CN115047053A - Preparation method of bismuth-containing screen-printed electrode and application of bismuth-containing screen-printed electrode in heavy metal ion detection - Google Patents
Preparation method of bismuth-containing screen-printed electrode and application of bismuth-containing screen-printed electrode in heavy metal ion detection Download PDFInfo
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- CN115047053A CN115047053A CN202210389562.4A CN202210389562A CN115047053A CN 115047053 A CN115047053 A CN 115047053A CN 202210389562 A CN202210389562 A CN 202210389562A CN 115047053 A CN115047053 A CN 115047053A
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- 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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- 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
Abstract
A preparation method of a bismuth-containing screen printing electrode and application thereof in heavy metal ion detection belong to the technical field of screen printing electrode preparation. In order to solve the problem that the existing method needs to additionally modify materials on the surface of an electrode or add bismuth ions into a solution when detecting cadmium ions, the method comprises the following steps: adding 1g-2g of bismuth powder into 10g of carbon ink, and mechanically stirring for 10-20min to obtain modified carbon ink doped with the bismuth powder; taking 0.5g-2g of conductive silver paste by a scraper plate, slightly scraping the conductive silver paste, printing the conductive silver paste on a screen printing plate, and curing for 10-20min at 60 ℃; and (3) taking the modified carbon ink by a scraper plate, printing the modified carbon ink on a screen printing plate printed with silver wires by lightly scraping the modified carbon ink for two times, curing the modified carbon ink for 10-20min at the temperature of 60 ℃, coating the joint of the wires and the working electrode by using an insulating tape, and carrying out insulating treatment to obtain the bismuth-containing screen printing electrode. According to the invention, the sensitivity of heavy metal cadmium ion detection can be improved after the bismuth-based metal modified carbon ink is used for preparing the screen-printed electrode.
Description
Technical Field
The invention belongs to the technical field of screen printing electrode preparation, and particularly relates to a preparation method of a bismuth-containing screen printing electrode and application of the bismuth-containing screen printing electrode in heavy metal ion detection.
Background
At present, the electrochemical method for detecting heavy metal ions by using a screen printing electrode mostly adopts the mode of additionally modifying MOFs (organic metal frameworks), nano materials and the like on the surface of the electrode to increase the specific surface area of the electrode, or adds bismuth ions into a solution to be detected, so that the enrichment and dissolution of the metal ions on the surface of the electrode are promoted. At present, the screen printing electrode with larger specific surface area is directly prepared, and a cadmium ion concentration detection method which can reach the national drinking water standard is not reported.
Disclosure of Invention
The invention provides a preparation method of a bismuth-containing screen printing electrode and application thereof in heavy metal ion detection, aiming at solving the problem that the existing method needs to additionally modify materials on the surface of the electrode or add bismuth ions into a solution when detecting cadmium ions.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a bismuth-containing screen-printed electrode, which comprises the following steps:
step one, preparing modified carbon ink:
adding 1g-2g of bismuth powder into 10g of carbon ink, and mechanically stirring the mixture for 10-20min by using a mechanical stirrer to obtain modified carbon ink doped with the bismuth powder; the modified carbon ink is prepared from bismuth powder;
step two, preparing a screen printing electrode:
taking 0.5g-2g of conductive silver paste by using a disposable scraper plate, printing the conductive silver paste on a screen printing plate by the disposable scraper plate and the screen printing plate at an angle of 45 degrees and slightly scraping the conductive silver paste from top to bottom, and curing for 10-20min at 60 ℃; and (2) taking a small amount of the modified carbon ink obtained in the first step by using a disposable scraper, printing the modified carbon ink on a screen printing plate printed with a silver wire, wherein the disposable scraper and the screen printing plate form an angle of 45 degrees, slightly scraping the modified carbon ink from top to bottom, printing the modified carbon ink on the screen printing plate, curing the modified carbon ink for 10-20min at the temperature of 60 ℃, coating the joint of the wire and a working electrode by using an insulating tape, and performing insulation treatment to obtain the bismuth-containing screen printing electrode.
Further, in the second step, the screen printing plate is a PET plate.
The application of the prepared bismuth-containing screen printing electrode in heavy metal ion detection is as follows: and (3) placing the prepared screen-printed electrode in a three-electrode system with saturated calomel as a reference electrode and a platinum wire as a counter electrode to detect cadmium ions.
Further, the detection limit of the heavy metal cadmium ions is 4.80 mu g/L.
Further, the pH value of the heavy metal detection is 4.0.
Further, the deposition voltage for heavy metal detection is-1.0V.
