CN107389761A - A kind of preparation method of carborundum decorating carbon paste electrode - Google Patents
A kind of preparation method of carborundum decorating carbon paste electrode Download PDFInfo
- Publication number
- CN107389761A CN107389761A CN201710565322.4A CN201710565322A CN107389761A CN 107389761 A CN107389761 A CN 107389761A CN 201710565322 A CN201710565322 A CN 201710565322A CN 107389761 A CN107389761 A CN 107389761A
- Authority
- CN
- China
- Prior art keywords
- electrode
- carborundum
- carbon paste
- preparation
- decorating carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
The invention discloses a kind of preparation method of carborundum decorating carbon paste electrode, comprise the following steps that：(1) graphite powder and carborundum are put into mortar and fully mixed, add atoleine afterwards, be fully ground, mix pastel is made；The pastel made is filled into polyfluortetraethylene pipe and is compacted, finally electrode surface is polished, polishes and obtains electrode；(2) in BR cushioning liquid, using three-electrode system, cyclic voltammetry scan is carried out to electrode prepared by step (1), until the cyclic voltammetry curve stablized, electrode is taken out, cleaned with secondary deionized water, the carborundum decorating carbon paste electrode of the present invention is prepared.Compared with naked carbon paste electrode, the carborundum decorating carbon paste electrode prepared with the present invention is to Hg2+Measure have significantly improved.
Description
Technical field
The present invention relates to electrochemical technology field, more particularly to a kind of preparation method of carborundum decorating carbon paste electrode.
Background technology
Chemically modified carbon paste electrode (the Chemically Modified Carbon that the 1970s, mid-term occurred
Paste Electrode, abbreviation CMCPE) grow up on the basis of CPE, it combines the excellent of chemically modified electrode
Point, the reactions such as enrichment, separation, catalysis and selection can be borrowed to carry out analysis measure to numerous materials.CMCPE is modified in carbon paste
A certain amount of appropriate dressing agent, can be according to the intention function predetermined to electrode modification by cutting out the molecule of electrode surface.
CMCPE inherits CPE all advantages, and by introducing the dressing agent with wholesomeness, so as to improving application and spirit
Sensitivitys, background current and overpotential are reduced, compared with CPE, can qualitatively, selectively be reacted with faster speed,
Having broken traditional electrode such as mercury electrode, noble metal electrode etc. only there is single electronics to award limitation the affected, improve electrode
Selectivity.Meanwhile CMCPE also has the feature of modified electrode, the electrode of various functions can such as be made, priority enrichment is to be measured
Component, show electro catalytic activity etc..
In recent years, CMCPE can obtain so rapid development performance unique with it and not in analytical chemistry field
Alternative advantage is closely related, and concrete analysis is as follows：
(1) potential window is wide, and use range is extensive.Oxidation reaction in organic matter test mostly occurs in positive potential area, and
Usable range of the classical dropping-mercury electrode in positive potential area is limited, and CMCPE expands positive potential scope, can be widely used in
The electrochemical analysis of machine thing and medicine.
(2) functional groups of the CMCPE due to the addition of some wholesomeness, while making electrode selectively be reacted
The transfer velocity of electronics in electrode reaction is accelerated, having broken traditional mercury electrode, noble metal electrode etc. only there is single electronics to award
Limitation the affected.And CMCPE dressing agent is a lot, various types of electrode, different types of electricity can be made
Effect extremely to various materials in solution is also different, that is to say, that CMCPE has good selectivity.
(3) in general solid modified electrode, although can be by the way that there is selective chemical in electrode surface continued access or coating
The modification film of group, which reaches, carries out manually modified purpose to electrode, but cumbersome in the presence of preparation formality, and condition is difficult to control,
The shortcomings of electrode performance is unstable.And CMCPE can by people wish and need different dressing agents, carbon dust, adhesive
It is well mixed that electrode is made, that is, reach the purpose for assigning certain predetermined function of electrode, there is simple for production, cheap excellent of cost again
Point.
