CN110146577A - A kind of electrochemical sensor and its method for detecting potassium ion - Google Patents
A kind of electrochemical sensor and its method for detecting potassium ion Download PDFInfo
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Abstract
The invention discloses a kind of electrochemical sensor and its methods for detecting potassium ion, belong to analysis detection field, the preparation method of electrochemical sensor working electrode includes: that -18 crown- of 1- azepine 6 ether functional graphene oxide (Crown-GO) ultrasonic disperse in aqueous solution, is obtained Crown-GO suspension；Crown-GO suspension is uniformly dripped in polished, cleaning, drying treated glassy carbon electrode surface, Crown-GO/GCE is obtained.Electrochemical property test shows, Crown-GO composite material modified glassy carbon electrode prepared by the present invention has high sensitivity to the detection of potassium ion, low detection limit and wide detection range, in addition electrochemical sensor prepared by the present invention has many advantages, such as that electrode material preparation process is simple, environmental-friendly, easy to operate, high sensitivity, has a good application prospect and potential application value in detection potassium ion field.
Description
Technical field
The invention belongs to analysis detection field, a kind of be related to electrochemical sensor and its detect potassium ion method.
Background technique
Dominant cation of the potassium ion as intracellular fluid, plays key player, especially in human-body biological system
Adjustable blood pressure and maintenance muscle strength.However, excessive or a small amount of potassium ion will lead to many diseases, such as nephrosis, anorexia
Disease, heart disease, diabetes and Addison's disease etc..It explores thus a kind of easy, quick, highly sensitive, highly selective, inexpensive
Potassium ion detection method is of great significance.The method of detection potassium ion has much at present, such as fluorescent optical sensor, Atomic absorption
Spectrophotometry etc..However, the equipment that most of method uses is extremely complex, experimentation is cumbersome, therefore limits theirs
Practical application.And also there is certain methods detection to limit relatively high, the small disadvantage of detection range.
Relative to these technologies, electrochemical method is had the following advantages that, such as the sensitivity of good selectivity and superelevation.Cause
All do not have for potassium ion in different potential windows electroactive, therefore cyclic voltammetry and ampere chronoamperometry cannot be passed through
Etc. being tested.Electrode with Electrochemical Impedance Spectroscopy is a kind of very sensitive effective technology for testing electrochemicaUy inert component, in reality
Room is tested to be widely studied.Therefore the present invention detects potassium ion using Electrode with Electrochemical Impedance Spectroscopy.
The chemical assay of potassium ion at present is mainly ion using multiple ring crown compound such as cave crown ether or spherical crown ether
Carrier is measured, and due to there is hole in macrocyclic structure, intramolecule oxygen atom has unshared electron pair can be with metal ion knot
It closes, according to hole size, alternative combines the metal ion of different-diameter, to can reach the purpose of detection ion concentration.
But different crown ether electrodes still compare shortage to the research in terms of metal ion response pattern, it is, thus, sought for
A kind of pair of potassium ion has lower detection limit, the electrochemical sensor that detection range is big, easy to operate.
Summary of the invention
The present invention is directed to the defect of prior art, a kind of method for providing electrochemical sensor and its detecting potassium ion,
The detection limit of the electrochemical sensor detection potassium ion is low, detection range is big, high sensitivity.
Used technical solution is as follows to solve above-mentioned technical problem by the present invention:
The present invention provides a kind of electrochemical sensors, by reference electrode, to electrode and crown ether functional graphene oxide
The working electrode composition of composite material modification.
Further, the reference electrode is saturated calomel electrode, and described is platinum electrode to electrode, and the working electrode is
Glass-carbon electrode.
Further, the crown ether is 6 ether of -18 crown- of 1- azepine.
Further, the preparation method of the working electrode of the crown ether functional graphene oxide composite material modification, packet
Include following steps:
(1) crown ether functional graphene oxide ultrasonic disperse is obtained into crown ether functional graphene oxide in ultrapure water
Suspension；
(2) crown ether functional graphene oxide suspension is coated uniformly on glassy carbon electrode surface, room temperature is dried, and is preced with
The working electrode of ether functional graphene oxide composite material modified glassy carbon electrode.
Further, the glass-carbon electrode is before coating suspension, successively with 0.2 μm and 0.03 μm of alumina powder
It is processed by shot blasting, then the successively ultrasound 3-5min in nitric acid solution, ultrapure water and acetone, is dried with nitrogen.
