CN110441367A - It is a kind of to detect Cu using nanogold-graphene combination electrode2+Electrochemical method - Google Patents
It is a kind of to detect Cu using nanogold-graphene combination electrode2+Electrochemical method Download PDFInfo
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Abstract
The present invention provides a kind of utilization nanogold-graphene combination electrode detection Cu2+Electrochemical method, belong to technical field of chemical detection.This method comprises: carrying out pre-treatment to matrix required for depositing；Prepare graphene oxide solution and electrochemical reduction oxidation graphene；Prepare the mixed solution of gold chloride and sulfuric acid；Potentiostatic method deposits nanogold；Optimal detection condition is determined by adjusting the pH of solution, the sedimentation time of Differential Pulse Stripping Voltammetry, sedimentation potential etc..Nanogold-graphene combination electrode prepared by the present invention, method is simple, controllable and environmentally protective, eliminates pollution of the chemical reduction method to original reagent.The advantages of nanogold-graphene combination electrode of preparation combines nanogold and graphene, not only electric conductivity is strong, large specific surface area, electrocatalysis characteristic is excellent, promote the electron transmission between electroactive material and electrode, and partial size is small, be tightly combined with matrix, high sensitivity, detection limit it is low, to Cu2+With good detection effect.
Description
Technical field
The invention belongs to technical field of chemical detection, are related to a kind of utilization nanogold-graphene combination electrode detection Cu2+
Electrochemical method.
Background technique
With the rapid development of science and technology, heavy metal pollution increasingly aggravates, and water pollution phenomenon is increasingly serious, wherein
Exceeded heavy metal ion content is a main cause for causing water pollution, including lead, cadmium, chromium, gold, silver, copper, iron etc.
Density be greater than 4.5g/cm3Metal.Heavy metal is difficult to be decomposed after bio-absorbable to excrete, and can pass through food instead
Object chain is constantly accumulated in animal and plant body from bottom to up.Last thousands of hundred times of enrichment enters human body, and each hatching egg in human body is truncated
The white reciprocation between enzyme, makes their disablements, loses activity, after accumulation reaches a certain level in human body,
It will cause slow poisoning.
Copper is animals and plants especially the essential trace elements of the human body.It maintains normal biological function under normal level.
But copper ion concentration is too high or too low, can all cause many health problems, the accumulation of copper will also result in human poisoning, damage
Evil liver and kidney and other organs.Therefore, to Cu2+It detects particularly important.Electrochemical analysis is some property to participate in reactive material
Matter (such as electric current, electricity, current potential and conductance) knows that the relationship of the amount of substance is foundation with oneself, carries out to test substance qualitative or fixed
The common analysis method of one kind of amount.With accuracy is high, measurement range is wide, instrument and equipment is easy to operate, easy to accomplish automatic
The advantages that change, simultaneously because its quick response, be easy to minimize and be miniaturized, it is highly sensitive and selectivity etc. intrinsic advantages and by
Concern.
Nanogold material has good catalytic performance, this has very big advantage, and nanogold material to heavy metal analysis
The big specific surface area and efficient electron transmission performance of material provide a huge platform for the detection of heavy metal, and because of it
Excellent electric conductivity is studied personnel and is widely applied to Electroanalytical Chemistry field.
Since graphene has, effective ratio area is big, electron transfer rate is high, bio-compatibility is good, high catalytic efficiency
Advantage can make various large biological molecules continue to original structure and bioactivity on the surface of graphene.So graphene
Research in terms of sensor field receives the extensive concern of electrochemical sensor researcher.
