CN115182012A - Preparation method and sensing application of bismuth nanoflower modified electrode - Google Patents
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Abstract
The invention discloses a preparation method of a bismuth nanoflower modified electrode and a sensing application thereof. The bismuth nanoflower is a flower-shaped nano bismuth simple substance which is composed of flaky bismuth crystals as structural units. The preparation method of the bismuth nanoflower comprises the following steps: preparing an acid electroplating solution containing stannous salt and bismuth salt, immersing an electrode in the electroplating solution, electroplating between a bismuth reduction potential and a tin reduction potential by adopting a potentiostatic method, washing, drying, and filling into a sealed bag. The bismuth nanoflower modified electrode is simple in preparation process, strong in microstructure adjustability, high in detection sensitivity and stability and capable of being used for detecting heavy metal ions in an aqueous solution.
Description
Technical Field
The invention relates to the field of heavy metal ion sensing, in particular to a preparation method of a bismuth nanoflower modified electrode and application of the bismuth nanoflower modified electrode in heavy metal ion detection.
Background
Heavy metal ions are a problem which cannot be ignored in environmental pollution monitoring and prevention because of high toxicity, biological accumulation in human, animal and plant tissues and non-biodegradation. The establishment of a rapid, efficient and portable heavy metal ion field detection technology suitable for field environments and sudden polluted fields is a great demand for environmental safety monitoring. Compared with the traditional atomic absorption spectrum and inductively coupled plasma-atomic emission spectrum methods, the electrochemical method has the advantages of low price, high detection speed, high sensitivity, capability of synchronously detecting various heavy metal ions, convenience in carrying of equipment and the like, and is particularly suitable for the detection requirements of the site, the field and the real time.
In electrochemical processes, electrodes are of critical importance. The bismuth electrode has the characteristics of wide negative window, good response sensitivity, dissolved oxygen inertness, undistorted dissolution signal, environmental friendliness and the like since being applied to the electrochemical voltammetry analysis of trace heavy metal ions. The common preparation methods of bismuth electrodes are divided into two types: one is to directly electroplate a bismuth film on an electrode in situ or ex situ, although the time consumption is short and the sensitivity is high, the stability and the reproducibility of electroanalysis are poor because the obtained bismuth is in the conventional shape of needles, rods, trees and the like which are easy to break; the other method is to synthesize bismuth nanoparticles by a solvent thermal method, a sol method, a microwave method and other chemical methods in advance, and then transfer and modify the bismuth nanoparticles onto an electrode by using 'drop coating' or 'bulk doping', wherein the obtained bismuth nanoparticles are mostly spherical with high specific surface, bi nanoparticles with other forms are not developed into a modification material for heavy metal ion detection, the spherical bismuth nanoparticles have the problem of agglomeration, the method needs multiple steps, the consumed time is long, and part of high-temperature and high-pressure reaction conditions have requirements on equipment.
With the intensive research on the bismuth electrode and the improvement of the actual demand, the requirements of high sensitivity, good stability, simple manufacture, low cost and the like are urgently required to be met. If the advantages of the two methods can be combined, the electrochemical method with short time consumption is adopted to directly prepare the bismuth nanoparticles with stable appearance, high specific surface area and good dispersibility on the electrode, and the method is a good choice. Therefore, the preparation method for obtaining the bismuth nanoflower modified electrode through one-step electroplating is provided by the invention, and the bismuth nanoflower modified electrode is applied to detection of lead ions, cadmium ions and zinc ions in water.
Disclosure of Invention
The invention provides a preparation method of a bismuth nanoflower modified electrode and a sensing application thereof.
One of the purposes of the invention is to provide a preparation method for simply and rapidly preparing a flower-shaped nano bismuth modified electrode. The method is realized by the following technical scheme:
selecting a stable carbon-based material electrode as a matrix electrode, such as: graphite felt electrode, graphite flake electrode, preforming carbon electrode (graphite alkene, carbon nanotube, acetylene black), screen printing carbon electrode etc. to but batch production, throwing formula screen printing electrode is very suitable.