(4) CMCPE has unique superiority in terms of selectivity and sensitivity is improved.Determinand is in electrode surface and repaiies
Decorations agent reacts so that the micro-structural on CMCPE surfaces can provide a variety of potential fields that can be utilized, and determinand can be carried out effectively
Separation and concentration, selectivity is further improved by means of coordination electrode current potential and can, and can also assay method (such as pulse voltammetry,
Stripping voltammetry etc.) sensitivity and dressing agent selectivity of chemical equation be combined, it is believed that CMCPE be separation, enrichment
The ideal system to integrate with selective determination three.
(5) CMCPE is typically only with millimetre-sized glass-tube, and dressing agent can improve sensitivity, broadening test limit,
Strengthen stability and avoid interference etc., be particularly conducive to electrode and develop to miniaturization, integrated direction.
Although CMCPE has many advantages in electrochemical analysis, application is also expanding day by day, and it is as one
The emerging electrode of kind, development is perfect not enough, and there is some shortcomings.
First, the data measured are not sufficiently stable, every time after measure, because measured object is largely adsorbed in electrode surface, institute
Must be updated before next determine to electrode surface.Most simply conventional method is to remove used modified carbon
Paste, prepares new modification carbon paste, this just necessarily causes the physico-chemical property of electrode surface to be not sufficiently stable, and also influences whether to survey surely again
Determine result.
Secondly, CMCPE use formality is numerous and diverse, time-consuming.CMCPE has to pass through preparation from starting to be prepared into come into operation
With activate the two processes, and pass through activation process again before reusing, or even to prepare new modification carbon paste again, it is impossible to
Enough continuous operations, can waste many times.
In addition, CMCPE reappearance is not good enough, the surface state of this and electrode has relation.At present CMCPE prepare it is most
It is or ripe not enough using the method for hand lapping, technology, it is difficult to ensure that carbon paste is mixed thoroughly.If carbon paste mixes not
Uniformly, after sanding and polishing, the active component on surface can not be distributed unanimously electrode, determinand be readily adsorbed on highenergy sites and
Pollute, inherently have an impact to the reappearance of measurement result.
With China's rapid development of economy, the energy, resource largely consume, and cause some mercury pollution problems or potential
Mercury pollution problem.Mercury is accumulated in human body and animal tissue, can cause the diseases such as anaemia, nervous function imbalance and injury of kidney,
Therefore the analysis method of measure mercury is constantly subjected to the concern of people.
At present, determining the common methods of mercury ion has AAS, atomic absorption spectrography (AAS), chemiluminometry
Deng the most sample handling processes of these methods are cumbersome, are related to valuable instrument and complicated operation.Electrochemical reaction is according to method
Law is drawn to carry out, so either how small material change can also be measured by electric current or electricity, and
And the chemical parameters for being typically difficult to determine can be translates directly into the electrical parameter easily determined and be surveyed by electrochemical analysis measure
Fixed, therefore, electrochemical analysis test has the characteristics that simple to operate, high sensitivity and practical.
The content of the invention
In order to solve the deficiency of existing measure mercury ion method, present invention aims at provide a kind of carborundum modified carbon
The preparation method of paste electrode, and determine lead ion content in solution.
The present invention adopts the technical scheme that：
The preparation method of the carborundum decorating carbon paste electrode of the present invention comprises the following steps that：
(1) graphite powder and carborundum are put into mortar and fully mixed, add atoleine afterwards, be fully ground,
Pastel is made in mixing；The pastel made is filled into polyfluortetraethylene pipe and is compacted, finally electrode surface is polished, polished
Obtain electrode；
(2) in BR cushioning liquid, using three-electrode system, cyclic voltammetry scan is carried out to electrode prepared by step (1),
Until the cyclic voltammetry curve stablized, electrode is taken out, cleaned with secondary deionized water, the carbonization of the present invention is prepared
Silicon decorating carbon paste electrode.
In step (1), the mass ratio of graphite powder and carborundum is 5-20：1, the mass ratio of preferably graphite powder and carborundum is
10：1.