The present invention also provides the methods that the electrochemical sensor carries out potassium ion detection, and working electrode is put into electrolysis
It is 10 in frequency range in liquid6Hz-0.01Hz, amplitude 5mV, initial voltage are that open-circuit voltage makes when time of repose is 30s
It is detected with potassium ion of the Electrode with Electrochemical Impedance Spectroscopy to various concentration.
Further, the concentration of the potassium ion is 10-15-10-4Mol/L。
Further, the electrolyte is the methylene blue solution of 1.5mM.
Technical effect of the invention is as follows:
Crown ether is as a kind of host molecule, due to the size relation between its ligand intracavity diameter and metal ion diameter,
There is very high combination selectivity to alkali and alkaline earth metal ions ion, and can with the of different sizes of ring and from different gold
Belong to ion complexation.It has been found that it can be made to show to guest molecule stronger binding force host molecule fixation.And oxygen
Graphite alkene has high specific surface area, good hydrophily and mechanical performance, has in water and most of polar organic solvents
There is good dispersion stabilization.Therefore crown ether is fixed to the high surface of graphene oxide of specific surface area by the present invention, not only can be with
Material is greatly improved to the adsorbance of metal ion, it is also possible that crown ether selectively improves the combination of metal ion.
The intracavity diameter of 6 ether of -18 crown- of 1- azepine matches the most with the diameter of potassium ion, but also can pass through amino reality
Now with the covalent bond functionalization of graphene oxide.Therefore the present invention carries out graphene oxide using 6 ether of -18 crown- of 1- azepine
Functionalization forms crown ether functional graphene oxide composite material, and repairs as the electrode of potassium ion electrochemical sensor
Exterior material.Using the mutual synergistic effect of crown ether and graphene oxide, the detection to potassium ion high sensitivity is realized, under detection
It is limited to 10-15M is limited far below the detection for making electrode potassium ion obtained with other materials.
The working electrode of crown ether functional graphene oxide composite material modification prevents electrochemical sensor to immerse to be measured
Dissolution after solution inhibits the generation of free convection, reduces ionic strength difference and limit between boundary layer and bulk solution
The formation for having made electrode surface convection current plume, makes electric current reach stable state, improves sensitivity of the electrochemical sensor to potassium ion,
Reduce the detection limit to potassium ion.
The working electrode that the present invention uses crown ether functional graphene oxide composite material to modify, due to -18 crown- of 1- azepine
The introducing of 6 ethers, on the one hand, prevent the reunion of graphene oxide, enhance detection sensitivity, on the other hand, increase electrode
To the selection coefficient of potassium ion, the influence of other ions is eliminated, reduces detection limit.Using methylenum careuleum as electrolyte, due to Asia
The blue good redox reversible of first, belongs to two electron reaction of a proton in neutral or meta-alkalescence solution, in wider pH
Preferable electrochemical response is all had in range, has widened detection range.
Crown-GO/GCE prepared by the present invention can be realized the detection of high sensitivity and very wide linear to potassium ion
Range, electrochemical sensor of the invention are 10 to the detection range of potassium ion-7-10-13M, detection are limited to 10-15M has wide
Application prospect.
Detailed description of the invention
Fig. 1 is electrochemical impedance spectrogram of the electrode of the preparation of embodiment 1 in the methylene blue solution of 1.5mM；
Fig. 2 is that Crown-GO/GCE electrode prepared by embodiment 1 is detecting the electrochemistry in various concentration potassium ion solution
Impedance spectra；
Fig. 3 is that charge transfer resistance and potassium concentration logarithm take positive linear relationship chart.
Specific embodiment
It is clearly and completely described below in conjunction with the technical solution in the embodiment of the present invention, it is clear that described reality
Applying example 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.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, With reference to embodiment
The present invention is described in further detail.
Electrode with Electrochemical Impedance Spectroscopy of the present invention is the conventional means that those skilled in the art carry out Electrode with Electrochemical Impedance Spectroscopy, herein
It does not repeat them here.
Embodiment 1
The preparation of crown ether functional graphene oxide 1. (Crown-GO) suspension
The preparation process of crown ether functional graphene oxide composite material (Crown-GO) is as follows: with ultrapure water by 10mL oxygen
Graphite alkene solution (6mg mL-1) it is diluted to 30mL, then sonic oscillation is uniform yellowish-brown to generate clarification in ice water water-bath
Then 6 ether of -18 crown- of 60mg 1- azepine and 0.8mL tetrabutylammonium hydroxide solution are added to graphene oxide by color dispersion
In solution, 85 DEG C are heated the mixture under magnetic stirring, are down to room temperature after keeping the temperature 10h.Finally with a large amount of ultrapure water from
Heart cleaning sample obtains crown ether functional graphene oxide composite material.
