CN111781268A - Voltammetry-based method for detecting heavy metal ions in brackish water - Google Patents
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Abstract
The application discloses detection method of heavy metal ions in brackish water based on voltammetry, which includes: s1, modifying a glassy carbon electrode, namely uniformly coating oxidized graphene on the surface of the glassy carbon electrode, reducing the oxidized graphene to obtain reduced oxidized graphene, depositing zero-valent nano iron on the glassy carbon electrode coated with the reduced oxidized graphene on the surface through electrodeposition, performing surface treatment on the electrodeposited glassy carbon electrode to finish modification of the glassy carbon electrode, and taking the modified glassy carbon electrode as a working electrode; and S2, performing electrochemical analysis by adopting an electrochemical detection three-electrode system and a stripping voltammetry, and simultaneously detecting heavy metal mercury, zinc, cadmium, copper, lead and chromium ions in the brackish water.
Description
Technical Field
The invention relates to a detection method of heavy metal ions, in particular to a detection method of heavy metal ions in brackish water based on voltammetry.
Background
In order to solve the problem of water consumption, fresh water resources in China are scarce, particularly in northern and eastern coastal areas, the rural areas generally drink brackish water, but the brackish water has high hardness, contains a large amount of neutral salt and has high pH value, heavy metal ions in the brackish water are high in content, and gastrointestinal dysfunction and low immunity are caused by long-term drinking of the brackish water, so that the health of residents is seriously threatened. At the present stage, in areas where brackish water is wide step by step, a brackish water purification mode is gradually adopted to fully utilize harmful resources, in the brackish water purification process, detection of heavy metal ions plays a crucial role, accurate data support can be provided for the purification process by detecting the content of the heavy metal ions in the brackish water, energy and resource consumption of the purification process is reduced, and detection of the purified brackish water can ensure that the purification process can accurately reach the standard. The electrochemical stripping voltammetry has the advantages of high sensitivity, simple operation, low cost, low detection limit, quick response and the like, can overcome the problems encountered by the traditional technology, and is a promising heavy metal ion detection method, wherein the anodic stripping voltammetry has high sensitivity and is particularly suitable for the detection of heavy metal ions.
The electrochemical anodic stripping voltammetry for detecting heavy metals comprises two processes of adsorption and stripping of heavy metal ions on a working electrode, in the existing detection method, the types of the heavy metal ions which can be detected simultaneously are very limited, usually at most 4, and the main heavy metal ions in the brackish water are mercury, copper, zinc, lead, cadmium and chromium ions, so that the detection efficiency of the heavy metal ions in the brackish water is severely limited, the detection cost is high, and the method is an important factor influencing the purification of the brackish water.
Disclosure of Invention
The invention aims to provide a detection method of heavy metal ions in brackish water based on voltammetry, aiming at overcoming the defects in the prior art, and the detection sensitivity and detection efficiency of the heavy metal ions can be obviously improved.
In order to achieve the purpose, the invention adopts the following scheme:
a detection method of heavy metal ions in brackish water based on voltammetry comprises the following steps:
s1, modification of glassy carbon electrode: preparing a glassy carbon electrode, uniformly dispersing graphene oxide in an aqueous solution containing chitosan, dropwise coating the aqueous solution of graphene oxide on the surface of the glassy carbon electrode, reducing the graphene oxide to obtain the glassy carbon electrode modified with reduced graphene oxide on the surface, taking the glassy carbon electrode modified with reduced graphene oxide on the surface as a cathode in an iron salt solution, uniformly depositing nano zero-valent iron with the particle size of 50-70 nm on the surface of the glassy carbon electrode modified with reduced graphene oxide on the surface by adopting an electrodeposition method, placing the glassy carbon electrode subjected to electrodeposition in deionized water, standing and reacting for 4 hours at 80 ℃, so that nano iron oxide is generated on the surface of the nano zero-valent iron, finishing the modification of the glassy carbon electrode, and taking the modified glassy carbon electrode as a working electrode;
s2, detection of heavy metal ions: and an electrochemical detection three-electrode system is adopted, electrochemical analysis is carried out by adopting stripping voltammetry, and heavy metal mercury, zinc, cadmium, copper, lead and chromium ions in the brackish water are detected.
Preferably, in step S1, the graphene oxide is uniformly dispersed in the aqueous solution containing chitosan, wherein the mass fraction of the graphene oxide in the aqueous solution is 8 wt% to 10 wt%, and the mass fraction of the chitosan is 1.5 wt%.