Further, the deposition time for heavy metal detection is 150 s.
Compared with the prior art, the invention has the following advantages:
1. the invention can directly apply the electrode to the research of the detection aspect of the heavy metal cadmium ions in a three-electrode system.
2. According to the invention, the sensitivity of heavy metal cadmium ion detection can be improved after the bismuth-based metal modified carbon ink is used for preparing the screen-printed electrode.
3. The screen-printed electrode prepared from the bismuth-based metal modified carbon ink can be used for directly detecting trace cadmium ions in a water sample, and the detection limit is 4.80 mug/L.
Drawings
FIG. 1 is a process for preparing a screen printed electrode;
FIG. 2 is a finished view of a screen printed electrode prepared;
FIG. 3 is an SEM image of a bismuth-containing screen printed electrode;
FIG. 4 is a mapping view of the working electrode portion of a bismuth-containing screen printed electrode;
FIG. 5 is a comparison of anodic stripping voltammograms for Bare screen printed electrodes (Bare-SPE) and screen printed electrodes prepared with modified carbon ink (Bi-SPE) with a cadmium ion concentration of 50 μ g/L in solution.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
a method for preparing a screen printing electrode based on bismuth-based material modified carbon ink and application of the screen printing electrode in heavy metal ion detection are disclosed. As shown in fig. 1 and fig. 2, the specific implementation steps are as follows:
step one, preparation of modified ink:
10g of the ink and 1.5g of bismuth powder were added to a container, and mechanically stirred for 10 min.
Step two, preparing a screen printing electrode:
(1) and (3) putting 1g of conductive silver paste on a 250-mesh screen printing plate, slightly scraping the plate with a disposable sterile scraper, carrying out primary lead printing on the front side close to the PET plate, putting the PET plate printed with the leads into an oven, and curing for 10min at 60 ℃.
(2) And (3) taking 1g of uniformly stirred modified carbon ink on a screen printing plate, lightly scraping the modified carbon ink on the screen printing plate by using a disposable sterile scraper, enabling the front surface of the modified carbon ink to be close to the PET plate and be aligned with the joint of the electrode and the lead, carrying out primary electrode printing, putting the PET plate printed with the working electrode into an oven, and curing for 10min at the temperature of 60 ℃.
(3) And cutting the insulating adhesive tape with a proper size, and coating part of the lead and the working electrode so that the working electrode part is exposed to the same electrode area. The obtained electrode is characterized as shown in figures 3 and 4;
step three, electrochemical detection:
and (2) taking the screen-printed electrode prepared in the step two as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire as a counter electrode, carrying out electrochemical detection on 0.1M acetic acid-sodium acetate buffer solution containing 50 mu g/L of cadmium ions and having the pH value of 4.0, wherein the deposition potential is-1.0V, the deposition time is 150s, then carrying out detection by using an anode square wave stripping voltammetry, wherein the voltage range is-1.3 to-0.4V, the sweep rate is 50mV/s, and measuring the voltammetry stripping curves before and after carbon ink modification.
Compared with the stripping voltammetry curves of the electrodes prepared before and after the carbon ink modification, as shown in fig. 5, the peak current value of the screen printing electrode with the carbon ink modified is obviously increased compared with the screen printing electrode without the carbon ink modified, because the bismuth powder is doped, the effective surface area of the working electrode of the screen printing electrode is increased, more active sites are possessed, and more cadmium ions are enriched on the surface of the working electrode.
Example 2:
a method for preparing a bismuth-containing screen-printed electrode and application thereof in heavy metal ion detection are disclosed, wherein carbon ink doped with bismuth powder is used as a raw material, the prepared screen-printed electrode is used as a working electrode, and the linear range and the detection limit of heavy metal cadmium ions are measured. As shown in fig. 1 and fig. 2, the specific implementation steps are as follows:
step one, preparation of modified ink:
adding 10g of printing ink and 2g of bismuth powder into a container, and mechanically stirring for 10 min;
step two, preparing a screen printing electrode:
(1) and (3) putting 2g of conductive silver paste on a 250-mesh screen printing plate, slightly scraping the plate with a disposable sterile scraper, carrying out primary lead printing on the front side close to the PET plate, putting the PET plate printed with the leads into an oven, and curing for 10min at 60 ℃.
(2) And (3) taking 2g of uniformly stirred modified carbon ink on a screen printing plate, slightly scraping the modified carbon ink on the plate by using a disposable sterile scraper, attaching the front side of the modified carbon ink to the PET plate, aligning the PET plate with the connection part of the electrode and the lead, printing the electrode for the first time, putting the PET plate printed with the working electrode into an oven, and curing for 10min at the temperature of 60 ℃.