In step (2), the pH=1.0-3.0 of BR cushioning liquid, concentration is 0.05-0.20mol/L, preferably BR cushioning liquid
PH=2.0, concentration is 0.10mol/L.
In step (2), three-electrode system is by Electrode (Working Electrode, WE), reference electrode
(Reference Electrode, RE) and auxiliary electrode (Counter Electrode, CE) form, and electric current is from working electrode stream
To auxiliary electrode, independent reference electrode only provides reference potential and no current passes through.
In step (2), the voltage of three-electrode system is 1.2V~-1.2V, and potential scanning speed is 50-150mV/s, preferably
Potential scanning speed is 100mV/s.
Carborundum has big surface area because particle diameter is small, so make that the ratio shared by surface atom is big, surface energy is high,
Cause Atomic coordinate insufficient, these atoms is easily combined with other atoms or ion and settle out, there is very high surface to live
Property, strong suction-operated can be produced to metal ion.Make dressing agent decorating carbon paste electrode with carborundum, by carborundum in electricity
Suction-operated on the surface of pole to mercury ion reaches the purpose of optimization enrichment, improves the sensitivity of electrode.Course of reaction such as formula 2.1
~formula 2.3：
(Hg2+)Solution+(SiC)Electrode surface→(Hg2+—SiC)Absorption(formula 2.1)
(Hg2+—SiC)Absorption+2e-→(Hg—SiC)Absorption(formula 2.2)
(Hg—SiC)Absorption- 2e-→(Hg2+)Solution+(SiC)Electrode surface(formula 2.3)
Cyclic voltammetry is the electric current of the measurement system under certain potentials, obtains VA characteristic curve.For a reduction
Reaction, control the potential of Electrode with speed v from EiStart to scan to potential negative direction, to time t=λ, (corresponding potential is
Eλ) when potential change scanning direction, with identical speed flyback to onset potential, then potential commutates again, is repeatedly scanned with, i.e.,
The potential control signal used is continuous triangle ripple signal, as record current-potential curve, cyclic voltammetry curve.Circulation volt
An Fayou " electrochemistry spectrum " title, is widely used in inorganic matter and organic electrodes process and biochemistry and polymer chemistry
The sign of middle polyelectron transmittance process.
The positive effect of the present invention is as follows：
Compared with naked carbon paste electrode, the carborundum decorating carbon paste electrode prepared with the present invention is relative to common Hg2+Survey
It is fixed, have that experiment is simple, it is easy to operate, the characteristics of high sensitivity：
Test result indicates that peak current and Hg2+Concentration is (1.0 × 10 in less scope-7~1.0 × 10-4mol/L)
In good linear relation, its signal responsiveness is higher (linearly dependent coefficient reaches 0.9971), and its detection limit can reach 3.7
×10-8mol/L。
Brief description of the drawings
Fig. 1 is the cyclic voltammetric of 1# bare electrodes and 3# modified electrodes in 1.0 × 10-4mol/LHg2+ solution (liquid containing bottom)
Figure.
Fig. 2 is Different electrodes 1.0 × 10-4mol/LHg2+Cyclic voltammogram in solution (liquid containing bottom).
Fig. 3 is # electrodes 1.0 × 10-4mol/LHg2+The continuous cyclic voltammetry scan figure of solution.
Fig. 4 is carborundum decorating carbon paste electrode (3# electrodes) to Hg2+Response curve.
Embodiment
The following examples are that the present invention is described in further detail.
Embodiment 1
The preparation method of the carborundum decorating carbon paste electrode of the present invention comprises the following steps that：
(1) graphite powder and carborundum are put into mortar and fully mixed, add atoleine afterwards, be fully ground,
Pastel is made in mixing；The pastel made is filled into polyfluortetraethylene pipe and is compacted, finally electrode surface is polished, polished
Obtain electrode；
(2) in BR cushioning liquid, using three-electrode system, cyclic voltammetry scan is carried out to electrode prepared by step (1),
Until the cyclic voltammetry curve stablized, electrode is taken out, cleaned with secondary deionized water, the carbonization of the present invention is prepared
Silicon decorating carbon paste electrode, labeled as 2# carborundum decorating carbon paste electrodes.
