CN110568042A - Electrochemical analysis device adopting nano boron-doped diamond membrane electrode and application thereof - Google Patents
Electrochemical analysis device adopting nano boron-doped diamond membrane electrode and application thereof Download PDFInfo
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- CN110568042A CN110568042A CN201910994548.5A CN201910994548A CN110568042A CN 110568042 A CN110568042 A CN 110568042A CN 201910994548 A CN201910994548 A CN 201910994548A CN 110568042 A CN110568042 A CN 110568042A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The invention provides an electrochemical analysis device adopting a nano boron-doped diamond membrane electrode, which comprises a base, an electrolytic cell and an electrolytic cell cover, wherein the base is provided with a plurality of grooves; the top of the base is provided with an electrolytic cell with an integrated structure, the base is also provided with a motor, and an output shaft of the motor extends to the bottom in the electrolytic cell and is connected with a stirring blade; the side wall of the electrolytic cell is provided with a reference electrode; the electrolytic cell cover is correspondingly provided with an auxiliary electrode and a working electrode; the working electrode is a nano boron-doped diamond membrane electrode; the electrolytic cell cover is also provided with an air vent; the lower part of the electrolytic cell is also provided with an electrolytic cell liquid outlet. The device disclosed by the invention is simple in structure and convenient to use, effectively avoids the complexity of the construction process of a three-electrode system, and simultaneously solves the problem of poor reproducibility caused by unfixed relative distance of three electrodes during construction; the invention also protects the application of the electrochemical analysis device in the detection of the chemical oxygen demand of the water body during sewage treatment, and the electrochemical analysis device has wider measurement range which can reach 7324.5mg/L and has higher practical significance.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to an electrochemical analysis device adopting a nanometer boron-doped diamond membrane electrode and application thereof.
Background
with social development and technological progress, people's environmental awareness is gradually strengthened, and detection and control of water pollution are more and more paid attention. At present, the major water body pollution in China is mainly organic pollution, and Chemical Oxygen Demand (COD) is an important parameter for evaluating the organic pollution degree of the water body. COD is the amount of an oxidizing agent consumed in treating a water sample with a specific strong oxidizing agent such as potassium dichromate or potassium permanganate under strong acid and heating conditions, and is expressed in terms of the equivalent oxygen concentration (mg/L). The standard method for measuring the COD of the water body is a potassium dichromate titration method, the method is accurate in measurement and good in reproducibility, but the operation process is too complicated, reflux titration is required in the test, and the consumed time is long. In recent years, new methods such as ultraviolet absorption spectroscopy, photocatalytic methods, photoelectrocatalysis methods, and electrochemical methods have appeared. The ultraviolet absorption spectrometry is to measure organic matters according to different absorptions of the organic matters in water under ultraviolet light with specific wavelength, but the ultraviolet absorption difference of different organic matters is large, so that the measurement of complex wastewater is easy to deviate; the photocatalytic method and the photoelectrocatalysis method oxidize reducing substances in wastewater by using cavities or free radicals during ultraviolet irradiation, and obtain corresponding COD by detecting electric quantity or current value, but the method is easy to generate deviation on wastewater with low light transmittance such as high turbidity, high chroma and the like. Relatively speaking, the COD is measured by the electrochemical method by applying a constant potential to a three-electrode system including a working electrode, electrolyzing water to generate hydroxyl radicals, wherein the hydroxyl radicals are used as a strong oxidant, organic matters in water can be quickly oxidized to generate an electric signal, and the concentration of the COD in the water is measured by utilizing the size of the generated response signal.
At present, most of electrodes used for testing COD by using electrochemical method are AgO/CuO composite electrodes or PbO2The electrode, however, AgO/CuO composite electrode has not high oxidation capacity, PbO2The electrode is not corrosion-resistant, and the heavy metal ions are eluted in an acidic or alkaline medium, so that the detection signal is interfered, and therefore, the design of an electrochemical analysis device with a proper electrode material is necessary.