2. the preparation of electrode
Successively use 0.3 μm and 0.05 μm of Al2O3The glass-carbon electrode that diameter is 3mm is polished into mirror surface, after polishing
Glass-carbon electrode is successively in nitric acid solution (HNO3:H2The volume ratio of O is ultrasound 3min in 1:1), ultrapure water and acetone, is blown with nitrogen
Dry, then by the suspended drop of Crown-GO of 10 μ L on through treated glass-carbon electrode, naturally dry obtains 1- nitrogen
The glass-carbon electrode (Crown-GO/GCE) of miscellaneous 6 ether functional graphene oxide (Crown-GO) of -18 crown- modification.As a comparison, with
Same method prepares the glass-carbon electrode (GO/GCE) of graphene oxide modification.
3. the detection of potassium ion
Using Crown-GO/GCE as working electrode, saturated calomel electrode is reference electrode, platinum electrode be to electrode,
In the methylene blue solution of 1.5mM, frequency range 106Hz-0.01Hz, amplitude 5mV, initial voltage are open-circuit voltage and quiet
It sets under time 30s, the detection using Electrode with Electrochemical Impedance Spectroscopy to the potassium ion of various concentration.The concentration of potassium ion is 10-15-10-4M。
It can be seen from figure 1, compared with bare glassy carbon electrode GCE and GO/GCE, the electric charge transfer of Crown-GO/GCE electrode
Resistance is maximum, illustrates the addition due to 6 ether of -18 crown- of 1- azepine, increases the resistance between working electrode and solution interface, increases
Strong detection sensitivity, increases detection range, reduces detection limit, detection range 10-7-10-13M, detection are limited to 10-15M。
By Fig. 3, it can be seen that when potassium concentration is 10-7-10-13When Mol/L, charge transfer resistance and potassium concentration
With good linear relationship, equation of linear regression Y=143.928X+2366.857,
R2=0.983, wherein X is potassium concentration, and Y is charge transfer resistance.
Embodiment 2
For the glass-carbon electrode modified using 6 ether of -18 crown- of 1- azepine as working electrode, saturated calomel electrode is reference electrode, platinum
Electrode is to electrode, in the methylene blue solution of 1.5mM, frequency range 106Hz-0.01Hz, amplitude 5mV, initial voltage
For the detection under open-circuit voltage and time of repose 30s, using Electrode with Electrochemical Impedance Spectroscopy to the potassium ion of various concentration.Potassium ion
Concentration is 10-15-10-4Mol/L.The wherein preparation method and -18 crown- of 1- azepine of the glass-carbon electrode of 6 ether of -18 crown- of 1- azepine modification
The preparation method of the glass-carbon electrode of 6 ether functional graphene oxides modification is identical.
Embodiment 3
Using the glass-carbon electrode of 6 ether functional graphene oxide of 4- amino benzo -18- crown- modification as working electrode, it is saturated sweet
Mercury electrode is reference electrode, and platinum electrode is to electrode, in the methylene blue solution of 1.5mM, frequency range 106Hz-0.01Hz,
Amplitude is 5mV, and initial voltage is under open-circuit voltage and time of repose 30s, using Electrode with Electrochemical Impedance Spectroscopy to the potassium of various concentration from
The detection of son.The concentration of potassium ion is 10-15-10-4Mol/L.Wherein 6 ether functional graphene oxide of 4- amino benzo -18- crown-
The preparation of the glass-carbon electrode of preparation method and 6 ether functional graphene oxide of -18 crown- of 1- the azepine modification of the glass-carbon electrode of modification
Method is identical.