In step (1), the mass ratio of graphite powder and carborundum is 15：1.
In step (2), the pH=1.0 of BR cushioning liquid, concentration is 0.20mol/L.
In step (2), three-electrode system is by Electrode (Working Electrode, WE), reference electrode
(Reference Electrode, RE) and auxiliary electrode (Counter Electrode, CE) form, and electric current is from working electrode stream
To auxiliary electrode, independent reference electrode only provides reference potential and no current passes through.
In step (2), the voltage of three-electrode system is 1.2V, and potential scanning speed is 150mV/s.
Embodiment 2
The preparation method of the carborundum decorating carbon paste electrode of the present invention comprises the following steps that：(1) by graphite powder and carbonization
Silicon is put into mortar and fully mixed, and adds atoleine afterwards, is fully ground, mixes pastel is made；The paste that will be made
Shape thing, which is filled into polyfluortetraethylene pipe, to be compacted, and finally electrode surface is polished, polishes and obtains electrode；
(2) in BR cushioning liquid, using three-electrode system, cyclic voltammetry scan is carried out to electrode prepared by step (1),
Until the cyclic voltammetry curve stablized, electrode is taken out, cleaned with secondary deionized water, the carbonization of the present invention is prepared
Silicon decorating carbon paste electrode, labeled as 3# carborundum decorating carbon paste electrodes.
In step (1), the mass ratio of graphite powder and carborundum is 10：1.
In step (2), the pH=2.0 of BR cushioning liquid, concentration is 0.10mol/L.
In step (2), three-electrode system is by Electrode (Working Electrode, WE), reference electrode
(Reference Electrode, RE) and auxiliary electrode (Counter Electrode, CE) form, and electric current is from working electrode stream
To auxiliary electrode, independent reference electrode only provides reference potential and no current passes through.
In step (2), the voltage of three-electrode system is 0V, and potential scanning speed is 100mV/s.
Embodiment 3
The preparation method of the carborundum decorating carbon paste electrode of the present invention comprises the following steps that：
(1) graphite powder and carborundum are put into mortar and fully mixed, add atoleine afterwards, be fully ground,
Pastel is made in mixing；The pastel made is filled into polyfluortetraethylene pipe and is compacted, finally electrode surface is polished, polished
Obtain electrode；
(2) in BR cushioning liquid, using three-electrode system, cyclic voltammetry scan is carried out to electrode prepared by step (1),
Until the cyclic voltammetry curve stablized, electrode is taken out, cleaned with secondary deionized water, the carbonization of the present invention is prepared
Silicon decorating carbon paste electrode, labeled as 4# carborundum decorating carbon paste electrodes.
In step (1), the mass ratio of graphite powder and carborundum is 8：1.
In step (2), the pH=3.0 of BR cushioning liquid, concentration is 0.05mol/L.
In step (2), three-electrode system is by Electrode (Working Electrode, WE), reference electrode
(Reference Electrode, RE) and auxiliary electrode (Counter Electrode, CE) form, and electric current is from working electrode stream
To auxiliary electrode, independent reference electrode only provides reference potential and no current passes through.
In step (2), the voltage of three-electrode system is -1.2V, and potential scanning speed is 50mV/s.
Comparative example
Take graphite powder to add atoleine in mortar, be fully ground, mix pastel is made, then by mixed paste
Shape thing, which is filled into electrode tube, to be compacted, and finally electrode surface is polished, polished, labeled as the naked carbon electrodes of 1#, dried for standby.
The sign of electrode
By make four electrodes 0.1mol/L K3[Fe(CN)6] cyclic voltammetry scan is carried out in solution, what is obtained follows
The oxidation of ring volt-ampere curve, reduction peak are symmetrical, and peak point current is equal, and spike potential difference is smaller, and five electrodes that this explanation makes belong to
Qualified electrode.