Heavy metal ions of the nanogold composite graphite alkene modified electrode in detection soil and water body also have important
Application.But the process for preparing nanogold and redox graphene is cumbersome, the method for usually preparing nanogold have physical method and
Chemical method.Physical method is divided into vapor phase method, liquid phase method, high-energy mechanical ball milling method, and this method is more demanding to instrument and equipment, production takes
With valuableness, the application of such methods is strongly limited.Chemical method is divided into oxidation-reduction method, microwave method, electrochemical process, microemulsion
Method；Wherein chemical reduction method process is cumbersome and is difficult pollution-free, and for microwave method to instrument requirements height, production is expensive.The oxygen of reduction
The preparation method of graphite alkene has a chemical reduction method and photo-reduction, and excessive reductant meeting used in both methods
Pollute the graphene oxide of obtained reduction；On the other hand, it by being chemically treated the oxidation material that cannot be completely removed, can drop
The Electronic Performance of the graphene oxide of low reduction and further limitation application.
Summary of the invention
The technical problem to be solved in the present invention is that providing a kind of utilization nanogold-graphene combination electrode detection Cu2+'s
Electrochemical method, the small gold nano-material of the graphene oxide and partial size of this method not only available reduction, but also entire mistake
Journey green non-pollution, method are simple to operation.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
It is a kind of to detect Cu using nanogold-graphene combination electrode2+Electrochemical method, this method is by by graphite oxide
Alkene dispersion liquid is uniformly deposited to the graphene oxide of reduction on matrix using cyclic voltammetry as deposition liquid, later,
Gold chloride mixed solution is deposited on the matrix for having covered the graphene oxide of reduction with potentiostatic electrodeposition method, obtains gold
Average grain diameter recycles nanogold-graphene combination electrode to treat in nanogold-graphene combination electrode material of Nano grade
Survey the Cu in liquid2+Carry out electrochemical analysis detection；Specifically includes the following steps:
The first step, the pre-treatment of matrix
Glass carbon base body required for depositing successively is activated, washed, is dried up.
Second step prepares graphene oxide deposition solution
Graphene oxide deposition solution includes graphene oxide powder and phosphate buffer: graphene oxide powder is molten
Enter in phosphate buffer, ultrasound removing one hour, oscillation is uniformly mixed it up and down after taking-up, forms the oxygen of 1~2mg/mL
Graphite alkene aqueous colloidal dispersion.
The phosphate buffer solution concentration is 0.2mol/L, pH=7.0.
Third step, electrochemical reduction deposited oxide graphene
Graphene oxide reduction is realized using cyclic voltammetric reduction method；The graphene oxide deposition solution that second step is obtained
It is deposited on matrix, is stirred in deposition process, carried out in the range of -1.50~0.60V with the sweep speed of 25mV/s
Seven current potential circulations；After electro-deposition, the electrode that the graphene oxide of obtained reduction is modified is cleaned with distilled water, in infrared lamp
Under dry, obtain uniform fold reduction graphene oxide matrix.
4th step prepares the mixed solution of gold chloride and sulfuric acid
Gold chloride concentration is 5~10mmol/L in the mixed solution, and sulfuric acid concentration is 0.5~1mol/L.
5th step, electrochemical deposition nanogold
The matrix that third step is obtained is placed in the mixed solution that the 4th step obtains, and carries out electrochemistry using potentiostatic method
Nanogold is deposited, sedimentation potential is -0.01V, sedimentation time 120s, obtains the compound glass-carbon electrode of nanogold-graphene, will answer
Composite electrode is cleaned with distilled water, is dried under infrared lamp.
6th step, to the Cu in prepare liquid2+Carry out electrochemical analysis detection
Electrochemistry detecting apparatus is immersed in the acidity solution to be measured containing heavy metal ion, working electrode is the 5th step system
Standby to obtain the compound glass-carbon electrode of nanogold-graphene, reference electrode Ag/AgCl is platinum filament to electrode；Apply sedimentation potential into
Row pretreatment, is detected with Differential Pulse Stripping Voltammetry, and the sedimentation potential is -1.5~0V, preferred deposition electricity
Position is -1.3V；Sedimentation time is 120~200s, and preferred sedimentation time is 180s.In preprocessing process to solution to be measured into
Row stirring, the mixing speed are 400~800 revs/min, and preferred mixing speed is 600 revs/min.Stop stirring
Afterwards, it is scanned with Differential Pulse Stripping Voltammetry, scanning current potential is -1.4~0V, and the current potential increment of scanning is 0.004V, is swept
Retouching amplitude is 0.05V；After scanning, Cu is recorded2+Spike potential and peak point current, and peak current and ion concentration are in certain linear
Relationship, to realize to Cu2+Detection.
