CN107478696B - The preparation method of carbon material modified glassy carbon electrode for cadmium ion detection - Google Patents
The preparation method of carbon material modified glassy carbon electrode for cadmium ion detection Download PDFInfo
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- CN107478696B CN107478696B CN201710574286.8A CN201710574286A CN107478696B CN 107478696 B CN107478696 B CN 107478696B CN 201710574286 A CN201710574286 A CN 201710574286A CN 107478696 B CN107478696 B CN 107478696B
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Abstract
The invention discloses a kind of preparation methods of carbon material modified glassy carbon electrode for cadmium ion detection, the following steps are included: step (1): zinc powder and dehydrated alcohol are added into stainless steel cauldron, and at a temperature of 500~600 DEG C reaction 12~for 24 hours, obtain nest like black product, successively it is rinsed with dilute hydrochloric acid, deionized water and dehydrated alcohol, and vacuum drying to get arrive nest like carbon material；Step (2): carbon material obtained in step (1) is added into cyclohexanol, is ultrasonically treated 20~25min to get carbon material dispersion liquid is arrived；Step (3): pipetting carbon material dispersion liquid with micropipettor, and is slowly added dropwise on by the mirror surface of pretreated glass-carbon electrode, is placed under infrared lamp and dries to get nest like carbon material modified glassy carbon electrode is arrived.It is preferable that modified glassy carbon electrode of the invention detects low sensitive height, detectable limit, strong antijamming capability and Repeatability.
Description
Technical field
The present invention relates to Electroanalytical Chemistry fields, relate more specifically to a kind of carbon material modification glass for cadmium ion detection
The preparation method of carbon electrode.
Background technique
With industrialized fast development, the murder by poisoning pollutant especially heavy metal ion of the discharge of enterprise's production in recent years
More and more, heavy metal contaminants are difficult to administer, they have quite high stability and refractory organics in water body.Heavy metal
Certain limit is run up in water body to generate serious harm to water body-water plant-aquatic animal system, and can be led to
Cross the life and health safety that food chain directly or indirectly threatens the mankind.And the detection of Heavy Metals in Waters ion be to its into
Precondition row prevention and administered, therefore the needs based on environmental protection and human health, to the heavy metal pollution in environment
The quantitative detection of object is very necessary.
Electrochemical methods be detect Heavy Metals in Waters ion effective means, and chemically modified electrode (CMEs) due to
Preparation is simple, high sensitivity, selectivity is good, response is rapid, replaces toxic mercury electrode to be widely used in analytical chemistry with it.
But prepare it is a kind of for the quick of cadmium ion, the electrode that detectable limit is low, stability is excellent be still electrochemical techniques neck
Domain needs the problem solved.In many electrode modified materials, carbon material carbon nanotube, carbosphere etc. are all more excellent
Good kind.Why carbon nanotube can improve the performance of electrode, be primarily due to carbon nanotube with high-specific surface area, good
The properties such as electronics conduction velocity.Carbosphere has the property similar with carbon nanotube, such as the carbon material being widely studied
High-specific surface area, good electronic conductivity.Novel electrode modified material is developed, electrode modified material can be not only enriched
Kind reduces the cost of electrode modified material, while being also expected further to promote the performance of modified electrode, to reduce detectable limit
With raising detection sensitivity.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of sensitive high, detectable limits of detection
Low, strong antijamming capability and Repeatability are preferably used for carbon material modified glassy carbon electrode and its preparation side of cadmium ion detection
Method.
To achieve the above object, the technical scheme is that a kind of carbon material for cadmium ion detection modifies glass carbon
The preparation method of electrode, comprising the following steps: step (1): zinc powder and dehydrated alcohol are added into stainless steel cauldron, and in
Reaction 12 at a temperature of 500~600 DEG C~for 24 hours, nest like black product is obtained, successively with dilute hydrochloric acid, deionized water and anhydrous
Ethyl alcohol is rinsed, and vacuum drying to get arrive nest like carbon material；Step (2): carbon material obtained in step (1) is added
Enter into cyclohexanol, is ultrasonically treated 20~25min to get carbon material dispersion liquid is arrived；Step (3): carbon is pipetted with micropipettor
Material dispersion liquid, and be slowly added dropwise on by the mirror surface of pretreated glass-carbon electrode, it is placed under infrared lamp and dries to get arriving
Nest like carbon material modified glassy carbon electrode.
