Preparation of bismuth membrane electrode

A bismuth film electrode and glassy carbon electrode technology, applied in the field of electrodes, can solve the problems of poor selectivity of glassy carbon electrodes, and achieve the effects of high sensitivity, short test process and simple operation.

Inactive Publication Date: 2010-05-12
烟台海岸带可持续发展研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since it came out in 2000, it has gradually become a research hotspot, but

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  • Preparation of bismuth membrane electrode
  • Preparation of bismuth membrane electrode
  • Preparation of bismuth membrane electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] After polishing the glassy carbon electrode, sweep cyclic voltammetry (about 20 times) in 0.5M sulfuric acid solution until the electrode reaches a stable state, and then dry it for later use.

[0016] 1% by weight of Nafion (diluted with superior pure anhydrous ethanolamine weight ratio) and ionophore with a molar concentration of 2mmol / L (using chromatographically pure tetrahydrofuran as solvent) were calculated as 1:1 ultrasonic Mix well for 30 minutes, then drop 3 μL onto the surface of the spare glassy carbon electrode above, dry at room temperature, and finally blow with hot air for 1 min to harden, cool to room temperature and place it in a Bi solution containing 1000 μg / L (III) In the acetic acid-sodium acetate buffer solution of pH 4.5, the Ag / AgCl electrode is used as the reference electrode, the platinum electrode is used as the counter electrode, and the bismuth film electrode is used as the working electrode, and a potential of -1.2V is applied under the con...

Embodiment 2

[0019] Using the electrode prepared by the present invention to measure lead in seawater is an example.

[0020] Seawater pretreatment: first filter with a filter membrane with a diameter of 0.45 μm, then place the filtrate under a high-pressure mercury lamp for digestion for 50 minutes, and then adjust the pH to 4.5 with 0.1M acetate buffer.

[0021] Measurement process:

[0022] 1) Take the bismuth film electrode prepared in Example 1 as the working electrode, insert it into the pretreated seawater containing 1000 μg / L Bi(III), and enrich it with a potential of -1.2V for 180s under the condition of stirring so that Both bismuth and lead are deposited on the electrode surface. The Ag / AgCl electrode (inner filled with 3M KCl) is used as the reference electrode, and the platinum electrode is used as the counter electrode, and then the potential remains unchanged for 15s, and then the differential pulse voltammetry is used to scan forward from -1.0V to -0.3V, during this proce...

Embodiment 3

[0028] The electrode prepared by the invention is used to measure the concentration of lead in a solution with tin present.

[0029] When measuring lead ions using a bismuth film electrode, the elution peak of tin present in the solution often overlaps with lead, which interferes with the measurement of lead. Adopt electrode of the present invention and existing bismuth film electrode to measure the concentration (referring to Table 1) of the solution lead of identical concentration lead and tin (molar concentration is 5nM),

[0030] Table 1

[0031]

[0032] As can be seen from Table 1, on the existing bismuth film electrode, when only lead exists, its stripping peak current is 33.06nA, but when lead and tin two kinds of ions exist in solution simultaneously, peak current is then 11.04nA, reduces nearly two-thirds, indicating that tin seriously interferes with the determination of lead. And under the same situation, on the electrode of the present invention, the strippin...

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Abstract

The invention relates to an electrode, in particular to a chemically modified bismuth membrane electrode. The bismuth membrane electrode is prepared by the following steps: mixing Nafion and ionophore according to the volume fraction of 1:1-1:1.5, and conducting ultrasound on the mixture for 20-40min to be uniform, then dripping the mixture to the surface of glassy carbon electrode polished cleanly, drying the mixture at room temperature, subsequently hardening the mixture by blowing hot air to the mixture, after the mixture cools to room temperature, putting the glassy carbon electrode to acetic acid-sodium acetate buffer solution which contains 100-1, 500mug/L Bi(III) and has the pH being 4.5, and applying -1.2V electric potential under stirring situation for 180s of deposition and enrichment. The electrode is simple in making, small, exquisite and nimble, wherein the sensitivity is up to 31.38nA/Nm, the detection limit can be up to 4.4 multiplied by 10-11M. The electrode can be used in the application fields such as environmental monitoring, food security and clinical detection and the like with simple operation and short test process, and can also be used for detecting the content of heavy metal in seawater, fresh water, blood, urine samples and vegetables.

Description

technical field [0001] The invention relates to an electrode, in particular to a chemically modified bismuth film electrode. Background technique [0002] Stripping voltammetry has become a highly sensitive electrochemical analysis method due to the combination of effective pre-concentration and electrochemical detection technology, and the key to using this method is to choose a suitable modification material. For a long time, mercury films and mercury dropping electrodes have been widely used for their high sensitivity, low background current, wide potential window, good reproducibility and easy surface renewal. However, as we all know, mercury is a toxic metal that will pollute the environment and endanger people's health, so it is urgent to find corresponding substitutes. The performance of bismuth film electrodes can be compared with mercury, and bismuth is a green, non-toxic and environmentally friendly metal. Since it came out in 2000, it has gradually become a rese...

Claims

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Application Information

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IPC IPC(8): G01N27/30
Inventor 秦伟王元娥潘大为
Owner 烟台海岸带可持续发展研究所
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