The pH value of the acidity solution to be measured is 3.6~5.4, and preferred pH value is 4.6.
Beneficial effects of the present invention:
(1) a kind of utilization nanogold-graphene combination electrode of the present invention detects Cu2+Electrochemical method, solely
Special place is to prepare the graphene oxide combination electrode of nanogold and reduction using electrochemical reducing and applied to Cu2+Inspection
Survey, the nanogold material particle size made is smaller, in conjunction with matrix it is more stable, and preparation process is easy to operate, environmentally friendly, condition
It is easily-controllable.The nanogold of preparation-graphene composite material purity is high, nanogold-graphene for electrochemical reducing preparation are compound
Electrode is suitable for different Cu2+Testing conditions provide guarantee.
(2) a kind of utilization nanogold-graphene combination electrode of the present invention detects Cu2+Electrochemical method, with change
It learns reduction method and other physics reduction methods is compared, influence of the chemical reducing agent of introduction to deposition liquid purity can be removed, more
It is environmentally protective, and obtained composite material average grain diameter is small, in conjunction with matrix more closely, and specific surface area greatly increases,
Accurately to identify and detecting Cu2+Provide guarantee.
(3) a kind of utilization nanogold-graphene combination electrode of the present invention detects Cu2+Electrochemical method, make with
The partial size of nanogold after graphene is compound becomes smaller, and structure becomes from the uniform two-dimensional film of round or ellipse
Along graphene film interface growth three-dimensional pine-tree structure, show that there is strong mutual between graphene and nano Au particle
Effect.Compared with traditional carbon structure film, the graphene with single layer carbon structure, which is more advantageous to, promotes electronics in nano material
The movement on surface improves electron transfer rate, produces in multilayer and graphene film surface with fold a kind of good
Orderly nanogold pine-tree structure, three-dimensional pine-tree structure can provide bigger electroactive surface product compared to single nanometer film,
More higher electronics binding sites of activity are provided, electronic conductivity is greatly improved, improves the electrochemistry of electrode
Can, the electrochemical response of metal ion to be measured is enhanced, the electrochemical sensor obtained from, detection limit is lower, and rate of precision is more
Height, and the prospect with good practical application.
Detailed description of the invention
Fig. 1 is that electrochemical reducing prepares the compound glass-carbon electrode detection Cu of nanogold-graphene in the present invention2+Schematic diagram；
Fig. 2 is the detection Cu of electrochemical reducing of the present invention preparation2+Nanogold-graphene composite material SEM figure；
Wherein, a is that nanogold-graphene composite material SEM that scale is 3 μm schemes, and b is that nanogold-graphene that scale is 5 μm is multiple
The SEM of condensation material schemes, and c is that nanogold-graphene composite material SEM that scale is 1 μm schemes, and d is the nanometer that scale is 30 μm
Gold-graphene composite material SEM figure；
Fig. 3 is the relational graph of sedimentation time and peak point current in 2~embodiment of embodiment 4 in the present invention；
Fig. 4 is the relational graph of sedimentation potential and peak point current in 5~embodiment of embodiment 7 in the present invention；
Fig. 5 is embodiment 8 in the present invention, detection various concentration Cu in embodiment 92+Differential pulse curve graph；
Fig. 6 is embodiment 8 in the present invention, Cu obtained in embodiment 92+Concentration and peak point current relational graph.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawing, and however, it is not limited to this, described
Embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff every other embodiment obtained without making creative work belongs to what the present invention protected
Range.
Agents useful for same is all commercially available in following embodiment.