Taking a screen printing electrode as an example, the method for modifying flower-shaped nano bismuth particles on the surface of the electrode by one step by adopting a potentiostatic method is described, and the specific operation is as follows: adopting a pretreated screen printing electrode as a three-electrode system (in the screen printing electrode, a working electrode is carbon, a counter electrode is carbon, and a reference electrode is a silver/silver chloride electrode), scanning for more than 10 circles in a 1.5V-1.5V solution at normal temperature by using a cyclic voltammetry method, wherein the scanning speed is preferably 50 mV/s, or immersing the screen printing electrode in 1 to 4 mol/L solution of sulfuric acid in batches and standing overnight for 12 hours; then putting the electrode system into a solution of nitric acid (10 percent by weight) and 1 mol/L potassium chloride which are taken as supporting electrolytes, adding bismuth nitrate and stannous chloride solutions with different concentrations, and depositing at constant potential between the reduction potential of bismuth and the reduction potential of tin to obtain the bismuth nanoflower modified electrode. .
The invention also aims to provide a method for applying the flower-shaped bismuth modified electrode to heavy metal ion detection. The method mainly comprises the following steps: by adopting the bismuth nanoflower modified electrode, the linear relation between the electrochemical signal intensity and the concentration of heavy metal ions (lead, cadmium and zinc) is determined by an electrochemical research method in a solution which takes an acetic acid-sodium acetate buffer solution (pH 5.3) as a supporting electrolyte solution and is added with heavy metal ions (lead, cadmium and zinc) standard solutions with different concentrations, so that a standard curve is obtained. Then, an unknown sample is added into a supporting electrolyte solution of an acetic acid-sodium acetate buffer solution (pH 5.3), the electrochemical signal intensity of the unknown sample is obtained under the same electrochemical test condition, and the concentration of heavy metal ions in the unknown sample is determined according to the standard curve.
The electrochemical method for measuring the heavy metal ions by adopting square wave stripping voltammetry can be adopted, and the specific operations are as follows: setting a negative deposition potential which is preferably equal to or negative than-1.2V, depositing for a certain time under the stirring condition, preferably in the range of 60 s-300 s, then closing the stirring, and balancing for a certain time under the equilibrium potential which is equal to or positive to the deposition potential, preferably in the range of 5-20 s; then, the solution is scanned and dissolved under the conditions of 20 to 50 Hz frequency, 5 mV step voltage and 20 to 50 mV amplitude, preferably not less than-1.2V to-0.4V.
The method can also be used for measuring the heavy metal ions by adopting an electrochemical means of differential pulse voltammetry, and comprises the following specific operations: setting an enrichment potential which is preferably equal to or less than-1.4V, enriching for a certain time under stirring conditions, preferably 60 s-300 s, then closing stirring, and balancing for a certain time under a static potential which is equal to or more than the enrichment potential, preferably 5-20 s; then, the material is scanned and dissolved under the conditions of pulse amplitude of 20-50 mV, pulse width of 40-80 ms, potential increment of 4-10 mV and frequency of 20-50 Hz, and the range of not less than-1.2V to-0.4V is preferred.
Compared with the preparation of the bismuth nanoflower modified electrode by other methods, the preparation method of the bismuth nanoflower modified electrode by adopting the constant potential method has the following advantages:
1. the preparation method is simple in preparation process, short in time consumption and convenient to use. The preparation of the bismuth nanoflower usually needs solvothermal synthesis and calcination, and can not be directly used, and the steps are various and the time is long. The preparation method provided by the invention is feasible at normal temperature, can be obtained in one step, has a simple process and low equipment requirement, and can be directly used in-situ growth.
