is added to the ammonia gas-ammonium chloride buffer solution with a pH value of 5 to form a 5mL test solution; the three-electrode system is inserted into the test solution, and the -1.0V constant volt...

Embodiment 3

[0034] The gelatin-carboxymethylcellulose sodium-bis(2-ethylhexyl)sodium sulfosuccinate microcapsules prepared by the complex coacervation method were freeze-dried and carbonized at 800°C for 5 hours under nitrogen protection; 5 mg of the carbonized Ultrasonic dispersion of microcapsule powder in 1mL1mg / mL chitosan acetic acid solution, the mass fraction of acetic acid solution is 0.5%; take 5μL of carbonized microcapsule dispersion as electrode material to modify the surface of the glassy carbon electrode after polishing and ultrasonic cleaning , as the working electrode, the platinum sheet as the counter electrode, and the silver / silver chloride as the reference electrode; Pb(NO 3 ) 2 The electrolyte solution is added to the sodium dihydrogen phosphate-disodium hydrogen phosphate buffer solution with a pH value of 4, and the lead ion in the solution to be tested is enriched at a constant voltage of -0.4V, and the enrichment time is 500s; the differential pulse anode strippin...

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Abstract

The invention discloses a preparation method of an electrochemical sensor for trace lead ion detection, belonging to the technical field of environmental detection and analysis. The method comprises the following steps: step 1: enabling gelatin-based microcapsules, which are prepared through a complex coacervation method, to be frozen and dried, and enabling carbonized microcapsule powder to be ultrasonically dispersed in a chitosan acetic acid solution; step 2: taking 5 mu L of carbonized microcapsule dispersion liquid, which is prepared in step 1, to serve as an electrode material so as to modify the surface of a glassy carbon electrode to act as a working electrode; step 3: adding different concentrations of lead ion electrolyte into a buffer solution to form 5 mL of a to-be-tested solution, inserting an electrode system in step 2 into the lead ion electrolyte, and enriching lead ions in the electrolyte at constant voltage; step 4: obtaining the standard curves of peak current values and lead ion concentrations by adopting a differential pulse anodic stripping voltammetry; and step 5: detecting lead ion concentrations in to-be-tested samples. The working electrode modification material prepared by the invention has the advantages of simple preparation, low cost, controllable structure, good repeatability and the like.

Description

technical field [0001] The invention relates to the technical field of environmental detection and analysis, in particular to a preparation method for electrochemical sensing for trace lead ion detection. Background technique [0002] In recent years, with the rapid development of industry, heavy metals have high biological toxicity, and the damage to the environment and human physical and mental health cannot be underestimated. Lead ions have trace toxicity and bioaccumulation, and are classified as Class II carcinogens by the International Agency for Research on Cancer, posing a serious threat to environmental safety and human health. Therefore, a simple, convenient and efficient method for the analysis and detection of lead ions has attracted much attention. [0003] At present, the analysis and detection methods of lead ions include atomic absorption spectrometry, atomic fluorescence spectrometry, biological dye test paper method and electrochemical analysis method. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/48
CPCG01N27/48
Inventor 卢丽敏戴润英胥荃
Owner 普瑞丰环保科技(武汉)有限公司
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