Disclosure of Invention
the invention aims to solve the defects of the technology and provides an electrochemical analysis device adopting the nano boron-doped diamond membrane electrode, the device is reasonable in design and simple to operate, the nano boron-doped diamond membrane electrode is used as a working electrode, strong oxidant hydroxyl radicals with high oxidation-reduction potential are generated on the surface of the working electrode in the detection process, organic pollutants in water can be completely oxidized, the nano boron-doped diamond membrane electrode is corrosion-resistant and pollution-resistant, harmful substances cannot be generated in the detection process and after the detection is finished, and the device is safe and environment-friendly.
in order to achieve the purpose, the invention adopts the technical scheme that:
The electrochemical analysis device adopting the nanometer boron-doped diamond membrane electrode comprises a base, an electrolytic cell and an electrolytic cell cover which can be hermetically connected with the electrolytic cell;
the top of the base is provided with an electrolytic cell with an integrated structure, the base is of a hollow structure and is internally provided with a motor, an output shaft of the motor penetrates through the base and extends to the inner bottom of the electrolytic cell, and the top of the output shaft is connected with a stirring blade;
a reference electrode mounting hole is formed in the side wall of the electrolytic cell, a reference electrode is arranged in the reference electrode mounting hole, and the front end of the reference electrode is positioned in the electrolytic cell;
An auxiliary electrode mounting hole and a working electrode mounting hole are arranged on the electrolytic cell cover in a penetrating manner, an auxiliary electrode is arranged in the auxiliary electrode mounting hole, a working electrode is arranged in the working electrode mounting hole, and the front ends of the auxiliary electrode and the working electrode are both positioned in the electrolytic cell;
The working electrode is a nano boron-doped diamond membrane electrode;
The electrolytic cell cover is also provided with an air vent;
The lower part of the side wall of the electrolytic cell is also communicated with a liquid outlet of the electrolytic cell, and a sealing plug is arranged on the liquid outlet of the electrolytic cell.
preferably, the electrochemical analyzer further comprises an electrochemical analyzer and a computer provided with workstation software of the electrochemical analyzer, the computer is electrically connected with the electrochemical analyzer, and the electrochemical analyzer is electrically connected with the reference electrode, the auxiliary electrode and the working electrode in a one-to-one correspondence manner through leads.
Preferably, the base is detachably connected with a jacket capable of surrounding the electrolytic cell, the jacket is internally provided with a heating wire and a temperature sensor, the jacket is externally provided with a controller, the controller can be electrically connected with an external power supply, and the controller is electrically connected with the heating wire and the temperature sensor.
Preferably, the sealing plug is a silicone sealing plug.
preferably, the electrolytic cell is in threaded connection with the electrolytic cell cover, and the electrolytic cell is made of transparent organic glass.
Preferably, the vent is further provided with a three-way piston for ventilation.
Preferably, the reference electrode is a saturated calomel electrode or an Ag/AgCl electrode, and the auxiliary electrode is a platinum electrode.
preferably, the upper part of the side wall of the electrolytic cell is also provided with an electrolyte adding port, and the electrolyte adding port is detachably connected with a sealing cover.
The invention also protects the application of the electrochemical analysis device in COD detection in sewage treatment.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the electrochemical analysis device, the reference electrode is arranged on the inner wall of the electrolytic cell, and the auxiliary electrode and the working electrode are arranged on the electrolytic cell cover, so that the position relation among the three electrodes and the relative distance among the three electrodes are defined, and the problem of poor reproducibility caused by the change of the relative distance in the process of building the device is effectively avoided;
2. According to the invention, through the arrangement of the motor and the stirring blade, the liquid to be detected can be uniformly stirred without additionally using a stirrer, the use is convenient, and the stirring blade is wrapped with the anti-corrosion coating, so that the influence of the stirring blade on the liquid to be detected is effectively avoided, and the service life of the stirring blade is ensured;
3. According to the invention, through the arrangement of the liquid outlet of the electrolytic cell and the electrolyte inlet, the replacement and the supplement of the electrolyte during the detection are facilitated, the electrolyte is discharged after the detection is finished, the electrolytic cell can be cleaned under the condition that the electrolytic cell and the electrolytic cell cover are not disassembled, and the working electrode is cleaned by replacing the sulfuric acid solution;
4. The electrochemical analysis device adopts the nanometer boron-doped diamond membrane electrode as the working electrode, and in the detection process, a certain voltage is applied between the boron-doped diamond membrane electrode and the platinum electrode, so that strong oxidant hydroxyl free radicals with high oxidation-reduction potential are generated on the surface of the boron-doped diamond membrane electrode, the oxidation-reduction potential (2.8V) of the boron-doped diamond membrane electrode is far higher than that of dichromate ions (1.4V), organic pollutants in water can be completely oxidized, the detection accuracy is high, the measurement range is wider, and the measurement range can reach 7324.5 mg/L; and other harmful substances are not generated in the detection process, so that the method is safe and environment-friendly;
5. The invention adopts a boron-doped diamond film electrode as a working electrode, wherein sp is formed between carbon atoms in diamond3the hybrid mode is combined, the structure is very stable, the chemical stability is high, and the activation can be carried out under a higher anode potential to remove the pollution on the surface; meanwhile, the boron-doped diamond membrane electrode has the advantages of pollution resistance, corrosion resistance and the like, and is long in service life.
drawings
FIG. 1 is a schematic view showing the construction of an electrochemical analysis apparatus of the present invention without a jacket;
FIG. 2 is a schematic view showing the structure of an electrochemical analysis apparatus according to the present invention in the case where the apparatus has a jacket.
