CN103499623A - Composite N2O selective microelectrode and preparation method thereof - Google Patents
Composite N2O selective microelectrode and preparation method thereof Download PDFInfo
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- CN103499623A CN103499623A CN201310395421.4A CN201310395421A CN103499623A CN 103499623 A CN103499623 A CN 103499623A CN 201310395421 A CN201310395421 A CN 201310395421A CN 103499623 A CN103499623 A CN 103499623A
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Abstract
The invention discloses a composite N2O selective microelectrode and a preparation method thereof. The microelectrode comprises a microelectrode main body and an external tubular conical glass sleeve. An Ag/AgCl anode, an Ag protection cathode, and a Pt cathode are arranged in the microelectrode main body. The three are respectively connected to a micro-voltmeter. A post-membrane electrolyte is injected in the microelectrode main body. A selective absorption liquid is injected in the external tubular conical glass sleeve. The external tubular conical glass sleeve is sealed by using epoxy resin sealant. The microelectrode main body and the bottom of the external tubular conical glass sleeve are connected in a sealed state by using a silicone membrane. After the microelectrode main body and the conical glass sleeve are sleeved, the distance between two tips is 100-180mum. The diameter of the tip of the electrode main body is 30-50mum. The tip diameter of the external tubular conical glass sleeve is 50-70mum. The method comprises the steps that: the microelectrode main body is assembled; the external tubular conical glass sleeve is assembled; and the composite N2O selective microelectrode is assembled. The microelectrode provided by the invention has the advantages of high resolution, high sensitivity, and stable signal. With the microelectrode, N2O spatial distribution regularity in biofilm and sludge floc precipitate layer can be determined on site.
Description
Technical field
The invention belongs to environmental microorganism and environmental monitoring technology field, relate generally to a kind of combined type N
2o selects microelectrode and preparation method thereof.
Background technology
For decades recently, microsensor (microelectrode) starts to become emerging electrochemical measuring technology gradually, due to its tip small (being generally tens microns even several microns).Microsensor can show good chemical property under this yardstick, not only can measure micron-sized concentration levels of species, and its signal also has highly sensitive characteristics.
Microsensor can be divided into two kinds of separate type and combined types usually.Separate type is working electrode and reference/to electrode separation, two kinds of electrodes need to be placed in identical electrolysis system simultaneously and just can complete mensuration.Combined type is exactly by within working electrode and reference/electrode is integrated into to an electrode.Than separated electrode, Combined type electric have test flexible, be subject to the sample environment and measure place and disturb little, the advantages such as electrochemical signals stable, the resolution high selectivity is good, safety simple to operate.Because its good performance has become the emerging research tool of field of environment protection and method.
N
2o discharges a kind of strong greenhouse gas in the wastewater biological denitrificaion process.It is reported, in sewage disposal system because of N
2the greenhouse effect that O discharge to produce account for sewage disposal system and discharge all gas and produce 26% of total greenhouse effect, in the nitrogen transition process to the N discharged in atmosphere
2o can cause the destruction to atmospheric environment largely.Therefore, explore N in the nitrogen transition process
2o is mechanism of production what, and carries out N
2the O minimizing is controlled and is had great importance and be worth.
Summary of the invention
For N at present existing nitrogen transition process
2defect and deficiency that O mechanism investigative technique means exist, the object of the invention is to, and a kind of combined type N is provided
2o selects microelectrode and preparation method thereof, and this microelectrode has working electrode and contrast electrode and, within electrode is incorporated into to an electrode, from the angle of microcosmic, discloses N
2the mechanism of production of O and control approach.It has advantages of that resolution is high, highly sensitive, signal stabilization, can the in-site detecting biological membrane, the N in the mud flco beds of precipitation
2the O space distribution rule.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of combined type N
2o selects microelectrode, and this microelectrode comprises a microelectrode main body and an outer tubular cone-shaped glass sleeve pipe that is socketed on its lower end, and described microelectrode main body one end is taper, and the other end is cylindrical; Its inner chamber is full of electrolytic solution after film, and is penetrated with Ag protection negative electrode, Pt negative electrode and Ag/AgCl anode along its inner chamber, and the three stretches out with the micro voltage meter and is connected from the cylindrical end face of microelectrode main body; The fixing sealing of epoxy resin for described microelectrode main body cylinder shape end face, cone point seals with pellosil; Described outer tubular cone-shaped glass sleeve pipe one end is taper, and the other end is cylindrical; Its inner chamber is full of the selection adsorption liquid, and its cone point seals with pellosil, and the tapering point of its cylindrical end face and microelectrode main body socket-connects, the socket place epoxy resin sealing.