The preparation of BR cushioning liquid
Electronic scale weighs 0.8gNaOH first, is dissolved in small beaker, and is transferred in 100ml volumetric flasks, then will be small
Beaker cleans 2-3 times, and cleaning solution is transferred in the volumetric flask, constant volume, fully shakes up rear standby, and the NaOH solution concentration is
0.2mol/L；
Then 1.2366g boric acid is weighed with assay balance, is then transferred to dissolving in small beaker in 500ml volumetric flasks, clearly
Wash small beaker 2-3 times, and be transferred in volumetric flask；1.3333ml phosphoric acid, 1.1535ml glacial acetic acid are measured respectively with 5ml pipettes again
In the volumetric flask, add water constant volume.It is transferred to after fully shaking up in wide-mouth bottle, adds the 0.2mol/L's of the above-mentioned preparations of 20ml
NaOH solution, shake up, thus made pH=1.98 BR cushioning liquid.Due to consideration that BR cushioning liquid should not be long
Put, and preparation is also more convenient, therefore this experiment is now with the current.
Hg2+The preparation of solution
The preparation of mother liquor
0.3235gHg (NO are weighed with electronic scale3)2, dissolved and be transferred in 100ml volumetric flask with small beaker, then will
Small beaker is washed about 2-3 times and is transferred to again in volumetric flask, and constant volume fully shakes up.The solution of above-mentioned preparation is 0.01mol/L Hg2+
Solution, it is stand-by as mother liquor.
Various concentrations Hg2+The preparation of solution
Appropriate above-mentioned 0.01mol/L Hg is taken with pipette2+Solution is added in 50ml volumetric flasks, is delayed with the BR of Optimal pH
Solution constant volume is rushed, prepares 1 × 10 respectively-4mol/L、1×10-5mol/L、1×10-6mol/L、1×10-7mol/L、1×10- 8mol/L、5×10-8A series of Hg of various concentrations such as mol/L2+Solution.
Experimental method
Before measurement, embodiment 1-3 and comparative example electrode are placed in BR buffer solutions (pH=1.98), with 100mV/s's
Sweep speed under 1.20~-1.20V scan round 16 times with activated electrode.During measure, to be enriched with -1.2V current potentials in prepare liquid
For a period of time, then in the range of 1.20V~-1.20V scan round is carried out.Carbon paste composition (modification is studied first in BR solution
Agent ratio) influence；After determining ratio, the influence of liquid acidity to be measured in Electrode reaction；After optimum pH also determines, grind
Study carefully sweep speed, the influence of scope and electrode pair Hg2+Measure and its stability.
The electrochemical behavior of modified electrode
Respectively with the naked carbon paste electrodes of 1# and 3# carborundum decorating carbon paste electrode bottom liquid (KCl's containing 0.10mol/L
0.10mol/LpH=2.53BR cushioning liquid) in 1.0 × 10-4mol/L Hg2+Cyclic voltammetry scan is carried out, as a result such as Fig. 1
It is shown.
It will be seen from figure 1 that the cyclic voltammogram of 1# bare electrodes, b curves in corresponding diagram, obvious oxidation is not observed also
Parent peak；3# carborundum decorating carbon paste electrode (graphite powder quality:Carborundum quality=10:1) cyclic voltammogram, a in corresponding diagram
Curve, there is a distant reduction peak and an obvious oxidation peak.Reducing peak width and put down, oxidation peak is sharp and high,
Reducing electrode reaction speed corresponding to explanation compared with slow and oxidizing electrode reaction speed is very fast, current potential -0.290V is aoxidized caused by place
The reduzate Hg that peak correspond to be enriched in electrode surface is oxidized to Hg2+Electrode process, and in the range of certain time, peak
Electric current raises with the extension of enrichment time, shows that system has obvious adsorptivity；And the peak current at the peak can be with
Hg2+Concentration reduce and lowers, can be used as detect Hg2+The characteristic peak of concentration is to the Hg in solution2+It is measured.