In the figure: 1. a base; 2. an electrolytic cell; 3. an electrolytic cell cover; 4. a motor; 5. a reference electrode; 6. an auxiliary electrode; 7. a working electrode; 8. a vent; 9. a liquid outlet of the electrolytic cell; 10. an electrolyte inlet; 11. and a jacket.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments. The scope of the invention is not limited to the specific embodiments.
Example 1
the electrochemical analysis device adopting the nano boron-doped diamond membrane electrode comprises a base 1, an electrolytic cell 2 and an electrolytic cell cover 3 which can be hermetically connected with the electrolytic cell 2, wherein the base 1 is used for providing support for the device and placing a motor, and the electrolytic cell 2 and the electrolytic cell cover 3 provide places for an electrochemical analysis process;
In order to facilitate the replacement of the electrolytic cell 2 or the electrolytic cell cover 3 when problems occur and facilitate the cleaning after the use, the electrolytic cell 2 and the electrolytic cell cover 3 are detachably connected, namely, connected through threads, and a sealing ring is arranged at the connecting part of the electrolytic cell 2 and the electrolytic cell cover 3; in order to facilitate the observation of the state of the detection process, the electrolytic cell 2 is made of transparent organic glass material;
The top of the base 1 is provided with an electrolytic cell 2 with an integrated structure, the base 1 is of a hollow structure and is internally provided with a motor 4, an output shaft of the motor 4 penetrates through the base 1 and extends to the inner bottom of the electrolytic cell 2, the top of the output shaft is connected with a stirring blade, the stirring blade is coated with an anti-corrosion coating, and the coating can be made of polytetrafluoroethylene materials; meanwhile, in order to prevent the liquid in the electrolytic cell 2 from flowing into the base 1, the connection parts of the output shaft and the base 1 and the electrolytic cell 2 are sealed, and the part of the output shaft extending into the electrolytic cell 2 is also coated with an anti-corrosion coating;
in order to avoid the influence of temperature difference on a detection structure during testing at different times, a temperature adjusting device is added in the device, namely a jacket 11 which can surround the electrolytic cell 2 is detachably connected on the base 1, an electric heating wire and a temperature sensor are arranged in the jacket 11, a controller is arranged outside the jacket 11, the controller can be electrically connected with an external power supply, and the controller is electrically connected with the electric heating wire and the temperature sensor; thus, in the detection process, the constant temperature is set through the controller, and when the environmental temperature is lower, the electric heating wire is started to heat the electrolytic cell 2, so that the detection temperature is ensured;
A reference electrode mounting hole is formed in the side wall of the electrolytic cell 2, a reference electrode 5 is arranged in the reference electrode mounting hole, the front end of the reference electrode 5 is positioned in the electrolytic cell 2, and the reference electrode 5 is a saturated calomel electrode or an Ag/AgCl electrode;
An auxiliary electrode mounting hole and a working electrode mounting hole are arranged on the electrolytic cell cover 3 in a penetrating manner, an auxiliary electrode 6 is arranged in the auxiliary electrode mounting hole, a working electrode 7 is arranged in the working electrode mounting hole, and the front ends of the auxiliary electrode 6 and the working electrode 7 are both positioned in the electrolytic cell 2;
the working electrode 7 is a nanometer boron-doped diamond membrane electrode, and the auxiliary electrode 6 is a platinum electrode;
The electrolytic cell cover 3 is also provided with an air vent 8, and in order to facilitate the introduction of different gases in the testing process, the air vent 8 is also provided with a three-way piston for air exchange;
the lower part of the side wall of the electrolytic cell 2 is also provided with an electrolytic cell liquid outlet 9, the electrolytic cell liquid outlet 9 is provided with a sealing plug, the sealing plug is a silica gel sealing plug, and the silica gel sealing plug can plug the electrolytic cell liquid outlet 9 tightly, can not be corroded by sewage and has long service life;
In order to facilitate the addition of the electrolyte, the upper part of the side wall of the electrolytic cell 2 is also provided with an electrolyte adding port 10, and the electrolyte adding port 10 can be detachably connected with a sealing cover; therefore, the sample can be easily added in the detection process, and after the detection is finished, the electrolytic cell can be cleaned by combining the electrolyte adding port with the electrolytic cell liquid outlet, and the working electrode can be cleaned by adding a sulfuric acid solution.