2. The bismuth nanoflower prepared by the method has strong micro-morphology and size adjustability. The microstructure of the bismuth nanoflower on the screen printing electrode is controlled by bismuth tin components and electroplating conditions, and the diameter of the flower pattern and the size of the inner hole of the flower pattern can be adjusted by adjusting the concentration ratio of bismuth tin, electroplating voltage, electroplating duration and the like.
3. The bismuth nanoflower modified electrode prepared by the method is high in detection stability. The nano bismuth prepared by the conventional electroplating method is generally rod needle and dendritic, is mostly combined with a substrate in a scattered and point mode, and has poor stability. The bottom of the flower-shaped nano bismuth prepared by the method is combined with the substrate in a transverse, regular and surface manner, the combination is firm, and the stability of repeated detection is obviously improved.
Drawings
Fig. 1 is an SEM image of the bismuth nanoflower modified electrode prepared in example 1.
Fig. 2 is an EDS diagram of the bismuth nanoflower modified electrode prepared in example 1.
Fig. 3 is an SEM image of the bismuth nanoflower modified electrode prepared in example 2.
Fig. 4 is a current-concentration standard working curve for detecting lead, cadmium and zinc ions by the bismuth nanoflower modified electrode prepared in example 2.
Fig. 5 is a stripping voltammetry curve for detecting lead, cadmium and zinc ions by repeating the process for 15 times for the bismuth nanoflower modified electrode prepared in example 2.
Detailed Description
Example 1:
(1) Chemical pretreatment of screen-printed electrodes: placing a screen printing carbon electrode (diameter of 3 mm) in a 3 mol/L sulfuric acid solution at normal temperature, standing for 12 h, taking out, washing with water, and drying in the air.
(2) Preparation of electroplating solution: weighing appropriate amount of bismuth nitrate pentahydrate, and adding 10% sodium nitrateAcid preparation of 0.01 mol/L Bi 3+ A stock solution; weighing a proper amount of stannous chloride dihydrate, and preparing 0.01 mol/L Sn by using 10% nitric acid 2+ And (4) stock solution. Remove 14.4 mLBi separately 3+ Stock solution and 8.4 mLSn 2+ The stock solution was mixed with 7.455 g of potassium chloride and made up with 10% nitric acid to 300 mg/L Bi 3+ And 100 mg/L Sn 2+ The plating solution of (1).
(3) Preparing a bismuth nanoflower modified screen printing electrode:immersing the pretreated screen-printed electrode into the electroplating solution, connecting a CHI760E electrochemical workstation, applying a potentiostatic method, setting the deposition potential to-0.35V (vs Ag/AgCl), and depositing for 180 s under stirring. Taking out the electrode, washing, drying, and packaging in a sealed bag. The SEM image and EDS of the bismuth electrode manufactured in this example are shown in fig. 1 and fig. 2, respectively, and it can be seen that the manufactured bismuth contains no Sn atoms, is elemental bismuth, exhibits a nanoporous flower morphology, has a particle diameter of 1.2 μm, is uniform in flower shape, has petals densely stacked by nano bismuth sheets, and has holes of several to tens of nanometers in a staggered configuration.
Example 2:
(1) Electrochemical pretreatment of screen-printed electrodes: placing a screen printing carbon electrode (with the diameter of 3 mm) in 1 mol/L sulfuric acid solution at normal temperature, connecting a CHI760 electrochemical workstation, applying cyclic voltammetry, and circularly scanning for 10 circles at the sweep speed of 1.0V/s within-1.5 to 1.5V.
(2) Preparation of electroplating solution: respectively transferring 9.6 mL of Bi 3+ Stock solution and 12.6 mLSn 2+ The stock solution was mixed with 7.455 g of potassium chloride and made up with 10% nitric acid to 200 mg/L Bi 3+ And 150 mg/L Sn 2+ The plating solution of (1).