Preferably, in step S1, the graphene oxide is reduced by dropping graphene oxide on the surface and drying the electrode, and performing microwave reduction in a protective gas environment, where the microwave power is 1200-1400W and the microwave reduction time is 5-8S.
Preferably, in step S1, the iron salt is specifically ferrous chloride, the solution includes manganese chloride and sodium dodecyl sulfate, the concentration of the ferrous chloride is 200g/L, the concentration of the manganese chloride is 20g/L, the concentration of the sodium dodecyl sulfate is 0.03g/L, and the pH value of the solution is adjusted to 1.8.
Preferably, the electrodeposition method in step S1 is specifically electrodeposition using direct current at a constant current density of 4-6A/cm2The electrodeposition time is 5-8 min.
Preferably, in step S2, selecting anodic stripping voltammetry by using an electrochemical workstation, selecting an enrichment potential of-1.5V to-1.6V, performing i-t enrichment, stirring during the enrichment process, using a platinum wire as a counter electrode, using silver/silver chloride as a reference electrode, connecting one end of the working electrode, the counter electrode and the reference electrode to the electrochemical workstation, respectively, placing the other end of the working electrode, the counter electrode and the reference electrode in an electrolyte in an electrolytic cell, respectively, wherein the electrolyte is an acetic acid-sodium acetate buffer solution containing brackish water, the pH value of the electrolyte is 5, and the concentration of the acetic acid-sodium acetate is 0.2M; and after the i-t enrichment is finished, stopping stirring, applying a forward scanning voltage of-1.4V-0.8V to the working electrode, obtaining a current-voltage curve by an electrochemical workstation, and obtaining the concentration of the heavy metal ions according to the relation between the concentration of the heavy metal ions and the peak current.
Preferably, in step S2, the enrichment time is 100S, and during the enrichment process, electric stirring is performed at a stirring speed of 350 rpm.
Advantageous effects
The detection capability of the glassy carbon electrode is greatly improved by modifying a conventional glassy carbon electrode, firstly, a graphene oxide aqueous solution is uniformly dispersed on the surface of the glassy carbon electrode, so that graphene oxide can be uniformly dispersed on the surface of the glassy carbon electrode, the graphene oxide is reduced to obtain the surface of the glassy carbon electrode in which reduced graphene oxide is uniformly dispersed, secondly, nano zero-valent iron is uniformly deposited on the surface of the glassy carbon electrode modified with the reduced graphene oxide by combining an electrodeposition method, the effective surface area of the glassy carbon electrode is increased by reducing the graphene oxide, the deposition amount of the nano zero-valent iron is increased while the reduced graphene oxide has better adsorption capability and electric conduction capability, and finally, nano iron oxide is prepared under the conditions of temperature and reaction, and after the nano zero-valent iron surface generates sheet iron oxide, by virtue of the adsorption effect of the sheet iron oxide, the adsorption capacity of the glassy carbon electrode on heavy metal ions is remarkably improved, the detection sensitivity is improved, the detection flux is increased, mercury, zinc, cadmium, copper, lead and chromium ions can be detected simultaneously, more accurate data are provided for the detection of the heavy metal ions in the brackish water, the detection time is saved, and a reliable basis is provided for the further desalination and purification treatment of the brackish water.
