CN115308284B - Cadmium ion detection electrode based on electrochemiluminescence, preparation method and application thereof - Google Patents
Cadmium ion detection electrode based on electrochemiluminescence, preparation method and application thereof Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 44
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 239000011701 zinc Substances 0.000 claims abstract description 22
- 239000011787 zinc oxide Substances 0.000 claims abstract description 20
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 19
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 10
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 10
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000004070 electrodeposition Methods 0.000 claims abstract description 6
- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 6
- 239000012498 ultrapure water Substances 0.000 claims abstract description 6
- -1 sulfur ion Chemical class 0.000 claims abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 3
- 239000011593 sulfur Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 claims description 6
- 229910001488 sodium perchlorate Inorganic materials 0.000 claims description 6
- 238000002484 cyclic voltammetry Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000004073 vulcanization Methods 0.000 claims description 5
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 22
- 230000035945 sensitivity Effects 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 4
- GTKRFUAGOKINCA-UHFFFAOYSA-M chlorosilver;silver Chemical compound [Ag].[Ag]Cl GTKRFUAGOKINCA-UHFFFAOYSA-M 0.000 description 3
- 238000002795 fluorescence method Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/301—Reference electrodes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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Abstract
The invention provides a cadmium ion detection electrode based on electrochemiluminescence, which comprises the following steps: polishing the glassy carbon electrode by using alumina suspension, cleaning by using ultrapure water, and drying to obtain a substrate electrode; after zinc is deposited on the surface of a substrate electrode through electrodeposition, standing in air, and oxidizing the zinc deposited on the surface of the electrode into zinc oxide by oxygen in the air to obtain a zinc oxide modified electrode; placing the zinc oxide modified electrode in a sulfur ion solution for standing to obtain a zinc sulfide modified electrode, namely a working electrode; the detection electrode comprises the working electrode, a reference electrode and a counter electrode. The invention also provides an electrochemiluminescence type cadmium ion detection method. The preparation of the detection electrode and the detection of cadmium ions thereof have the characteristics of simple operation, no harm, no easy interference by other ions and the like.
Description
Technical Field
The invention belongs to the field of testing or analyzing materials by utilizing an optical means, and particularly relates to a cadmium ion detection electrode based on electrochemiluminescence, a preparation method and application thereof.
Background
The existing analysis methods for cadmium ions (Cd 2+) mainly comprise atomic absorption spectrometry, inductively coupled plasma mass spectrometry, spectrophotometry and the like. The method has the advantages of mature technology, low detection limit, high sensitivity and the like, but still requires expensive large-scale instruments, and limits the wide application of the method. In contrast, fluorescence and electrochemical methods have received much attention for their convenience, low cost and high sensitivity characteristics. However, fluorescence methods are often limited by noisy backgrounds, limiting the detection sensitivity of fluorescence methods and their applications. The electrochemical method has the advantages of being quick, sensitive, low in cost and the like, and toxic heavy metals such as Hg 2+、Bi3+、Sb3+ are often used as a substrate in detection, so that Cd 2+ is effectively deposited on the electrode to realize detection, and popularization and application of the method are limited.
In view of the foregoing, there is a need to develop a method for detecting cadmium ion Cd 2+ that is simple and harmless to operate and is not susceptible to interference from other ions.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to overcome the technical drawbacks of the prior art, such as complex detection operation, low sensitivity, and high component of Cd 2+;
The invention also aims to solve the technical problem that the prior art needs to use toxic heavy metals such as Hg 2+、Bi3+ or Sb 3+ as a substrate to bring secondary pollution when detecting Cd 2+;
to achieve the above and other related objects, the present invention provides a method for preparing a cadmium ion detection electrode based on electrochemiluminescence, comprising the steps of:
Step 1, preparing a substrate electrode: polishing the glassy carbon electrode by using alumina suspension, cleaning by using ultrapure water, and drying to obtain a substrate electrode;
Step 2, zinc deposition: after zinc is deposited on the surface of a substrate electrode through electrodeposition, standing in air, and oxidizing the zinc deposited on the surface of the electrode into zinc oxide by oxygen in the air to obtain a zinc oxide modified electrode;
Step 3, vulcanization modification: and placing the zinc oxide modified electrode in a sulfur ion solution for standing to obtain a zinc sulfide modified electrode, namely a working electrode, wherein the detection electrode comprises the working electrode, a reference electrode and a counter electrode.
Preferably, the method comprises the following steps:
Step 1, preparing a substrate electrode: polishing the glassy carbon electrode by using alumina suspension with the particle size of 0.5 mu m, cleaning by using ultrapure water, and drying to obtain the substrate electrode
Step 2, zinc deposition: immersing a substrate electrode into a Zn 2+ solution with the concentration of 1-5 mmol/L, depositing for 10s under the voltage of-1.4V, depositing zinc on the surface of the substrate electrode through electrodeposition, standing in the air for 6-10 min, and oxidizing the zinc deposited on the surface of the electrode into zinc oxide by oxygen in the air to obtain a zinc oxide modified electrode;
Step 3, vulcanization modification: placing the zinc oxide modified electrode in 5-20 mmol/L Na 2 S solution, standing for 5-15 min to obtain a zinc sulfide modified electrode, namely a working electrode; the detection electrode comprises the working electrode, a reference electrode and a counter electrode.