(3) Preparing a bismuth nanoflower modified screen printing electrode:immersing the pretreated screen-printed electrode into electroplating solution, connecting CHI760E electrochemical workstation, applying potentiostatic method, setting deposition potential at-0.35V (vs Ag/AgCl), and stirring for deposition for 120 s. Taking out the electrode, washing, drying, and packaging in a sealed bag. The bismuth on the electrode prepared in this example also presents the morphology of a nanoporous flower, as shown in fig. 3, the diameter is about 1.4 μm, and the petals are dense with lamellar nano bismuth as structural unitsAnd the holes of several to dozens of nanometers are formed by the integration and the interlacing.
(4) And (3) standard curve preparation:placing the modified screen printing electrode into Pb with different concentrations 2+ 、Cd 2+ 、Zn 2+ And (4) detecting in the liquid. Setting square wave stripping voltammetry conditions: the stirring was turned on, adsorption was carried out for 180 s at the deposition potential-1.2V, the stirring was turned off, equilibration was carried out for 10 s at the rest potential-1.2V, and dissolution was subsequently scanned from-1.2V to-0.4V at a frequency of 25 Hz, a step voltage of 5 mV, and an amplitude of 50 mV. The dissolution curves of the materials are measured under the same square wave dissolution voltammetry conditions, and as shown in figure 4, the materials show good dissolution response curves in 20-200 mug/L lead ion, cadmium ion solution and 50-500 mug/L zinc ion solution, and the detection limits are respectively 7.5, 7.1 and 18.5 mug/L (S/N = 3).
The stripping voltammetry curves of the electrode prepared in this example for detecting the lead, cadmium and zinc solution in water for 15 times in succession are shown in fig. 5, and the Relative Standard Deviations (RSD) of the response peak current values are 1.92%,3.31% and 4.26%, respectively, and show excellent stability.
Example 3:
(1) Preparation of electroplating solution: respectively transferring 9.6 mL of Bi 3+ Stock solution with 12.6 mLSn 2+ The stock solution was mixed with 7.455 g of potassium chloride and made up with 10% nitric acid to 200 mg/L Bi 3+ And 150 mg/L Sn 2+ The plating solution of (1).
(3) Preparing a bismuth nanoflower modified screen printing electrode:will be provided withElectrochemistry methodImmersing the pretreated screen printing electrode into electroplating solution, connecting CHI760E electrochemical workstation, applying potentiostatic method, setting deposition potential at-0.30V (vs Ag/AgCl), and stirring for deposition for 150 s. Taking out the electrode, washing, drying, and packaging in a sealed bag.
(4) And (3) standard curve preparation:placing the modified screen printing electrode into Pb with different concentrations 2+ 、Cd 2+ 、Zn 2+ And (4) detecting in the liquid. Setting differential pulse voltammetry conditions: starting stirring, adsorbing for 180 s at-1.4V of enrichment potential, closing stirring, balancing for 10 s at-1.4V of rest potential, and then increasing potential by 30 mV, 50 ms of pulse width and 6 ms of potential incrementmV, dissolution was scanned from-1.2V to-0.4V at a frequency of 25 Hz. The response curve is measured under the same differential pulse voltammetry condition.
TABLE 1 spiking recovery test results
(5) And (3) determining the content of lead, cadmium and zinc in the actual water sample:the method comprises the steps of detecting lead, cadmium and zinc ions in tap water by a standard addition method, taking a water sample from laboratory tap water, preparing an acetic acid/sodium acetate buffer solution with the pH value of 5.3 by using the water sample of the laboratory tap water, and preparing lead, cadmium and zinc ion water samples with the pH values of 30 mu g/L, 60 mu g/L and 90 mu g/L by using the buffer solution. The recovery rate measured under the differential pulse voltammetry condition is 94% -104%.
Claims (7)
1. A preparation method of a bismuth nanoflower modified electrode is characterized in that a screen printing electrode is used as a substrate, and flower-shaped nano bismuth particles are modified on the surface of the electrode in one step by an electrochemical method after pretreatment.