Drawings
FIG. 1 is a flow chart of the technical scheme of the invention
FIG. 2 is the anodic stripping voltammetry response graph obtained by mercury, zinc, cadmium, copper, lead and chromium ion detection on brackish water in example 3
Detailed Description
Example 1
A detection method of heavy metal ions in brackish water based on voltammetry comprises the following steps:
s1, modification of glassy carbon electrode: preparing a glassy carbon electrode, and uniformly dispersing graphene oxide in an aqueous solution containing chitosan, wherein the mass fraction of the graphene oxide in the aqueous solution is 8 wt%, and the concentration of the chitosan is 1.5 wt%; dropwise coating a graphene oxide aqueous solution on the surface of a glassy carbon electrode, drying, and reducing graphene oxide, specifically, carrying out microwave reduction on the electrode which is dropwise coated with the graphene oxide aqueous solution and dried in a protective gas environment, wherein the microwave power is 1200W, and the microwave reduction time is 5s, so as to obtain the glassy carbon electrode modified with reduced graphene oxide on the surface; uniformly depositing nanometer zero-valent iron with the particle size of 50nm on the surface of a glassy carbon electrode modified with reduced graphene oxide on the surface by an electrodeposition method, wherein the ferric salt is ferrous chloride, the solution comprises manganese chloride and sodium dodecyl sulfate, the concentration of the ferrous chloride is 200g/L, the concentration of the manganese chloride is 20g/L, the concentration of the sodium dodecyl sulfate is 0.03g/L, and the pH value of the solution is adjusted to 1.8; the electrodeposition method specifically comprises the step of performing electrodeposition by using direct current with constant current density of 4A/cm2The electrodeposition time is 5 min; placing the glassy carbon electrode subjected to electrodeposition in deionized water, standing at 80 ℃ for reaction for 4 hours to generate nanoscale iron oxide on the surface of the nanoscale zero-valent iron, finishing the modification of the glassy carbon electrode, and taking the modified glassy carbon electrode as a working electrode;
s2, detection of heavy metal ions: and an electrochemical detection three-electrode system is adopted, electrochemical analysis is carried out by adopting stripping voltammetry, and heavy metal mercury, zinc, cadmium, copper, lead and chromium ions in the brackish water are detected. Specifically, an electrochemical workstation is adopted, an anodic stripping voltammetry is selected, an enrichment potential is selected to be-1.5V-1.6V, i-t enrichment is carried out, wherein the enrichment time is 100s, electric stirring is carried out in the enrichment process, the stirring speed is 350rpm, a platinum wire is adopted as a counter electrode, silver/silver chloride is adopted as a reference electrode, one ends of the working electrode, the counter electrode and the reference electrode are respectively connected to the electrochemical workstation, the other ends of the working electrode, the counter electrode and the reference electrode are respectively placed in electrolyte in an electrolytic cell, the electrolyte is an acetic acid-sodium acetate buffer solution containing brackish water, the pH value of the electrolyte is 5, and the concentration of the acetic acid-sodium acetate is 0.2M; and after the i-t enrichment is finished, stopping stirring, applying a forward scanning voltage of-1.4V-0.8V to the working electrode, obtaining a current-voltage curve by an electrochemical workstation, and obtaining the concentration of the heavy metal ions according to the relation between the concentration of the heavy metal ions and the peak current.
Example 2
A detection method of heavy metal ions in brackish water based on voltammetry comprises the following steps:
s1, modification of glassy carbon electrode: preparing a glassy carbon electrode, and uniformly dispersing graphene oxide in an aqueous solution containing chitosan, wherein the mass fraction of the graphene oxide in the aqueous solution is 9 wt%, and the concentration of the chitosan is 1.5 wt%; dropwise coating a graphene oxide aqueous solution on the surface of a glassy carbon electrode, drying, and reducing graphene oxide, specifically, carrying out microwave reduction on the electrode which is dropwise coated with the graphene oxide aqueous solution and dried in a protective gas environment, wherein the microwave power is 1300W, and the microwave reduction time is 7s, so as to obtain the glassy carbon electrode modified with reduced graphene oxide on the surface; uniformly depositing nanometer zero-valent iron with the particle size of 60nm on the surface of a glassy carbon electrode modified with reduced graphene oxide on the surface by an electrodeposition method, wherein the ferric salt is ferrous chloride, the solution comprises manganese chloride and sodium dodecyl sulfate, the concentration of the ferrous chloride is 200g/L, the concentration of the manganese chloride is 20g/L, the concentration of the sodium dodecyl sulfate is 0.03g/L, and the pH value of the solution is adjusted to 1.8; the electrodeposition method specifically comprises the step of performing electrodeposition by using direct current with constant current density of 5A/cm2The electrodeposition time is 6 min; electrically charging the glassy carbon after electrodepositionPlacing the electrode in deionized water, standing and reacting for 4h at 80 ℃ to generate nanoscale iron oxide on the surface of the nanoscale zero-valent iron, finishing the modification of the glassy carbon electrode, and taking the modified glassy carbon electrode as a working electrode;
s2, detection of heavy metal ions: and an electrochemical detection three-electrode system is adopted, electrochemical analysis is carried out by adopting stripping voltammetry, and heavy metal mercury, zinc, cadmium, copper, lead and chromium ions in the brackish water are detected. Specifically, an electrochemical workstation is adopted, an anodic stripping voltammetry is selected, an enrichment potential is selected to be-1.5V-1.6V, i-t enrichment is carried out, wherein the enrichment time is 100s, electric stirring is carried out in the enrichment process, the stirring speed is 350rpm, a platinum wire is adopted as a counter electrode, silver/silver chloride is adopted as a reference electrode, one ends of the working electrode, the counter electrode and the reference electrode are respectively connected to the electrochemical workstation, the other ends of the working electrode, the counter electrode and the reference electrode are respectively placed in electrolyte in an electrolytic cell, the electrolyte is an acetic acid-sodium acetate buffer solution containing brackish water, the pH value of the electrolyte is 5, and the concentration of the acetic acid-sodium acetate is 0.2M; and after the i-t enrichment is finished, stopping stirring, applying a forward scanning voltage of-1.4V-0.8V to the working electrode, obtaining a current-voltage curve by an electrochemical workstation, and obtaining the concentration of the heavy metal ions according to the relation between the concentration of the heavy metal ions and the peak current.