Preferably, the reference electrode is a silver chloride electrode, and the counter electrode is a platinum sheet electrode.
Preferably, the particle size of the zinc nano-particles on the surface of the zinc oxide modified electrode is 10-20 nm.
The cadmium ion detection electrode based on electrochemiluminescence is prepared by adopting the preparation method.
The application of the cadmium ion detection electrode is that the cadmium ion detection electrode is placed in a solution to be detected containing cadmium ions, an electrochemiluminescence signal of the cadmium ions is obtained through electrochemical scanning, and the concentration of the cadmium ions in the solution to be detected is obtained through conversion calculation of the intensity of the electrochemiluminescence signal obtained through measurement.
Preferably, the cadmium ion detection electrode is placed in a solution to be detected containing cadmium ions for 20-30 min, an electrochemiluminescence signal of the cadmium ions is obtained through electrochemical scanning, and the concentration of the cadmium ions in the solution to be detected is obtained through conversion calculation of the intensity of the electrochemiluminescence signal obtained through measurement.
Preferably, the electrochemical scanning mode is cyclic voltammetry, the scanning range is 0-1.5V, and the scanning speed is 0.05V/s.
Preferably, the components of the solution to be detected containing cadmium ions comprise H 2O2、NaClO4 and Cd 2+.
Preferably, the components of the solution to be detected containing cadmium ions comprise 2-5 mmol/L H 2O2、0.1~0.5mol/L NaClO4 and Cd 2+ with different concentrations.
The cadmium ion detection electrode based on electrochemiluminescence, the preparation method and the detection method have the following beneficial effects:
1) According to the invention, the Cd 2+ in the solution is rapidly detected by preparing the zinc sulfide nanoparticle modified electrode and generating a strong ECL (electrogenerated chemilumines electrochemiluminescence) signal by utilizing the displacement reaction of Cd 2+ and the surface of the zinc sulfide modified electrode, and compared with the prior art, the method has the advantages of simple operation, high sensitivity and almost zero background interference, and can realize rapid and sensitive detection of Cd 2+ in water;
2) The method does not need to introduce Hg 2+、Bi3+ or Sb 3+ and other toxic heavy metals as a substrate to prepare the electrode, and does not cause secondary pollution.
Drawings
FIG. 1 is a schematic diagram of detection electrode preparation and detection of Cd 2+;
FIG. 2 is a scanning electron microscope image of zinc sulfide nanoparticles modified on the surface of the working electrode in accordance with the present invention;
FIG. 3 is a graph of electrochemiluminescence signals of a test solution with and without Cd 2+ added to a detection electrode according to the present invention;
FIG. 4 is a graph of electrochemiluminescence signals of the detection electrode pair of the present invention at different concentrations Cd 2+;
FIG. 5 is a graph of electrochemiluminescence signals of the detection electrode pair of the present invention for different metal ions.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described by the following specific examples.
Example 1:
the preparation method of the cadmium ion detection electrode based on electrochemiluminescence comprises the following steps:
Step 1, preparing a substrate electrode: polishing the glassy carbon electrode by using alumina suspension with the particle size of 0.5 mu m, cleaning by using ultrapure water, and drying to obtain a substrate electrode;
step 2, zinc deposition: immersing a substrate electrode into a Zn 2+ solution with the concentration of 1-5 mmol/L, depositing for 10s under the voltage of-1.4V, depositing zinc on the surface of the substrate electrode through electrodeposition, standing in the air for 6-10 min, and oxidizing the zinc deposited on the surface of the electrode into zinc oxide by oxygen in the air to obtain a zinc oxide modified electrode;
Step 3, vulcanization modification: placing the zinc oxide modified electrode in a 10mmol/L Na 2 S solution and standing for 5-15 min to obtain a zinc sulfide modified electrode, namely a working electrode; the detection electrode comprises the working electrode, a reference electrode and a counter electrode; as shown in fig. 1 and 2. The reference electrode is a silver chloride electrode, and the counter electrode is a platinum sheet electrode.
Example 2:
the detection electrode (using silver-silver chloride electrode as reference electrode and platinum sheet electrode as counter electrode) in example 1 was placed in a solution containing Cd 2+ and not containing Cd 2+, and the electrochemiluminescence signal of Cd 2+ was monitored by electrochemical scanning, wherein the electrochemical scanning was cyclic voltammetry, the scanning range was 0-1.5V, the scanning speed was 0.05V/s, and the cycle was two; the composition of the solution to be detected containing Cd 2+ is 2mmol/L H 2O2、0.1mol/L NaClO4 and Cd 2+ of 5X10 -7 mol/L, and the control group is as follows: the composition of the solution to be tested, which does not contain Cd 2+, is 2mmol/L H 2O2、0.1mol/LNaClO4.