2. The electrode pretreatment method according to claim 1, wherein the pretreatment is performed by cyclic voltammetry by the following steps: a screen printing electrode is adopted as a three-electrode system (in the screen printing electrode, a working electrode is carbon, a counter electrode is carbon, and a reference electrode is a silver/silver chloride electrode), then the electrode system is placed in a sulfuric acid solution with the concentration of 0.5 to 2 mol/L, and the electrode system is scanned for more than 10 circles at the normal temperature within the range of-1.5V to 1.5V by using a cyclic voltammetry, wherein the scanning speed is preferably 50 mV/s.
3. The electrode pretreatment method according to claim 1, wherein the pretreatment is carried out chemically by the following steps: and (3) placing the screen printing electrode system in 1-4 mol/L sulfuric acid solution for overnight, and washing for 12 hours.
4. The preparation method of the electrode according to claim 1, wherein the flower-like nano bismuth particles are modified on the surface of the electrode in one step by a potentiostatic method, which comprises the following steps: adopting a pretreated screen printing electrode as a three-electrode system, then placing the electrode system in a solution (10 percent by weight) of nitric acid and 1 mol/L of potassium chloride as supporting electrolytes, adding solutions of bismuth nitrate and stannous chloride with different concentrations, and depositing at constant potential between the bismuth reduction potential and the tin reduction potential to obtain the bismuth nanoflower modified electrode.
5. A sensing application method of a bismuth nanoflower modified electrode comprises the following steps: by adopting the bismuth nanoflower modified electrode, in a solution in which acetic acid-sodium acetate buffer solution (pH 5.3) is used as supporting electrolyte solution and heavy metal ion (lead, cadmium and zinc) standard solutions with different concentrations are added, the linear relation between the electrochemical signal intensity and the heavy metal ion concentration is determined by an electrochemical research method, and a standard curve is obtained; then, an unknown sample is added into a supporting electrolyte solution of an acetic acid-sodium acetate buffer solution (pH 5.3), the electrochemical signal intensity of the unknown sample is obtained under the same electrochemical test condition, and the concentration of heavy metal ions in the unknown sample is determined according to the standard curve.
6. The sensing application method of the bismuth nanoflower modified electrode according to claim 4, wherein a square wave stripping voltammetry is used for determining a linear relation between an electrochemical signal and a heavy metal ion concentration, and the specific operations are as follows: setting a negative deposition potential which is preferably equal to or negative than-1.2V, depositing for a certain time under the stirring condition, preferably in the range of 60 s-300 s, then closing the stirring, and balancing for a certain time under the equilibrium potential which is equal to or positive to the deposition potential, preferably in the range of 5-20 s; then, the sample is scanned and dissolved under the conditions of frequency of 20-50 Hz, step voltage of 5 mV, and amplitude of 20-50 mV, preferably not less than 0.0V to 1.0V.
7. A sensing application method of a bismuth nanoflower modified electrode according to claim 4, wherein a linear relation between an electrochemical signal and a heavy metal ion concentration is determined by adopting a differential pulse voltammetry method, and the specific operations are as follows: setting an enrichment potential which is preferably equal to or less than-1.4V, enriching for a certain time under stirring conditions, preferably 60 s-300 s, then closing stirring, and balancing for a certain time under a static potential which is equal to or more than the enrichment potential, preferably 5-20 s; then, the sample is scanned and dissolved under the conditions of pulse amplitude of 20-50 mV, pulse width of 40-80 ms, potential increment of 4-10 mV and frequency of 20-50 Hz, preferably not less than 0.0V-1.0V.
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| CN116726908A (en) * | 2023-08-14 | 2023-09-12 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Bismuth-doped high-performance electrocatalytic composite material, preparation method and application |
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| CN116726908A (en) * | 2023-08-14 | 2023-09-12 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Bismuth-doped high-performance electrocatalytic composite material, preparation method and application |
| CN116726908B (en) * | 2023-08-14 | 2023-11-10 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Bismuth-doped high-performance electrocatalytic composite material, preparation method and application |
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