Influence of the dressing agent ratio to electrode performance
2#, 3#, 4# electrode are placed in containing 1.0 × 10 respectively-4mol/L Hg2+Bottom liquid (containing 0.10mol/LKCl's
0.10mol/LpH=2.5BR cushioning liquid) in enrichment 6min, then with 100mV/s sweep speed in current potential 1.2V~-1.2V
In the range of carry out cyclic voltammetry scan, as a result as shown in Figure 2.
The cyclic voltammogram of 4# electrodes, a curves in corresponding diagram, the cyclic voltammogram of 3# electrodes, b curves in corresponding diagram, 2#
The cyclic voltammogram of electrode, c curves in corresponding diagram, as illustrated, b curves Hg2+Characteristic peak it is most obvious, illustrate graphite silty
Amount:Carborundum quality=10:1 this carbon paste ratio is optimal proportion, and 3# electrodes are optimum electrode.
The reappearance and stability of electrode
Under optimum experimental condition, with same branch 3# electrodes (only being cleaned after measure) to 1.0 × 10-4Mol/L Hg2+
Solution METHOD FOR CONTINUOUS DETERMINATION 10 times, its relative standard deviation (RSD) are 1.38%；New modified electrode is remake after measure every time,
Same 1.0 × 10-4Mol/L Hg2+Parallel determination 5 times in solution, RSD 1.11%, this shows that the modified electrode has preferably
Reappearance.
The modification carbon paste of electrode surface sensitivity decrease, can be cut down one by modified electrode after using 10 times or so
Segment, again sanding and polishing, then lied prostrate in prepare liquid with 100mV/s sweep speed in the range of 1.0V~-1.0V with circulation
Modified electrode is carried out activation process by peace method, you can obtains the effect as new electrode.By carborundum decorating carbon paste electrode (3#
Electrode) it is placed in dry and deposits 18 days at room temperature, replication every other day, measurement result is more stable (as shown in Figure 3), illustrates that this is repaiied
Decorations electrode has good stability, and service life is long.
Standard curve and detection limit
It is measured with 3# electrodes electrode of working under optimum experimental condition, the results showed that 0.10mol/LpH=2.3's
In BR cushioning liquid (KCl containing 0.10mol/L), feature peak current and Hg2+Concentration is 1.0 × 10-7Mol/L~1.0 × 10- 4It is in good linear relationship (such as Fig. 4) in the range of mol/L, linear equation is E=-0.0259lgc (Hg2+)+0.1408, linearly
Coefficient R=0.9971, its detection are limited to 3.7 × 10-8mol/L。
The selectivity of electrode
Under optimum experimental condition, in containing 1.0 × 10-6mol/L Hg2+Bottom liquid in, investigated other gold with 3# electrodes
Belong to ion such as Ni2+、Cd2+、Fe3+Disturbed condition.As a result show：Under optimum experimental condition, these ions there is no dry
Disturb, illustrate that the selectivity of electrode is preferable.
The measure of sample
Under optimum experimental condition, using standard addition method to the Hg in simulated water sample2+It is determined, experimental result is shown in
Table 1.
Hg in the simulated water sample of table 12+The measurement result of the rate of recovery
Compared with naked carbon paste electrode, with carborundum decorating carbon paste electrode to Hg2+Measure have significantly improved, carbon paste ratio
Example is graphite powder quality:Carborundum quality=10:1 modified electrode effect is best.It is electrolysed by support of 0.10mol/L KCl
Matter, with optimum electrode to Hg in the BR cushioning liquid that 0.10mol/L pH are 2.332+Enter in 1.2V~-1.2V potential ranges
Row cyclic voltammetry scan (sweep speed 100mV/s).As a result show, peak current and Hg2+Concentration is 1.0 × 10-7Mol/L~
1.0×10-4It is in good linear relation in the range of mol/L, linear equation is E=-0.0259lgc (Hg2+)+0.1408, linear phase
Relation number is R=0.9971, and its detection is limited to 3.7 × 10-8mol/L.Experiment is simple, easy to operate, high sensitivity, be it is a kind of compared with
Good measure Hg2+Method.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
- A kind of 1. preparation method of carborundum decorating carbon paste electrode, it is characterised in that：Methods described comprises the following steps that：(1) graphite powder and carborundum are put into mortar and fully mixed, add atoleine afterwards, be fully ground, mixed Pastel is made；The pastel made is filled into polyfluortetraethylene pipe and is compacted, finally electrode surface is polished, polishes and obtains Electrode；(2) in BR cushioning liquid, using three-electrode system, cyclic voltammetry scan is carried out to electrode prepared by step (1), until The cyclic voltammetry curve stablized, electrode is taken out, and is cleaned with secondary deionized water, and the carborundum that the present invention is prepared is repaiied Adorn carbon paste electrode.