In the solution to be detected containing Cd 2+, because CdS of a strong electrochemiluminescence signal is generated on the surface of the electrode (working electrode) modified by the zinc sulfide nano particles, the obvious electrochemiluminescence signal is obtained; in the test solution containing no Cd 2+, no CdS was generated, so no obvious electrochemiluminescence signal could be obtained, as shown in fig. 3.
Example 3:
The detection electrode (silver-silver chloride electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode) in the embodiment 1 is placed in a solution to be detected containing Cd 2+ with different concentrations, and electrochemiluminescence signals are monitored through electrochemical scanning, as shown in fig. 4, wherein the electrochemical scanning is cyclic voltammetry, the scanning range is 0-1.5V, the scanning speed is 0.05V/s, the solution to be detected containing Cd 2+ with different concentrations is circulated for two circles, and the composition of the solution to be detected containing Cd 2+ with different concentrations is 2mmol/L H 2O2、0.1mol/L NaClO4 and Cd 2+ with different concentrations.
Example 4:
placing the detection electrode (silver-silver chloride electrode is used as a reference electrode and a platinum sheet electrode is used as a counter electrode) in the embodiment 1 in a plurality of solutions to be detected containing different metal ions, and monitoring electrochemiluminescence signals through electrochemical scanning, as shown in fig. 5, wherein the electrochemical scanning is cyclic voltammetry, the scanning range is 0-1.5V, the scanning speed is 0.05V/s, and the two circles are circulated; as can be seen from the test chart of FIG. 5, the method has electrochemiluminescence signals only for the solution to be tested containing Cd 2+; the electrochemiluminescence signal is not detected for the solution to be detected containing other kinds of metal ions, so that the interference of the other kinds of metal ions to the method is avoided, and the detection method has good selectivity to Cd 2+.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. The preparation method of the cadmium ion detection electrode based on electrochemiluminescence is characterized by comprising the following steps of:
Step 1, preparing a substrate electrode: polishing the glassy carbon electrode by using alumina suspension, cleaning by using ultrapure water, and drying to obtain a substrate electrode;
Step 2, zinc deposition: after zinc is deposited on the surface of a substrate electrode through electrodeposition, standing in air, and oxidizing the zinc deposited on the surface of the electrode into zinc oxide by oxygen in the air to obtain a zinc oxide modified electrode;
Step 3, vulcanization modification: placing the zinc oxide modified electrode in a sulfur ion solution for standing to obtain a zinc sulfide modified electrode, namely a working electrode; the detection electrode comprises the working electrode, a reference electrode and a counter electrode.
2. The method for preparing the cadmium ion detection electrode based on electrochemiluminescence according to claim 1, comprising the following steps:
Step 1, preparing a substrate electrode: polishing the glassy carbon electrode by using alumina suspension with the particle size of 0.5 mu m, cleaning by using ultrapure water, and drying to obtain a substrate electrode;
step 2, zinc deposition: immersing a substrate electrode into a Zn 2+ solution with the concentration of 1-5 mmol/L, depositing for 10s under the voltage of-1.4V, depositing zinc on the surface of the substrate electrode through electrodeposition, standing in the air for 6-10 min, and oxidizing the zinc deposited on the surface of the electrode into zinc oxide by oxygen in the air to obtain a zinc oxide modified electrode;
Step 3, vulcanization modification: placing the zinc oxide modified electrode in 5-20 mmol/L Na 2 S solution, standing for 5-15 min to obtain a zinc sulfide modified electrode, namely a working electrode; the detection electrode comprises the working electrode, a reference electrode and a counter electrode.
3. The method for preparing a cadmium ion detection electrode based on electrochemiluminescence according to claim 1 or 2, wherein the reference electrode is a silver chloride electrode and the counter electrode is a platinum sheet electrode.
4. The method for preparing a cadmium ion detection electrode based on electrochemiluminescence according to claim 3, wherein the particle size of the zinc nanoparticle on the surface of the zinc oxide modified electrode is 10-20 nm.
5. A cadmium ion detection electrode based on electrochemiluminescence, characterized in that the cadmium ion detection electrode is prepared by the preparation method of claim 4.
6. The application of the cadmium ion detection electrode is characterized in that the cadmium ion detection electrode in claim 5 is placed in a solution to be detected containing cadmium ions, and an electrochemiluminescence signal of the cadmium ions is obtained through electrochemical scanning.
7. The use according to claim 6, wherein the cadmium ion detection electrode is placed in a solution to be detected containing cadmium ions for 20-30 min, and the electrochemiluminescence signal of the cadmium ions is obtained by electrochemical scanning.
8. The use according to claim 7, wherein the electrochemical scanning mode is cyclic voltammetry, the scanning range is 0-1.5V, and the scanning speed is 0.05V/s.
9. The use of claim 8, wherein the components of the solution to be tested containing cadmium ions include H 2O2、NaClO4 and Cd 2+.
10. The use according to claim 9, wherein the components of the solution to be measured containing cadmium ions comprise 2-5 mmol/L H 2O2、0.1~0.5mol/L NaClO4 and different concentrations of Cd 2+.
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