in order to realize the detection of COD, an electrochemical analyzer and a computer provided with workstation software of the electrochemical analyzer are added into the device, the computer is electrically connected with the electrochemical analyzer, the electrochemical analyzer is electrically connected with the reference electrode 5, the auxiliary electrode 6 and the working electrode 7 in a one-to-one correspondence manner through leads, so that when the COD of the sewage is detected, constant voltage can be directly applied between the working electrode and the auxiliary electrode for testing.
In specific implementation, adding a liquid to be detected as an electrolyte into an electrolytic cell 2, covering an electrolytic cell cover 3, adding the electrolyte with specific pH into the electrolytic cell 2, starting a stirrer 4 to stir, applying a constant potential, adding test liquids with different COD concentrations into the electrolytic cell 2 after the background current is stable, and recording a response current signal; and then measuring the standard sample and the actual sewage sample under the same test condition, drawing a standard curve, comparing a current signal obtained by measuring the actual sewage sample with the standard curve, and calculating to obtain the COD.
Example 2
COD detection was carried out on municipal sewage and chemical plant wastewater using the electrochemical analysis apparatus of example 1. The nanometer boron-doped diamond film electrode is used as a working electrode, and the saturated calomel electrode is used as a reference electrode.
The electrochemical analysis device of example 1 can detect the organic contaminants (nitrophenol, hydroquinone, salicylic acid, etc.) that are common in chemical and pharmaceutical wastewater, and the intermediates (oxalic acid, etc.) that are common when electrolyzing organic contaminants, including reference substances (sucrose, glucose, glutamic acid, etc.) that are common in COD tests. Glucose, sucrose, p-hydroxybenzoic acid, hydroquinone and the like are used as standard substances, high-purity water is used for preparing a simulation water sample, and then municipal sewage and chemical plant wastewater are used as actual water samples and are detected by using the electrochemical analysis device.
Firstly, adding 10mL of sodium sulfate solution with the mass concentration of 25mM into an electrolytic cell 2, applying a constant potential of 1.4V to a three-electrode system, recording a corresponding current response value after background current is stable, then injecting a simulated water sample and an actual water sample with the concentration of 2mLCOD of 10mg/L into the electrolytic cell 2, and finding that the background current reaches a relatively stable state after about 75s before the actual water sample is not added; after a water sample is added, the oxidation current is rapidly increased, about 10s reaches 95% of the current stable stage, and the organic matter response characteristic is good.
then, the electrochemical analysis device is used for detecting simulated water samples of glucose, sucrose, nitrophenol, hydroquinone, p-hydroxybenzoic acid and tetracycline to obtain data of COD values and response currents of various substances, namely, the corresponding current of nitrobenzene with the COD concentration of 50mg/L is 98.2 muA, the corresponding current of sucrose with the COD concentration of 50mg/L is 96.1 muA, the corresponding current of hydroquinone with the COD concentration of 150mg/L is 147.4 muA, the corresponding current of tetracycline with the COD concentration of 150mg/L is 138.5 muA, and the corresponding current of glucose with the COD concentration of 200mg/L is 401.5 muA, and the test results are subjected to linear fitting to obtain the corresponding detection limit of 0.3 mg/L.
Finally, the electrochemical analysis device and the potassium dichromate standard method are adopted to detect municipal sewage and chemical plant wastewater, the pH of the wastewater is 5-9, the detection results are shown in table 1, and the results show that the relative error of the measurement value of the electrochemical analysis device is less than +/-5.1%, and the electrochemical analysis device has high detection accuracy.
TABLE 1 table of results of electrochemical analysis apparatus and potassium dichromate standard method in wastewater determination
Example 3
The electrochemical analyzer of example 1 was used to detect waste water from the food industry, which mainly contains organic substances such as ethyl lactate. A nanometer boron-doped diamond film electrode is used as a working electrode, and a saturated calomel electrode is used as a reference electrode.
Standard test solutions with different COD concentrations are added into 15mL of sodium nitrate solution with 0.5mol/L, pH of 7, the obtained solution is taken as electrolyte, added into an electrolytic cell 2, applied with 2.00V of voltage, recorded with response current signals, measured for three times on average, averaged, fitted to obtain a calibration curve of the current value and the standard sample COD, and then the food industry wastewater is detected, wherein the detection results are shown in Table 2.