Combined type N of the present invention
2o selects microelectrode to be further characterized in that:
The tip diameter of described microelectrode main body taper is 30-50 μ m.
After the film that described microelectrode main body inner chamber is full of, 1:1 is formulated by volume by the KCl of 2mol/L and the NaOH of 0.2mol/L for electrolytic solution.
Described outer tubular cone-shaped glass sleeve pipe cone point diameter is 50-70 μ m.
The selection adsorption liquid that described outer tubular cone-shaped glass cannula cavity is full of is the ascorbic acid salt solusion that the pH value is 11.5-12.5.
After described microelectrode main body and the socket of cone-shaped glass sleeve pipe, two distance between two tips are 100-180 μ m.
Correspondingly, the present invention gives a kind of combined type N
2o selects the preparation method of microelectrode, comprises the steps:
The first step, assembling microelectrode main body
1) make tapered glass tube blank post: by two automatic coupling voltage regulator series connection, with miniature manipulater, glass tube is fixed on to the heater coil middle part; The glass tube lower end is connected to heavy burden with adhesive plaster; After opening power, coil heats is melted glass tube, when glass tube falls down soon, turns off rapidly power supply, completes for the first time and draws; Glass tube tip after drawing for the first time again, is fixed on the middle part of heater coil upward, after opening power, when glass tube falls down soon, rapidly a step voltage increased, and rapid powered-down, complete for the second time and draw; With sand paper, its tip is polished flat after drawing completes, make tapered glass tube blank post;
2) tapered glass tube blank post tip is cut flat: with blade, the most advanced and sophisticated rib thorn of the blank post that drawn place is cut smoothly, obtaining tip diameter is 30-50 μ m tapered glass tube;
3) assemble tubular tapered glass tube electrode: the tapered glass tube tip is sealed with pellosil, the sealing degree of depth is 20-30 μ m, to filling with electrolytic solution after film in tubular tapered glass tube, Pt negative electrode and Ag protection negative electrode are inserted into to tip from the cylindrical end face of tubular tapered glass tube respectively, the Pt cathode point is front, Ag protection negative electrode is rear, and the two distance is controlled at 80-100 μ m; Finally insert the Ag/AgCl anode, obtain tubular tapered glass tube electrode;
4) the fixing and sealing of microelectrode main body circular end surface: use the cylindrical end face of the tubular tapered glass tube electrode of epoxy resin sealing, complete Pt negative electrode, Ag are protected to the fixing of negative electrode and Ag/AgCl anode, obtain the microelectrode main body;
Second step, assembling outer tubular cone-shaped glass sleeve pipe
1) make outer tubular cone-shaped glass sleeve pipe blank post: by two automatic coupling voltage regulator series connection, with miniature manipulater, glass tube is fixed on to nickel alloy heater coil middle part; The glass tube lower end is connected to heavy burden with adhesive plaster; After opening power, coil heats is melted glass tube, when glass tube falls down soon, turns off rapidly power supply, completes for the first time and draws; With sand paper, its tip is polished flat after drawing completes, make outer tubular cone-shaped glass sleeve pipe blank post;
2) outer tubular cone-shaped glass sleeve pipe blank post tip is cut flat: with blade, the most advanced and sophisticated rib thorn of the blank post that drawn place is cut smoothly, obtaining tip diameter is 50-70 μ m outer tubular cone-shaped glass sleeve pipe;
3) outer tubular cone-shaped glass casing length is cut to 3-3.5cm, its tip is sealed with pellosil, and injects and be full of the selection adsorption liquid to its inside, makes outer tubular cone-shaped glass sleeve pipe;
The 3rd step, assembling combined type N
2o selects microelectrode
1) microelectrode main body tapering point is inserted from outer tubular cone-shaped glass sleeve pipe cylinder end face, and to keep under the microscope the two distance between two tips be 100-180 μ m;
2) with epoxy resin, microelectrode main body and the outer tubular cone-shaped glass sleeve pipe place of socket-connecting are sealed, complete combined type N
2o selects the making of microelectrode.
