CN110231389A - Based on sodium carboxymethylcellulose/bismuth film modified electrode detection cadmium ion method - Google Patents
Based on sodium carboxymethylcellulose/bismuth film modified electrode detection cadmium ion method Download PDFInfo
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- CN110231389A CN110231389A CN201910574194.9A CN201910574194A CN110231389A CN 110231389 A CN110231389 A CN 110231389A CN 201910574194 A CN201910574194 A CN 201910574194A CN 110231389 A CN110231389 A CN 110231389A
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- sodium carboxymethylcellulose
- cadmium
- electrochemical sensor
- bismuth
- constructed based
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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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- 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
- G01N27/333—Ion-selective electrodes or membranes
- G01N27/3335—Ion-selective electrodes or membranes the membrane containing at least one organic component
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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
Abstract
The invention discloses the detection methods that a kind of electrochemical sensor constructed based on sodium carboxymethylcellulose/bismuth film is applied to heavy metal cadmium.The Sensitive Detection of trace heavy metal cadmium ion may be implemented in the electrochemical sensor, and detection method is differential pulse anodic stripping voltammetry, and sedimentation time is 120 ~ 180 s, and sedimentation potential is -1.0 ~ -1.3 V, and the detection range of linearity is 0.05 ~ 10 μM.Electrochemical sensor preparation is easy, while showing preferable reproducibility, repeatability and interference free performance, is expected to the heavy metal cadmium ion being applied in detection actual water sample product.
Description
Technical field
The invention belongs to electrochemical sensors and heavy metal analysis field, are related to a kind of based on sodium carboxymethylcellulose/bismuth
The method for the electrochemical sensor detection heavy metal cadmium that film is constructed.
Background technique
With industrialized rapid development, the pollution of heavy metal also becomes increasingly severe.Cadmium pollution can provide big gas and water
Source and agricultural production have an adverse effect, and migrate and be enriched with by food chain, and human body is caused Itai-itai diseases, cancer etc. occur.
In the 1960s, related cadmium pollution and its bioavailability problems increasingly cause full generation after " Itai-itai diseases " occurs in Japan
The concern on boundary.Heavy metal cadmium non-degradable in the natural environment can enter human body by food chain after being enriched in vivo and draw
Slow poisoning is played, carcinogenic risk is increased.Cadmium ion is regarded as a kind of carcinogen by international cancer research institution.With warp
The development of Ji and the raising of living standards of the people, people increasingly focus on the monitoring of environmental protection and environmental pollution, so research
Develop sensitive, quick, accurate, the convenient method of one kind and real-time accurate detection is carried out to trace heavy metal ion, and then is stringent
Control monitoring drinking water, the heavy metal cadmium ion concentration in food, to holding for protection food safety and human health and environment
Supervention exhibition has very important significance.
Since 2000, bismuth film electrode is used to replace mercury film modified electrode as the sensor for detecting heavy metal ion
It receives more and more attention, the electrochemical sensor detection heavy metal ion based on bismuth film is widely answered
With.
Sodium carboxymethylcellulose is that glucose polymerization degree is 100-2000 cellulose derivative, oxygen-containing function rich in
Group, can form strong complex compound with heavy metal, to be applied to quickly detection heavy metal ion.Based on this, we have developed
Sodium carboxymethylcellulose/bismuth film modified electrode detection cadmium ion method.
Summary of the invention
The invention solves the technical issues of be: based on the above issues, the present invention provides a kind of based on carboxymethyl cellulose
The method for the electrochemical sensor detection heavy metal cadmium that plain sodium/bismuth film is constructed.