- 2. the preparation method of carborundum decorating carbon paste electrode as claimed in claim 1, it is characterised in that：In step (1), graphite The mass ratio of powder and carborundum is 5-20：1.
- 3. the preparation method of carborundum decorating carbon paste electrode as claimed in claim 1, it is characterised in that：In step (1), graphite The mass ratio of powder and carborundum is 10：1.
- 4. the preparation method of carborundum decorating carbon paste electrode as claimed in claim 1, it is characterised in that：In step (2), BR delays The pH=1.0-3.0 of solution is rushed, concentration is 0.05-0.20mol/L.
- 5. the preparation method of carborundum decorating carbon paste electrode as claimed in claim 1, it is characterised in that：In step (2), BR delays The pH=2.0 of solution is rushed, concentration is 0.10mol/L.
- 6. the preparation method of carborundum decorating carbon paste electrode as claimed in claim 1, it is characterised in that：In step (2), three electricity Polar body is by Electrode (Working Electrode, WE), reference electrode (Reference Electrode, RE) and auxiliary Electrode (Counter Electrode, CE) forms, and electric current flows to auxiliary electrode from working electrode, and independent reference electrode only carries For reference potential, no current passes through.
- 7. the preparation method of carborundum decorating carbon paste electrode as claimed in claim 1, it is characterised in that：In step (2), three electricity The voltage of polar body system is 1.2V~-1.2V, and potential scanning speed is 50-150mV/s.
- 8. the preparation method of carborundum decorating carbon paste electrode as claimed in claim 7, it is characterised in that：In step (2), current potential Sweep speed is 100mV/s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710565322.4A CN107389761A (en) | 2017-07-12 | 2017-07-12 | A kind of preparation method of carborundum decorating carbon paste electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710565322.4A CN107389761A (en) | 2017-07-12 | 2017-07-12 | A kind of preparation method of carborundum decorating carbon paste electrode |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107389761A true CN107389761A (en) | 2017-11-24 |
Family
ID=60340362
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710565322.4A Pending CN107389761A (en) | 2017-07-12 | 2017-07-12 | A kind of preparation method of carborundum decorating carbon paste electrode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107389761A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110297021A (en) * | 2019-06-28 | 2019-10-01 | 济南大学 | Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074941A (en) * | 2007-06-21 | 2007-11-21 | 中国科学院长春应用化学研究所 | Method for producing carbon magma bismuth membrane electrode |
| CN101368929A (en) * | 2008-09-24 | 2009-02-18 | 福州大学 | Temperature modulating electro-chemical electrode and its heating method |
| CN102253095A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院长春应用化学研究所 | Carbon paste electrode and preparation method thereof |
| CN104483364A (en) * | 2014-12-03 | 2015-04-01 | 上海应用技术学院 | Graphene/SDS (Sodium Dodecyl Sulfate)-modified carbon paste electrode and preparation method thereof |
| CN106471646A (en) * | 2014-10-31 | 2017-03-01 | 株式会社Lg 化学 | Electrode for secondary battery, its manufacture method, the secondary cell comprising it and cable Type Rechargeable Battery |
-
2017
- 2017-07-12 CN CN201710565322.4A patent/CN107389761A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074941A (en) * | 2007-06-21 | 2007-11-21 | 中国科学院长春应用化学研究所 | Method for producing carbon magma bismuth membrane electrode |
| CN101368929A (en) * | 2008-09-24 | 2009-02-18 | 福州大学 | Temperature modulating electro-chemical electrode and its heating method |
| CN102253095A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院长春应用化学研究所 | Carbon paste electrode and preparation method thereof |