(3) And cutting the insulating adhesive tape with a proper size, and coating part of the lead and the working electrode so that the working electrode part is exposed to the same electrode area.
Step three, electrochemical detection:
and (2) taking the screen-printed electrode prepared in the step two as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire as a counter electrode, carrying out electrochemical detection on a 0.1M acetic acid-sodium acetate buffer solution containing 5 mu g/L-50 mu g/L cadmium ions and having the pH value of 4.0, wherein the deposition potential is-1.0V, the deposition time is 150s, obtaining the maximum peak current under the conditions, then carrying out detection by using an anodic square wave stripping voltammetry, wherein the voltage range is-1.3V-0.4V, the sweep rate is 50mV/s, and measuring the stripping voltammetry curves of the screen-printed electrode in cadmium ion solutions with different concentrations.
The electrode can detect trace cadmium (5 mu g/L) in a water sample, the peak current of the stripping voltammetry curve is increased along with the increase of the concentration of a solution to be detected, and the peak current of the stripping voltammetry curve is linearly fitted, and the peak current of the stripping voltammetry curve is linearly related to the concentration of cadmium ions. And calculating the detection limit of the electrode to be 4.80 mug/L, which accords with the national cadmium ion content standard in drinking water.
Claims (7)
1. A method for preparing a bismuth-containing screen printing electrode is characterized by comprising the following steps: the method comprises the following steps:
step one, preparing modified carbon ink:
adding 1g-2g of bismuth powder into 10g of carbon ink, and mechanically stirring for 10-20min to obtain modified carbon ink doped with bismuth powder;
step two, preparing a screen printing electrode:
taking 0.5g-2g of conductive silver paste by a scraper plate, slightly scraping the conductive silver paste, printing the conductive silver paste on a screen printing plate, and curing for 10-20min at 60 ℃; and (2) taking a small amount of the modified carbon ink obtained in the first step by using a scraper, slightly scraping the modified carbon ink for two times, printing the modified carbon ink on a screen printing plate printed with a silver wire, curing the modified carbon ink for 10-20min at the temperature of 60 ℃, coating the joint of the wire and a working electrode by using an insulating adhesive tape, and carrying out insulating treatment to obtain the bismuth-containing screen printing electrode.
2. The method for preparing the bismuth-containing screen-printed electrode according to claim 1, wherein the method comprises the following steps: in the second step, the screen printing plate is a PET plate.
3. The application of the bismuth-containing screen-printed electrode prepared according to the claim 1 or 2 in heavy metal ion detection is characterized in that: the screen printing electrode is used for detecting heavy metal cadmium ions in a water body, and specifically comprises the following steps: and (3) placing the prepared screen-printed electrode in a three-electrode system with saturated calomel as a reference electrode and a platinum wire as a counter electrode to detect cadmium ions.
4. The application of the bismuth-containing screen-printed electrode in heavy metal ion detection according to claim 3, characterized in that: the detection limit of the heavy metal cadmium ions is 4.80 mug/L.
5. The application of the bismuth-containing screen-printed electrode in heavy metal ion detection according to claim 3, characterized in that: the pH value for heavy metal detection is 4.0.
6. The application of the bismuth-containing screen-printed electrode in heavy metal ion detection according to claim 3, characterized in that: the deposition voltage for heavy metal detection is-1.0V.
7. The application of the bismuth-containing screen-printed electrode in heavy metal ion detection according to claim 3, characterized in that: the deposition time for the heavy metal detection was 150 s.
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| CN202210389562.4A CN115047053A (en) | 2022-04-13 | 2022-04-13 | Preparation method of bismuth-containing screen-printed electrode and application of bismuth-containing screen-printed electrode in heavy metal ion detection |
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| KR20000000811A (en) * | 1998-06-03 | 2000-01-15 | 박종만 | Mercury oxide modified electrode of screen print type |
| KR20080101648A (en) * | 2007-05-16 | 2008-11-21 | 한국원자력연구원 | Water quality sensor detecting heavy metal and method of manufacturing the same |
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| CN104267086A (en) * | 2014-10-14 | 2015-01-07 | 深圳大学 | Chemically modified carbon paste electrode as well as preparation method and application thereof |
| CN110320256A (en) * | 2019-06-27 | 2019-10-11 | 广州钰芯传感科技有限公司 | A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for measuring micro lead in water |
| CN110333276A (en) * | 2019-06-28 | 2019-10-15 | 广州钰芯传感科技有限公司 | A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for fast detection of trace cadmium |
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2022
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