Example 3
A detection method of heavy metal ions in brackish water based on voltammetry comprises the following steps:
s1, modification of glassy carbon electrode: preparing a glassy carbon electrode, and uniformly dispersing graphene oxide in an aqueous solution containing chitosan, wherein the mass fraction of the graphene oxide in the aqueous solution is 10 wt%, and the mass fraction of the chitosan is 1.5 wt%; dropwise coating a graphene oxide aqueous solution on the surface of a glassy carbon electrode, drying, and reducing graphene oxide, specifically, carrying out microwave reduction on the electrode which is dropwise coated with the graphene oxide aqueous solution and dried in a protective gas environment, wherein the microwave power is 1400W, and the microwave reduction time is 8s, so as to obtain the glassy carbon electrode modified with reduced graphene oxide on the surface; dissolving a glassy carbon electrode modified with reduced graphene oxide on the surface in iron saltUniformly depositing nanometer zero-valent iron with the particle size of 70nm on the surface of a glassy carbon electrode with the surface modified with reduced graphene oxide by adopting an electrodeposition method, wherein a ferric salt is ferrous chloride, the solution comprises manganese chloride and sodium dodecyl sulfate, the concentration of the ferrous chloride is 200g/L, the concentration of the manganese chloride is 20g/L, the concentration of the sodium dodecyl sulfate is 0.03g/L, and the pH value of the solution is adjusted to 1.8; the electrodeposition method specifically comprises the step of performing electrodeposition by adopting direct current with constant current density of 6A/cm2The electrodeposition time is 8 min; placing the glassy carbon electrode subjected to electrodeposition in deionized water, standing at 80 ℃ for reaction for 4 hours to generate nanoscale iron oxide on the surface of the nanoscale zero-valent iron, finishing the modification of the glassy carbon electrode, and taking the modified glassy carbon electrode as a working electrode;
s2, detection of heavy metal ions: and an electrochemical detection three-electrode system is adopted, electrochemical analysis is carried out by adopting stripping voltammetry, and heavy metal mercury, zinc, cadmium, copper, lead and chromium ions in the brackish water are detected. Specifically, an electrochemical workstation is adopted, an anodic stripping voltammetry is selected, an enrichment potential is selected to be-1.5 to-1.6V, i-t enrichment is carried out, wherein the enrichment time is 100s, electric stirring is carried out in the enrichment process, the stirring speed is 350rpm, a platinum wire is adopted as a counter electrode, silver/silver chloride is adopted as a reference electrode, one ends of the working electrode, the counter electrode and the reference electrode are respectively connected to the electrochemical workstation, the other ends of the working electrode, the counter electrode and the reference electrode are respectively placed in electrolyte in an electrolytic cell, the electrolyte is an acetic acid-sodium acetate buffer solution containing brackish water, the pH value of the electrolyte is 5, and the concentration of the acetic acid-sodium acetate is 0.2M; and after the i-t enrichment is finished, stopping stirring, applying a forward scanning voltage of-1.4V-0.8V to the working electrode, obtaining a current-voltage curve by an electrochemical workstation, and obtaining the concentration of the heavy metal ions according to the relation between the concentration of the heavy metal ions and the peak current.