The invention has the benefit that the carbon material that the present invention is prepared is in nest like and by cyclohexanol decentralized processing
Afterwards, specific surface area with higher and electronics conduction velocity are applied on glass-carbon electrode, and the detection that can be improved to cadmium ion is sensitive
Degree, detectable limit is low, and strong antijamming capability and repeatability are preferably；Preparation method of the invention simultaneously is simple, at low cost.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure for the nest like carbon material that the present invention is prepared；
Fig. 2 is the cyclic voltammetry curve under different concentration of cadmium ions are corresponding；
Linear relationship chart of the Fig. 3 between peak current and concentration of cadmium ions.
Specific embodiment
The present invention will be described in detail combined with specific embodiments below, and the description of this part is only exemplary and explains
Property, there should not be any restriction effect to protection scope of the present invention.
A kind of preparation method of carbon material modified glassy carbon electrode for cadmium ion detection of the invention, including following step
It is rapid:
Step (1): zinc powder and dehydrated alcohol are added into stainless steel cauldron, and anti-at a temperature of 500~600 DEG C
Answer 12~for 24 hours, nest like black product is obtained, is successively rinsed with dilute hydrochloric acid, deionized water and dehydrated alcohol, and vacuum is dried
It does to get nest like carbon material is arrived；
Step (2): carbon material obtained in step (1) is added into cyclohexanol, be ultrasonically treated 20~25min to get
To carbon material dispersion liquid；
Step (3): pipetting carbon material dispersion liquid with micropipettor, and is slowly added dropwise to by pretreated glass-carbon electrode
Mirror surface on, be placed under infrared lamp and dry to get to nest like carbon material modified glassy carbon electrode.
In above-mentioned technical proposal, the preprocess method of glass-carbon electrode is as follows in the step (3): by glass-carbon electrode particle
The Al that diameter is 0.05~0.1 μm2O3Powder sanding and polishing is at mirror surface, and after being rinsed well with deionized water, it is molten to be sequentially placed into nitrous acid
Liquid, dehydrated alcohol are ultrasonically treated 2~4min in deionized water, and dry under infrared lamp.
In above-mentioned technical proposal, the mass ratio of zinc powder and dehydrated alcohol is 1:15~20 in the step (1).
In above-mentioned technical proposal, the mass ratio of carbon material and cyclohexanol is 1.5~2:5 in the step (2).
Embodiment 1
The preparation process of the carbon material modified glassy carbon electrode for cadmium ion detection of the present embodiment is as follows: (1) taking 1g zinc
Powder and 15g dehydrated alcohol are added into stainless steel cauldron, and react 12h at a temperature of 600 DEG C, obtain the production of nest like black
Object successively carries out repeated flushing with dilute hydrochloric acid, deionized water and dehydrated alcohol, is dried under vacuum after cleaning up to get arriving
Nest like carbon material, Fig. 1 are scanning electron microscope (SEM) figure of the nest like carbon material；(2) take 2mg carbon material be added to
In 5mL cyclohexanol, 20min is ultrasonically treated to get black, uniform nest like carbon material-cyclohexanol dispersion liquid is arrived；(3) by glass
The Al that carbon electrode particle diameter is 0.05 μm2O3Powder sanding and polishing is at mirror surface, after being rinsed well with deionized water, is sequentially placed into
Nitrous acid solution, dehydrated alcohol are ultrasonically treated 2min in deionized water, and dry under infrared lamp；(4) it is moved with micropipettor
10 μ L nest like carbon materials-cyclohexanol dispersion liquid is taken, and is slowly added dropwise to the mirror surface of treated glass-carbon electrode, and level is set
Dried under infrared lamp, to solvent volatilization completely to get arrive nest like carbon material modified glassy carbon electrode.
Embodiment 2
The preparation process of the carbon material modified glassy carbon electrode for cadmium ion detection of the present embodiment is as follows: (1) taking 1g zinc
Powder and 15g dehydrated alcohol are added into stainless steel cauldron, and react for 24 hours at a temperature of 600 DEG C, obtain the production of nest like black
Object successively carries out repeated flushing with dilute hydrochloric acid, deionized water and dehydrated alcohol, is dried under vacuum after cleaning up to get arriving
Nest like carbon material；(2) 1.5mg carbon material is taken to be added into 5mL cyclohexanol, be ultrasonically treated 20min to get to black, uniformly
Nest like carbon material-cyclohexanol dispersion liquid；(3) Al for being 0.05 μm by glass-carbon electrode particle diameter2O3Powder sanding and polishing at
Mirror surface after being rinsed well with deionized water, is sequentially placed into nitrous acid solution, dehydrated alcohol, is ultrasonically treated 2min in deionized water,
And it is dried under infrared lamp；(4) 10 μ L nest like carbon materials-cyclohexanol dispersion liquid is pipetted with micropipettor, and be slowly added dropwise
It to the mirror surface of treated glass-carbon electrode, and is horizontally placed under infrared lamp and dries, to solvent volatilization completely to get arriving nest like
Carbon material modified glassy carbon electrode.Conventional chemical property is carried out to the nest like carbon material modified glassy carbon electrode of the present embodiment to survey
Examination, as a result well.