A: bare glassy carbon electrode uses 1.0,0.3 and 0.05 μM of Al respectively2O3Powder polishing, then in ultrapure water, ethyl alcohol
Be respectively cleaned by ultrasonic 3 ~ 5 min, naturally dry in ultrapure water.Sodium carboxymethylcellulose is certain density with ultrapure water preparation
Solution draws the solution drop coating of 3 ~ 8 μ L in bare glassy carbon electrode surface, at room temperature after natural drying, obtains carboxymethyl cellulose
Plain sodium modified electrode；
B: it detection of the sodium carboxymethylcellulose modified electrode to heavy metal cadmium ion: prepares and contains certain density bismuth nitrate and nitre
The step a modified electrode prepared is placed in Acetic acid-sodium acetate buffer, is stirring by the NaAc_HAc buffer solution of sour cadmium
Under the conditions of mixing, while bismuth ion and cadmium ion are deposited, cadmium ion is detected using differential pulse anodic stripping voltammetry.
Further, the concentration of sodium carboxymethylcellulose are as follows: 0.1 ~ 0.8 mg/mL,
Further, in step b, the pH of Acetic acid-sodium acetate buffer is 4 ~ 6, and concentration is 0.05 ~ 0.2 mol/L
Further, the concentration of bismuth nitrate is 0.1 ~ 0.8 mM.
Further, in step b, sedimentation time is set as 120 ~ 180 s, and sedimentation potential is set as -1.0 ~ -1.3
V
Further, the potential range that cadmium ion detects in step b is -1.0 ~ -0.6 V
The beneficial effects of the present invention are: using sodium carboxymethylcellulose/bismuth film modified electrode detection cadmium ion method, operation letter
Just, environmentally protective, it is nontoxic and pollution-free, and sodium carboxymethylcellulose is cheap is easy to get.
Detailed description of the invention
Fig. 1 is the electrochemical signals of different concentration of cadmium ions in embodiment 2；
Fig. 2 is influence of the sedimentation potential to detection cadmium ion in embodiment 3；
Fig. 3 is influence of the sedimentation time to detection cadmium ion in embodiment 4.
Specific embodiment
Embodiment 1
The preparation of sodium carboxymethylcellulose modified electrode
Naked glassy carbon electrode uses 1.0,0.3 and 0.05 μm of Al2O3 powder to polish respectively, then respectively ultrapure water, ethyl alcohol and
It is cleaned by ultrasonic 3min in ultrapure water, 10 mg carboxymethyl celluloses are dissolved in ultrapure water and are configured to 1 mg/mL solution by naturally dry,
5 μ L solution are added drop-wise to naked glassy carbon electrode surface, sodium carboxymethylcellulose modification electricity is obtained after spontaneously drying at room temperature
Pole；
Embodiment 2
Sodium carboxymethylcellulose modified electrode is prepared first, and preparation process is same as Example 1.
The relationship for having investigated different concentration of cadmium ions and electric current, is respectively adopted 0.05 μM, and 0.5 μM, 1 μM, 2 μM, 4 μ
M, 6 μM, 8 μM, 10 μM.Its testing result is as shown in Figure 1, show that peak current and cadmium ion are within the scope of 0.05 ~ 10 μM
Good linear relationship.
Embodiment 3
Sodium carboxymethylcellulose modified electrode is prepared first, and preparation process is same as Example 1.
In order to investigate influence of the sedimentation potential to detection cadmium ion, therefore, using -0.9 V, -1.0 V, -1.1 V, -1.2
V, -1.3 V, -1.4 V different potentials are enriched with.It is as shown in Figure 2 to the testing result of cadmium ion.It can be seen that in -1.2 V
When, peak current is maximum, therefore selects -1.2 V as sedimentation potential.
Embodiment 4
Sodium carboxymethylcellulose modified electrode is prepared first, and preparation process is same as Example 1.
In order to investigate influence of the sedimentation time to detection cadmium ion, selecting sedimentation time is respectively 30 s, 60 s, 90 s,
120 s, 150 s, 180 s carry out cadmium ion detection.Its result is as shown in Figure 3.It can be seen that after 150 s, the suction of modified electrode
Attached amount reaches maximum.So selecting the optimal deposition time for 150 s.