| CN106471646A (en) * | 2014-10-31 | 2017-03-01 | 株式会社Lg 化学 | Electrode for secondary battery, its manufacture method, the secondary cell comprising it and cable Type Rechargeable Battery |
| CN104483364A (en) * | 2014-12-03 | 2015-04-01 | 上海应用技术学院 | Graphene/SDS (Sodium Dodecyl Sulfate)-modified carbon paste electrode and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 郭凌雁 等: "碳化硅修饰碳糊电极测定汞离子", 《材料导报》 * |
| 韩媛媛 等: "化学修饰碳糊电极的研究进展", 《化工中间体》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110297021A (en) * | 2019-06-28 | 2019-10-01 | 济南大学 | Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Afkhami et al. | Gold nanoparticles modified carbon paste electrode as an efficient electrochemical sensor for rapid and sensitive determination of cefixime in urine and pharmaceutical samples | |
| CN104267086B (en) | Chemically modified carbon paste electrode as well as preparation method and application thereof | |
| Yosypchuk et al. | Solid amalgam composite electrode as a new sensor for the determination of biologically active compounds | |
| CN103983681B (en) | A kind of for electrochemical sensor detecting heavy metal and its preparation method and application | |
| Zhang et al. | High sensitive on-site cadmium sensor based on AuNPs amalgam modified screen-printed carbon electrodes | |
| CN105717174A (en) | Electrochemical detection method for detecting trace heavy metal ions in water with modified graphene oxide composite modified electrode | |
| CN103808779A (en) | Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode | |
| CN105928996B (en) | Electrochemical detection device for preparing and assembling graphene oxide and polyaniline modified electrode | |
| CN103278541A (en) | Electrochemical biosensor for detecting bisphenol-A, and preparation method and application thereof | |
| Xu et al. | Nitrogen, sulfur dual-doped mesoporous carbon modified glassy carbon electrode for simultaneous determination of hydroquinone and catechol | |
| CN102680549B (en) | A kind of 9-hydroxyphenyl fluorene assay method based on galvanochemistry hairpin DNA biosensor | |
| Moreno-Baron et al. | Graphite-epoxy composite as an alternative material to design mercury free working electrodes for stripping voltammetry | |
| CN102269730B (en) | Carbon paste electrode and preparation method thereof | |
| CN107389761A (en) | A kind of preparation method of carborundum decorating carbon paste electrode | |
| Xiu-Yun et al. | A novel electrochemiluminescence electrospun carbon nanofiber based sensor for atropine | |
| CN205749393U (en) | Graphene oxide and phytic acid modified electrode and electrochemical sensor thereof | |
| CN102830147B (en) | Modified electrode and applications of modified electrode on detecting micro/trace nitro aromatic compound | |
| CN110988095A (en) | Preparation method of nano material modified electrode and method for detecting heavy metal ions and phenolic compounds | |
| CN103901139A (en) | Pretreatment method for analyzing tetrabromobisphenol A in biologic urine | |
| CN105675583A (en) | Method for determination of content of verapamil hydrochloride in drug by using electrogenerated chemiluminescence behavior of composite modifier-supported pyrolytic graphite electrode | |
| CN105699455A (en) | Preparation method of ionic liquid modified carbon paste electrode | |
| CN103033545A (en) | Application of gold/cobalt hydroxide film modified glassy carbon electrode in phenol substance detection | |
| CN106018532A (en) | Preparation of graphene oxide and phytate modified electrode and electrochemical detection device assembled by graphene oxide and phytate modified electrode | |
| CN102253095A (en) | Carbon paste electrode and preparation method thereof | |
| CN102331449B (en) | Electrochemical sensor and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171124 |