Embodiment 1
The graphene oxide solution of 5mL, 1mg/mL are added in electrolytic cell, electrochemical apparatus is immersed in graphite oxide
In alkene solution.It is stirred during deposition and graphene oxide solution is deposited on glass carbon base body, realize graphite oxide
The cyclic voltammetric of alkene restores, and carries out seven current potential circulations in the range of -1.50~0.60V with the sweep speed of 25mV/s.Electricity
After deposition, the electrode that the graphene oxide of obtained reduction is modified is cleaned with distilled water, is dried under infrared lamp, obtained uniformly
Cover the matrix of the graphene oxide of reduction.
The matrix of the graphene oxide of uniform fold reduction is placed in prepared gold chloride and sulfuric acid later
In mixed solution, electrochemical deposition nanogold is carried out using potentiostatic method: by 5mL, 5mmol/L gold chloride and 0.5mol/L sulfuric acid
Mixed solution be added in electrolytic cell, electrochemical apparatus is immersed in solution, using potentiostatic method, applies sedimentation potential-
0.01V simultaneously deposits 120s, obtains the glass-carbon electrode of graphene composite nano-gold modification, electrode is cleaned with distilled water, infrared
It is dried under lamp, for use.
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 10 μ g/L.Electrochemistry
The compound glass-carbon electrode of nanogold-graphene of reduction method preparation is working electrode, and Ag/AgCl is reference electrode, is platinum to electrode
Silk.Using Differential Pulse Stripping Voltammetry, the sedimentation potential of application -1.2V pre-processes 180s, makes ion enrichment in electrode surface,
Enrichment process is stirred with 600 revs/min of speed.After pretreatment, stop stirring.Difference is selected within the scope of current potential -1.4~0V
Pulse Stripping Voltammetry is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records
Cu2+Spike potential and peak point current.
Embodiment 2
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 10 μ g/L, embodiment
The compound glass-carbon electrode of nanogold-graphene that in 1 prepared by electrochemical reducing is working electrode, and Ag/AgCl is reference electrode,
It is platinum filament to electrode.The sedimentation potential of application -1.3V pre-processes 120s, makes ion enrichment in electrode surface, enrichment process is with 600
Rev/min speed stirring.After pretreatment, stop stirring.Differential pulse Stripping Voltammetry is selected within the scope of current potential -1.4~0V
Method is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records Cu2+Spike potential with
Peak point current.
Embodiment 3
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 10 μ g/L, embodiment
The compound glass-carbon electrode of nanogold-graphene that in 1 prepared by electrochemical reducing is working electrode, and Ag/AgCl is reference electrode,
It is platinum filament to electrode.The sedimentation potential of application -1.3V pre-processes 200s, makes ion enrichment in electrode surface, enrichment process is with 600
Rev/min speed stirring.After pretreatment, stop stirring.Differential pulse Stripping Voltammetry is selected within the scope of current potential -1.4~0V
Method is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records Cu2+Spike potential with
Peak point current.
Embodiment 4
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 10 μ g/L, embodiment
The compound glass-carbon electrode of nanogold-graphene that in 1 prepared by electrochemical reducing is working electrode, and Ag/AgCl is reference electrode,
It is platinum filament to electrode.The sedimentation potential of application -1.3V pre-processes 160s, makes ion enrichment in electrode surface, enrichment process is with 600
Rev/min speed stirring.After pretreatment, stop stirring.Differential pulse Stripping Voltammetry is selected within the scope of current potential -1.4~0V
Method is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records Cu2+Spike potential with
Peak point current.
Embodiment 5
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 10 μ g/L, embodiment
The compound glass-carbon electrode of nanogold-graphene that in 1 prepared by electrochemical reducing is working electrode, and Ag/AgCl is reference electrode,
It is platinum filament to electrode.The sedimentation potential for applying 0V pre-processes 180s, makes ion enrichment in electrode surface, enrichment process with 600 turns/
The speed stirring of minute.After pretreatment, stop stirring.Within the scope of current potential -1.4~0V select Differential Pulse Stripping Voltammetry into
Row scanning (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and record Cu2+Spike potential and peak electricity
Flow valuve.