Claims (6)
1. a kind of electrochemical sensor constructed based on sodium carboxymethylcellulose/bismuth film is applied to the detection method of heavy metal cadmium,
Characterized by comprising the following steps:
The preparation of sodium carboxymethylcellulose modified electrode
A: bare glassy carbon electrode uses 1.0,0.3 and 0.05 μM of Al respectively2O3Powder polishing, then in ultrapure water, ethyl alcohol and super
Respectively it is cleaned by ultrasonic 3 ~ 5 min in pure water, naturally dry is certain density molten with ultrapure water preparation by sodium carboxymethylcellulose
Liquid draws the solution drop coating of 3 ~ 8 μ L in bare glassy carbon electrode surface, at room temperature after natural drying, obtains carboxymethyl cellulose
Sodium modified electrode；
Detection of the sodium carboxymethylcellulose modified electrode to heavy metal cadmium ion
B: the NaAc_HAc buffer solution for containing certain density bismuth nitrate and cadmium nitrate is prepared, step a is prepared
Modified electrode is placed in the Acetic acid-sodium acetate buffer, under agitation, while bismuth ion and cadmium ion is deposited, using difference
Show that pulsed anode stripping voltammetry detects cadmium ion.
2. a kind of electrochemical sensor detection weight constructed based on sodium carboxymethylcellulose/bismuth film according to claim 1
The method of cadmium metal, which is characterized in that in the step a, the concentration of sodium carboxymethylcellulose is 0.1 ~ 0.8 mg/mL.
3. a kind of electrochemical sensor detection weight constructed based on sodium carboxymethylcellulose/bismuth film according to claim 1
The method of cadmium metal, which is characterized in that in the step b, the pH of Acetic acid-sodium acetate buffer is 4 ~ 6, concentration is 0.05 ~
0.2 mol/L。
4. a kind of electrochemical sensor detection weight constructed based on sodium carboxymethylcellulose/bismuth film according to claim 1
The method of cadmium metal, which is characterized in that in the step b, the concentration of bismuth nitrate is 0.1 ~ 0.8 mM.
5. a kind of electrochemical sensor detection weight constructed based on sodium carboxymethylcellulose/bismuth film according to claim 1
The method of cadmium metal, which is characterized in that in the step b, sedimentation time is set as 120 ~ 180 s, and sedimentation potential is set as-
1.0 ~ -1.3 V。
6. a kind of electrochemical sensor detection weight constructed based on sodium carboxymethylcellulose/bismuth film according to claim 1
The method of cadmium metal, which is characterized in that the potential range that cadmium ion detects in the step b is -1.0 ~ -0.6 V.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112557467A (en) * | 2020-12-07 | 2021-03-26 | 山西农业大学 | Polymer film modified electrode and preparation method and application thereof |
| CN114002279A (en) * | 2021-10-12 | 2022-02-01 | 华中科技大学 | Method for efficiently detecting content of germanium ions in trace amount and application of method in germanium ore metallurgy |
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| CN107966485A (en) * | 2017-12-07 | 2018-04-27 | 中国石油化工股份有限公司 | A kind of electrochemical heavy metals detector and its detection method based on graphene test paper electrode structure |
| CN108318568A (en) * | 2018-02-05 | 2018-07-24 | 哈尔滨工业大学深圳研究生院 | A kind of electrochemical sensor and preparation method for Sensitive Detection heavy metal cadmium ion |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112557467A (en) * | 2020-12-07 | 2021-03-26 | 山西农业大学 | Polymer film modified electrode and preparation method and application thereof |
| CN112557467B (en) * | 2020-12-07 | 2023-05-26 | 山西农业大学 | Polymer membrane modified electrode and preparation method and application thereof |
| CN114002279A (en) * | 2021-10-12 | 2022-02-01 | 华中科技大学 | Method for efficiently detecting content of germanium ions in trace amount and application of method in germanium ore metallurgy |
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Application publication date: 20190913 |