Embodiment 4
Using the glass-carbon electrode (Crown-GO/GCE) that 6 ether functional graphene oxide of -18 crown- of 1- azepine is modified as work
Electrode, hydrogen electrode are reference electrode, and platinum electrode is to electrode, in the methylene blue solution of 1.5mM, frequency range 106Hz-
0.01Hz, amplitude 5mV, initial voltage are under open-circuit voltage and time of repose 30s, using Electrode with Electrochemical Impedance Spectroscopy to different dense
The detection of the potassium ion of degree.The concentration of potassium ion is 10-15-10-4Mol/L。
Embodiment 5
Using the glass-carbon electrode (Crown-GO/GCE) that 6 ether functional graphene oxide of -18 crown- of 1- azepine is modified as work
Electrode, saturated calomel electrode are reference electrode, and graphite electrode is to electrode, and in the methylene blue solution of 1.5mM, frequency range is
106Hz-0.01Hz, amplitude 5mV, initial voltage are to use Electrode with Electrochemical Impedance Spectroscopy pair under open-circuit voltage and time of repose 30s
The detection of the potassium ion of various concentration.The concentration of potassium ion is 10-15-10-4Mol/L。
Electrochemical sensor described in embodiment 2-5 is shown in Table 1. to the detection limit and response range of potassium ion
Table 1
By embodiment 1-5 it is found that using different types of working electrode, reference electrode and the electrification that electrode is prepared
Sensor is learned, all smaller to the response range of potassium ion, detection limit is also higher.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements, should all fall into claims of the present invention determine protection scope in.
Claims (8)
1. a kind of electrochemical sensor, which is characterized in that by reference electrode, compound to electrode and crown ether functional graphene oxide
The working electrode composition of material modification.
2. electrochemical sensor according to claim 1, which is characterized in that the reference electrode is saturated calomel electrode,
Described is platinum electrode to electrode, and the working electrode is glass-carbon electrode.
3. electrochemical sensor according to claim 1, which is characterized in that the crown ether is 6 ether of -18 crown- of 1- azepine.
4. electrochemical sensor according to claim 1, which is characterized in that the crown ether functional graphene oxide is compound
Material modification working electrode the preparation method is as follows:
It (1) is 6mgmL by 10mL concentration with ultrapure water-1Graphene oxide solution be diluted to 30mL, then in ice water water-bath
Middle sonic oscillation is to generate the uniform yellowish-brown dispersion of clarification, then by 6 ether of -18 crown- of 60mg1- azepine and the 0.8mL tetrabutyl
Ammonia is added in graphene oxide solution, heats the mixture to 85 DEG C under magnetic stirring, is dropped after keeping the temperature 10h
Crown ether functional graphene oxide composite material is obtained to room temperature finally with the abundant eccentric cleaning sample of ultrapure water.
(2) it is suspended to be obtained into crown ether functional graphene oxide in ultrapure water for crown ether functional graphene oxide ultrasonic disperse
Liquid；
(3) crown ether functional graphene oxide suspension is coated uniformly on glassy carbon electrode surface, room temperature is dried, and crown ether function is obtained
The working electrode of graphene oxide composite material modified glassy carbon electrode can be changed.
5. electrochemical sensor according to claim 2, which is characterized in that the glass-carbon electrode coating suspension it
Before, it is successively processed by shot blasting with the alumina powder of 0.2 μm and 0.03 μm, then successively in the HNO of volume ratio 1:13With H2O
Mixed solution, ultrasound 3-5min in ultrapure water and acetone, be dried with nitrogen.
6. the method for carrying out potassium ion detection with the described in any item electrochemical sensors of claim 1-5, which is characterized in that will
Working electrode is put into electrolyte electrode and reference electrode, is 10 in frequency range6Hz-0.01Hz, amplitude 5mV, initially
Voltage is that open-circuit voltage is detected when time of repose is 30s using potassium ion of the Electrode with Electrochemical Impedance Spectroscopy to various concentration.
7. the method that electrochemical sensor as claimed in claim 6 carries out potassium ion detection, which is characterized in that the potassium ion
Concentration be 10-15-10-4Mol/L。
8. the method that electrochemical sensor as claimed in claim 7 carries out potassium ion detection, which is characterized in that the electrolyte
For the methylene blue solution of 1.5mM.
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Cited By (2)
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| CN111337559A (en) * | 2020-04-06 | 2020-06-26 | 东莞正大康地饲料有限公司 | Method for rapidly detecting potassium content in feed by using potassium ion selective electrode |
| CN112284844A (en) * | 2020-09-30 | 2021-01-29 | 温州大学 | Preparation method of composite modified glass micron pore channel and method for separating alkali metal ions by using same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111337559A (en) * | 2020-04-06 | 2020-06-26 | 东莞正大康地饲料有限公司 | Method for rapidly detecting potassium content in feed by using potassium ion selective electrode |
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| CN112284844A (en) * | 2020-09-30 | 2021-01-29 | 温州大学 | Preparation method of composite modified glass micron pore channel and method for separating alkali metal ions by using same |
| CN112284844B (en) * | 2020-09-30 | 2022-06-21 | 温州大学 | Preparation method of glass micron pore channel and separation of alkali metal ions by using same |
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