The detection sensitivity, detection limit and linear range of the modified glassy carbon electrodes in the embodiments 1 to 3 are shown in tables 1 to 3, and it can be seen from tables 1 to 3 that the detection effect of the glassy carbon electrode in the embodiment 3 is the best.
TABLE 1
TABLE 2
TABLE 3
FIG. 1 is a flow chart of the technical scheme of the invention
Fig. 2 is an anodic stripping voltammetry response diagram obtained by detecting mercury, zinc, cadmium, copper, lead and chromium ions in brackish water in example 3, and as can be seen from fig. 2, the detection method in the application can realize simultaneous detection of six ions of mercury, zinc, cadmium, copper, lead and chromium in brackish water, and has the advantages of low detection limit, high sensitivity, and significantly improved detection flux and detection efficiency.
The above embodiments are preferred embodiments of the present invention, and those skilled in the art can make variations and modifications to the above embodiments, therefore, the present invention is not limited to the above embodiments, and any obvious improvements, substitutions or modifications made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (7)
1. A detection method of heavy metal ions in brackish water based on voltammetry comprises the following steps:
s1, modification of glassy carbon electrode: preparing a glassy carbon electrode, uniformly dispersing graphene oxide in an aqueous solution containing chitosan, dropwise coating the aqueous solution of graphene oxide on the surface of the glassy carbon electrode, reducing the graphene oxide to obtain the glassy carbon electrode modified with reduced graphene oxide on the surface, taking the glassy carbon electrode modified with reduced graphene oxide on the surface as a cathode in an iron salt solution, uniformly depositing nano zero-valent iron with the particle size of 50-70 nm on the surface of the glassy carbon electrode modified with reduced graphene oxide on the surface by adopting an electrodeposition method, placing the glassy carbon electrode subjected to electrodeposition in deionized water, standing and reacting for 4 hours at 80 ℃, so that nano iron oxide is generated on the surface of the nano zero-valent iron, finishing the modification of the glassy carbon electrode, and taking the modified glassy carbon electrode as a working electrode;
s2, detection of heavy metal ions: and an electrochemical detection three-electrode system is adopted, electrochemical analysis is carried out by adopting stripping voltammetry, and heavy metal mercury, zinc, cadmium, copper, lead and chromium ions in the brackish water are detected.
2. The method of claim 1, wherein in step S1, the graphene oxide is uniformly dispersed in the aqueous solution containing the chitosan, the mass fraction of the graphene oxide in the aqueous solution is 8 wt% to 10 wt%, and the concentration of the chitosan is 1.5 wt%.
3. The method as claimed in claim 1, wherein in step S1, the graphene oxide is reduced by microwave reduction in a protective gas environment at a microwave power of 1200 and 1400W for a period of 5-8S.
4. The method of claim 1, wherein in step S1, the iron salt is ferrous chloride, the solution comprises manganese chloride and sodium dodecyl sulfate, the ferrous chloride concentration is 200g/L, the manganese chloride concentration is 20g/L, the sodium dodecyl sulfate concentration is 0.03g/L, and the pH of the solution is adjusted to 1.8.
5. The method according to claim 1, wherein the electrodeposition method in step S1 is specifically: performing electrodeposition with constant current density Direct Current (DC) at 4-6A/cm2The electrodeposition time is 5-8 min.
6. The method as claimed in claim 1, wherein in step S2, an electrochemical workstation is adopted, anodic stripping voltammetry is selected, the enrichment potential is selected to be-1.5V to-1.6V, i-t enrichment is performed, the enrichment process is stirred, a platinum wire is used as a counter electrode, silver/silver chloride is used as a reference electrode, one ends of the working electrode, the counter electrode and the reference electrode are respectively connected to the electrochemical workstation, the other ends of the working electrode, the counter electrode and the reference electrode are respectively placed in electrolyte in an electrolytic cell, the electrolyte is an acetic acid-sodium acetate buffer solution containing brackish water, the pH value of the electrolyte is 5, and the concentration of the acetic acid-sodium acetate is 0.2M; and after the i-t enrichment is finished, stopping stirring, applying a forward scanning voltage of-1.4V-0.8V to the working electrode, obtaining a current-voltage curve by an electrochemical workstation, and obtaining the concentration of the heavy metal ions according to the relation between the concentration of the heavy metal ions and the peak current.
7. The process according to claim 6, wherein the enrichment time is 100s, and the electric stirring is carried out during the enrichment process, and the stirring speed is 350 rpm.
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