Embodiment 3
The preparation process of the carbon material modified glassy carbon electrode for cadmium ion detection of the present embodiment is as follows: (1) taking 1g zinc
Powder and 18g dehydrated alcohol are added into stainless steel cauldron, and react for 24 hours at a temperature of 500 DEG C, obtain the production of nest like black
Object successively carries out repeated flushing with dilute hydrochloric acid, deionized water and dehydrated alcohol, is dried under vacuum after cleaning up to get arriving
Nest like carbon material；(2) 1.8mg carbon material is taken to be added into 5mL cyclohexanol, be ultrasonically treated 25min to get to black, uniformly
Nest like carbon material-cyclohexanol dispersion liquid；(3) Al for being 0.1 μm by glass-carbon electrode particle diameter2O3Powder sanding and polishing at
Mirror surface after being rinsed well with deionized water, is sequentially placed into nitrous acid solution, dehydrated alcohol, is ultrasonically treated 3min in deionized water,
And it is dried under infrared lamp；(4) 10 μ L nest like carbon materials-cyclohexanol dispersion liquid is pipetted with micropipettor, and be slowly added dropwise
It to the mirror surface of treated glass-carbon electrode, and is horizontally placed under infrared lamp and dries, to solvent volatilization completely to get arriving nest like
Carbon material modified glassy carbon electrode.Conventional chemical property is carried out to the nest like carbon material modified glassy carbon electrode of the present embodiment to survey
Examination, as a result well.
Embodiment 4
The preparation process of the carbon material modified glassy carbon electrode for cadmium ion detection of the present embodiment is as follows: (1) taking 1g zinc
Powder and 20g dehydrated alcohol are added into stainless steel cauldron, and react 12h at a temperature of 600 DEG C, obtain the production of nest like black
Object successively carries out repeated flushing with dilute hydrochloric acid, deionized water and dehydrated alcohol, is dried under vacuum after cleaning up to get arriving
Nest like carbon material；(2) it takes 2mg carbon material to be added into 5mL cyclohexanol, is ultrasonically treated 25min to get to black, uniform
Nest like carbon material-cyclohexanol dispersion liquid；(3) Al for being 0.1 μm by glass-carbon electrode particle diameter2O3Powder sanding and polishing Cheng Jing
Face after being rinsed well with deionized water, is sequentially placed into nitrous acid solution, dehydrated alcohol, is ultrasonically treated 4min in deionized water, and
It is dried under infrared lamp；(4) pipette 10 μ L nest like carbon materials-cyclohexanol dispersion liquid with micropipettor, and be slowly added dropwise to
It on the mirror surface of treated glass-carbon electrode, and is horizontally placed under infrared lamp and dries, to solvent volatilization completely to get arriving nest like carbon
Material modified glassy carbon electrode.Conventional chemical property is carried out to the nest like carbon material modified glassy carbon electrode of the present embodiment to survey
Examination, as a result well.
Below by taking the carbon material modified glassy carbon electrode being prepared in the present embodiment 1 as an example, conventional electrochemistry is carried out
It can test, reproducibility and interference free performance test.
1, electrochemical property test: electrochemical test method is cyclic voltammetry.
Select the phosphate buffer of 0.1mol/L as supporting electrolyte, the pH value of buffer is 6.0, and sweep speed is
0.1V/s, enrichment time 100s.Under optimal test condition, the results show that 1.0 × 10-8~8.0 × 10-8mol/L
With 8.0 × 10-8~8.3 × 10-7The section mol/L has good linear relationship, and linear equation is respectively I1(10-6A)=
42.800+1.1202(10-8) and I mol/L2(10-6A)=- 4.174+6.8721C (10-8Mol/L), related coefficient is respectively
0.9988 and 0.9973, detectable limit is up to 10-10mol/L.Fig. 2 is the cyclic voltammetry curve under different concentration of cadmium ions are corresponding；
Linear relationship chart of the Fig. 3 between peak current and concentration of cadmium ions.