TABLE 2 table of results of electrochemical analysis apparatus and potassium dichromate standard method in wastewater of food industry
Example 4
Pharmaceutical wastewater containing mainly organic substances such as adamantane and amines was detected by the electrochemical analyzer of example 1. A nanometer boron-doped diamond film electrode is used as a working electrode, and a saturated Ag/AgCl electrode is used as a reference electrode.
The standard test solution with different COD concentrations is added into 10mL of sodium sulfate solution with 0.2mol/L, pH of 2, the obtained liquid is taken as electrolyte, added into an electrolytic cell 2, applied with 2.40V voltage, recorded with response current signals, measured for three times on average, averaged, fitted to obtain a calibration curve of current value and standard sample COD, and then the pharmaceutical wastewater is detected, and the detection result is shown in Table 3.
TABLE 3 test result table of electrochemical analysis device and potassium dichromate standard method in pharmaceutical wastewater
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (9)
1. The electrochemical analysis device adopting the nano boron-doped diamond membrane electrode is characterized by comprising a base (1), an electrolytic cell (2) and an electrolytic cell cover (3) which can be hermetically connected with the electrolytic cell (2);
The electrolytic cell (2) of an integrated structure is arranged at the top of the base (1), the base (1) is of a hollow structure, a motor (4) is arranged in the base (1), an output shaft of the motor (4) penetrates through the base (1) and extends to the inner bottom of the electrolytic cell (2), and the top of the output shaft is connected with a stirring blade;
a reference electrode mounting hole is formed in the side wall of the electrolytic cell (2), a reference electrode (5) is arranged in the reference electrode mounting hole, and the front end of the reference electrode (5) is positioned in the electrolytic cell (2);
an auxiliary electrode mounting hole and a working electrode mounting hole penetrate through the electrolytic cell cover (3), an auxiliary electrode (6) is arranged in the auxiliary electrode mounting hole, a working electrode (7) is arranged in the working electrode mounting hole, and the front ends of the auxiliary electrode (6) and the working electrode (7) are both positioned in the electrolytic cell (2);
the working electrode (7) is a nano boron-doped diamond membrane electrode;
The electrolytic cell cover (3) is also provided with an air vent (8);
the lower part of the side wall of the electrolytic cell (2) is also communicated with an electrolytic cell liquid outlet (9), and a sealing plug is arranged on the electrolytic cell liquid outlet (9).
2. the electrochemical analysis device adopting the nano boron-doped diamond membrane electrode as set forth in claim 1, further comprising an electrochemical analyzer and a computer equipped with workstation software of the electrochemical analyzer, wherein the computer is electrically connected with the electrochemical analyzer, and the electrochemical analyzer is electrically connected with the reference electrode (5), the auxiliary electrode (6) and the working electrode (7) in a one-to-one correspondence manner through leads.
3. The electrochemical analysis device adopting the nano boron-doped diamond membrane electrode as set forth in claim 1, wherein a jacket (11) capable of surrounding the electrolytic cell (2) is detachably connected to the base (1), a heating wire and a temperature sensor are disposed in the jacket (11), a controller is disposed outside the jacket (11), the controller can be electrically connected with an external power supply, and the controller is electrically connected with both the heating wire and the temperature sensor.
4. The electrochemical analysis device adopting the nano boron-doped diamond membrane electrode according to claim 1, wherein the sealing plug is a silica gel sealing plug.
5. The electrochemical analysis device adopting the nano boron-doped diamond membrane electrode as set forth in claim 1, wherein the electrolytic cell (2) is connected with the electrolytic cell cover (3) by a screw thread, and the electrolytic cell (2) is made of transparent organic glass material.
6. the electrochemical analysis device adopting the nano boron-doped diamond membrane electrode as set forth in claim 1, wherein a three-way piston for ventilation is further provided on the vent (8).
7. the electrochemical analysis device adopting the nano boron-doped diamond membrane electrode as set forth in claim 1, wherein the reference electrode (5) is a saturated calomel electrode or an Ag/AgCl electrode, and the auxiliary electrode (6) is a platinum electrode.
8. the electrochemical analysis device adopting the nano boron-doped diamond membrane electrode as set forth in claim 1, wherein an electrolyte inlet (10) is further provided on an upper portion of a sidewall of the electrolytic cell (2), and a sealing cover is detachably connected to the electrolyte inlet (10).
9. The use of the electrochemical analyzer with the nano boron-doped diamond membrane electrode according to any one of claims 1 to 8, wherein the electrochemical analyzer is used in chemical oxygen demand measurement in sewage treatment.
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