Embodiment 6
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 10 μ g/L, embodiment
The compound glass-carbon electrode of nanogold-graphene that in 1 prepared by electrochemical process is working electrode, and Ag/AgCl is reference electrode, to electricity
Extremely platinum filament.The sedimentation potential of application -1.5V pre-processes 180s, makes ion enrichment in electrode surface, enrichment process with 600 turns/
The speed stirring of minute.After pretreatment, stop stirring.Differential Pulse Stripping Voltammetry is selected within the scope of current potential -1.4~0V
It is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records Cu2+Spike potential with
Peak point current.
Embodiment 7
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 10 μ g/L.Using reality
The method preparation compound glass-carbon electrode of nanogold-graphene in example 1 is applied, wherein difference are as follows: the graphite oxide in the first step
Alkene solution concentration is 2mg/mL, and the gold chloride concentration in the 4th step mixed solution is 10mmol/L, sulfuric acid concentration 1mol/L,
The operation of remaining preparation compound glass-carbon electrode of nanogold-graphene and embodiment 1 are all the same.
Again using the compound glass-carbon electrode of nanogold-graphene being prepared as working electrode, Ag/AgCl is reference electrode,
It is platinum filament to electrode.The sedimentation potential of application -1.2V pre-processes 180s, makes ion enrichment in electrode surface, enrichment process is with 600
Rev/min speed stirring.After pretreatment, stop stirring.Differential pulse Stripping Voltammetry is selected within the scope of current potential -1.4~0V
Method is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records Cu2+Spike potential with
Peak point current.
Embodiment 8
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 60 μ g/L, embodiment
The compound glass-carbon electrode of nanogold-graphene that in 1 prepared by electrochemical process is working electrode, and Ag/AgCl is reference electrode, to electricity
Extremely platinum filament.The sedimentation potential of application -1.3V pre-processes 180s, makes ion enrichment in electrode surface, enrichment process with 600 turns/
The speed stirring of minute.After pretreatment, stop stirring.Differential Pulse Stripping Voltammetry is selected within the scope of current potential -1.4~0V
It is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records Cu2+Spike potential with
Peak point current, and peak current and Cu2+Concentration is in certain linear relationship.
Embodiment 9
Cu is added in the hac buffer of 0.1mol/L, pH=4.62+, make Cu2+Concentration be 80 μ g/L, embodiment
The compound glass-carbon electrode of nanogold-graphene that in 1 prepared by electrochemical process is working electrode, and Ag/AgCl is reference electrode, to electricity
Extremely platinum filament.The sedimentation potential of application -1.3V pre-processes 180s, makes ion enrichment in electrode surface, enrichment process with 600 turns/
The speed stirring of minute.After pretreatment, stop stirring.Differential Pulse Stripping Voltammetry is selected within the scope of current potential -1.4~0V
It is scanned (scanning constant parameter: current potential increment is 0.004V, scan amplitude 0.05V), and records Cu2+Spike potential with
Peak point current, and peak current and Cu2+Concentration is in certain linear relationship.
Embodiment described above only expresses embodiments of the present invention, and but it cannot be understood as to the invention patent
Range limitation, it is noted that for those skilled in the art, without departing from the inventive concept of the premise, also
Several modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.