2, reproducibility is tested: the continuous several times to nest like carbon material modified glassy carbon electrode for cadmium ion measure, test
There is good reproducibility and stability as the result is shown.Every time after measurement, electrode is placed in the liquid of blank bottom, is repeatedly swept
It retouches, to wash off the remaining cadmium ion of electrode surface.
3, anti-interference capability testing: in the water sample containing cadmium ion, 100 times of Cu has been separately added into it2+、Pb2+And Fe3+,
And electrochemical analysis is carried out under the conditions of same detection, compared with being subject to when not adding other ions, the peak current of cadmium ion is almost
It is not influenced by what, illustrates that nest like carbon material modified glassy carbon electrode has good anti-interference ability.
The above described is only a preferred embodiment of the present invention, not making any limit to technical scope of the invention
System, therefore any subtle modifications, equivalent variations and modifications to the above embodiments according to the technical essence of the invention,
It still falls within the scope of technical solution of the present invention.
Claims (3)
1. a kind of preparation method of the carbon material modified glassy carbon electrode for cadmium ion detection, which is characterized in that including following step
It is rapid:
Step (1): zinc powder and dehydrated alcohol are added into stainless steel cauldron, and react 12 at a temperature of 500~600 DEG C
~for 24 hours, nest like black product is obtained, is successively rinsed with dilute hydrochloric acid, deionized water and dehydrated alcohol, and vacuum drying,
Obtain nest like carbon material；The mass ratio of zinc powder and dehydrated alcohol is 1:15~20；
Step (2): carbon material obtained in step (1) is added into cyclohexanol, is ultrasonically treated 20~25min to get carbon is arrived
Material dispersion liquid；
Step (3): pipetting carbon material dispersion liquid with micropipettor, and is slowly added dropwise to the mirror by pretreated glass-carbon electrode
On face, it is placed under infrared lamp and dries to get nest like carbon material modified glassy carbon electrode is arrived.
2. the preparation method for the carbon material modified glassy carbon electrode of cadmium ion detection, feature exist as described in claim 1
In the preprocess method of glass-carbon electrode is as follows in the step (3): being 0.05~0.1 μm by glass-carbon electrode particle diameter
Al2O3Powder sanding and polishing is at mirror surface, after being rinsed well with deionized water, is sequentially placed into nitrous acid solution, dehydrated alcohol, deionization
It is ultrasonically treated 2~4min in water, and is dried under infrared lamp.
3. the preparation method for the carbon material modified glassy carbon electrode of cadmium ion detection, feature exist as described in claim 1
In the mass ratio of carbon material and cyclohexanol is 1.5~2:5 in the step (2).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102011110924A1 (en) * | 2011-08-02 | 2013-02-07 | Marianne Auernhammer | Method for manufacturing electric contact on self-organized layer during manufacturing of sensor element, involves thermally treating conductive dispersion or solution during drying step at room temperature |
| CN103018304A (en) * | 2013-01-08 | 2013-04-03 | 上海师范大学 | Glassy carbon electrode modified by nickel oxide-graphene nano material, preparation method and application thereof |
| CN104020213A (en) * | 2014-06-18 | 2014-09-03 | 中国科学院新疆理化技术研究所 | Electrochemical sensor for simultaneously detecting cadmium and lead ions and preparation method |
| CN103399063B (en) * | 2013-08-07 | 2015-07-08 | 上海师范大学 | Graphene nano material-modified glassy carbon electrode based on phytic acid dispersion, preparation method and application |
| CN107315042A (en) * | 2017-06-09 | 2017-11-03 | 扬州大学 | zinc metal organic framework nano material and its application |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102011110924A1 (en) * | 2011-08-02 | 2013-02-07 | Marianne Auernhammer | Method for manufacturing electric contact on self-organized layer during manufacturing of sensor element, involves thermally treating conductive dispersion or solution during drying step at room temperature |
| CN103018304A (en) * | 2013-01-08 | 2013-04-03 | 上海师范大学 | Glassy carbon electrode modified by nickel oxide-graphene nano material, preparation method and application thereof |
| CN103399063B (en) * | 2013-08-07 | 2015-07-08 | 上海师范大学 | Graphene nano material-modified glassy carbon electrode based on phytic acid dispersion, preparation method and application |
| CN104020213A (en) * | 2014-06-18 | 2014-09-03 | 中国科学院新疆理化技术研究所 | Electrochemical sensor for simultaneously detecting cadmium and lead ions and preparation method |
| CN107315042A (en) * | 2017-06-09 | 2017-11-03 | 扬州大学 | zinc metal organic framework nano material and its application |
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