Claims (5)
1. a kind of detect Cu using nanogold-graphene combination electrode2+Electrochemical method, which is characterized in that this method includes
Following steps:
The first step, the pre-treatment of matrix
Matrix required for depositing successively is activated, washed, is dried up；
Second step prepares graphene oxide deposition solution
Graphene oxide powder to be dissolved in phosphate buffer solution, ultrasound removing, oscillation is uniformly mixed it up and down after taking-up,
Form the graphene oxide aqueous colloidal dispersion of 1~2mg/mL；
Third step, electrochemical reduction deposited oxide graphene
Graphene oxide reduction is carried out using cyclic voltammetry；The graphene oxide deposition solution that second step obtains is deposited on base
It on body, is stirred in deposition process, multiple current potential is carried out in the range of -1.50~0.60V with the sweep speed of 25mV/s
Circulation；After electro-deposition, the electrode that the graphene oxide restored is modified is cleaned, is dried, obtains the oxygen of uniform fold reduction
The matrix of graphite alkene；
4th step prepares the mixed solution of gold chloride and sulfuric acid
Gold chloride concentration is 5~10mmol/L in the mixed solution, and sulfuric acid concentration is 0.5~1mol/L；
5th step, electrochemical deposition nanogold
The matrix that third step is obtained is placed in the mixed solution of gold chloride and sulfuric acid that the 4th step obtains, using potentiostatic method
Electrochemical deposition nanogold is carried out, sedimentation potential is -0.01V, sedimentation time 120s, obtains nanogold-graphene compound electric
Combination electrode is cleaned, is dried by pole；
6th step, to the Cu in prepare liquid2+Carry out electrochemical analysis detection
Electrochemistry detecting apparatus is immersed in the acidity solution to be measured containing heavy metal ion, the pH value of the acidity solution to be measured
It is 3.6~5.4；Working electrode is nanogold-graphene combination electrode that the 5th step obtains, reference electrode Ag/AgCl, to electricity
Extremely platinum filament；Apply sedimentation potential to be pre-processed, sedimentation potential is -1.5~0V, and sedimentation time is 120~200s；Pretreatment
Solution to be measured is stirred in the process, mixing speed is 400~800 revs/min；After stopping stirring, dissolved out with differential pulse
Voltammetry is scanned, and scanning current potential is -1.4~0V；After scanning, Cu is recorded2+Spike potential and peak point current, realize to Cu2+
Detection.
2. a kind of utilization nanogold-graphene combination electrode according to claim 1 detects Cu2+Electrochemical method,
It is characterized in that, matrix described in the first step is glass carbon.
3. a kind of utilization nanogold-graphene combination electrode according to claim 1 or 2 detects Cu2+Electrochemical method,
It is characterized in that, phosphate buffer solution concentration is 0.2mol/L, pH=7.0 in the second step.
4. a kind of utilization nanogold-graphene combination electrode according to claim 1 or 2 detects Cu2+Electrochemical method,
It is characterized in that, in the 6th step, it is preferred that the pH value of the acidity solution to be measured is 4.6；Pretreated sedimentation potential be-
1.3V, sedimentation time 180s；It is 600 revs/min to the speed of solution to be measured stirring in preprocessing process；Differential pulse dissolution
The current potential increment of voltammetry scanning is 0.004V, scan amplitude 0.05V.
5. a kind of utilization nanogold-graphene combination electrode according to claim 3 detects Cu2+Electrochemical method,
It is characterized in that, in the 6th step, it is preferred that the pH value of the acidity solution to be measured is 4.6；Pretreated sedimentation potential be-
1.3V, sedimentation time 180s；It is 600 revs/min to the speed of solution to be measured stirring in preprocessing process；Differential pulse dissolution
The current potential increment of voltammetry scanning is 0.004V, scan amplitude 0.05V.
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| CN111304716A (en) * | 2020-03-12 | 2020-06-19 | 陕西煤业化工技术研究院有限责任公司 | Preparation method of pencil graphite modified electrode and method for detecting benzenediol isomer in water body |
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| CN113030209A (en) * | 2021-03-16 | 2021-06-25 | 青岛大学 | Method for rapidly and controllably preparing flexible graphene electrode and application |
| CN113030209B (en) * | 2021-03-16 | 2023-04-28 | 青岛大学 | Method for preparing flexible graphene electrode in rapid and controllable manner and application |
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Application publication date: 20191112 |