The inventive method is further characterized in that:
The making of described Pt negative electrode comprises the following steps:
1) wrap up and cut flat Pt silk: the glass capillary of the Pt silk being put into to heavy burden, be fixed in nickel alloy heater coil middle part with miniature manipulater, make the glass capillary fusing and under Action of Gravity Field, the Pt silk wrapped up fully by heater coil, then with blade, scraping off the glass rib wrapped up at Pt silk tip and sting so that the Pt silk exposes;
2) corrosion with clean the Pt silk: will cut Pt silk after flat as anode, carbon-point is as negative electrode, and puts into KCN solution after the 7V power supply is connected and corroded; Clean after corrosion, obtain the Pt silk after excessive erosion;
3) electroplate the Pt silk: by the Pt silk after excessive erosion, as anode, carbon-point, as negative electrode, is connected to be placed in saturated chlorauric acid solution with the 2V power supply and electroplates 20-30s, makes the Pt negative electrode.
The making of described Ag protection negative electrode comprises the following steps:
1) wrap up and cut flat Ag silk: the glass capillary of the Ag silk being put into to heavy burden, be fixed in nickel alloy heater coil middle part with miniature manipulater, make the glass capillary fusing and under Action of Gravity Field, the Ag silk wrapped up fully by heater coil, then scrape off with blade the glass rib thorn wrapped up at Ag silk tip, the Ag silk is exposed;
2) corrosion with clean the Ag silk: will cut Ag silk after flat as anode, carbon-point is as negative electrode, and puts into KCN solution after the 5V power supply is connected and electroplated, and after electroplating, cleans, and makes Ag and protects negative electrode.
The method for making of described Ag/AgCl anode is: using the Ag silk as anode, carbon-point is negative electrode, electroplate 5s with being positioned in saturated KCl solution after the 5V power supply is connected, make the Ag/AgCl anode.
Compared with prior art, the present invention has that volume is light and handy, stable performance, highly sensitive, accuracy good, respond advantage rapidly.Can be to suspended state mud and the inner N of biological membrane
2o produces with the spatial distribution characteristic of migration and is measured.In environmental monitoring and biological denitrificaion mechanism research field be commonly employed potentiality and space.
The accompanying drawing explanation
Below in conjunction with the drawings and the specific embodiments, the present invention will be further described.
Fig. 1 is combined type N
2o selects microelectrode to assemble figure.
Fig. 2 is combined type N
2o selects the most advanced and sophisticated partial enlarged drawing of microelectrode.
Fig. 3 is combined type N
2o selects microelectrode and computing machine to be used in conjunction the mensuration schematic diagram.
In figure, 501. microelectrode main bodys; 502. cone-shaped glass sleeve pipe; 503. selection adsorption liquid; 504. epoxy resin; 505.Ag protection negative electrode; 506.Pt negative electrode; 507.Ag/AgCl anode; 508. electrolytic solution after film; 509. pellosil;
In Fig. 3,1. operator's console; 2. heelpiece; 3. net; 4. matrix to be measured; 5 combined type N
2o selects microelectrode; 6.MM33 miniature manipulater; 7. stepper motor; 8.PHM210 micro voltage meter; 9.ADC-216USB converter; 10.MC-232 microcontroller; 11.PC computer.
Embodiment
Below in conjunction with instantiation, the present invention is further illustrated, but described example is not construed as limiting the invention.
Shown in Fig. 1, Fig. 2, provided combined type N
2o selects the structure of microelectrode; comprise selection adsorption liquid (the ascorbic acid salt solusion that pH value is 11.5-12.5) 503, epoxy resin 504, pellosil 509 in electrolytic solution (composition is KCI1mol/L, NaOH0.1mol/L) 508 after microelectrode main body 501, cone-shaped glass sleeve pipe 502, Ag protection negative electrode 505, Ag/AgCl anode 507, the Pt negative electrode 506 after the KCN solution corrosion, the film in the microelectrode main body, cone-shaped glass sleeve pipe.
In the structure of this microelectrode, outer tubular cone-shaped glass sleeve pipe 502 is socketed on microelectrode main body 501 lower ends, and microelectrode main body 501 1 ends are taper, and the other end is cylindrical; Be placed into Ag protection negative electrode 505, Ag/AgCl anode 507 and the Pt negative electrode 506 after the KCN solution corrosion in microelectrode main body 501; then to electrolytic solution 508 after the interior injectable membrane of microelectrode main body 501, and use epoxy resin 504 to fix at microelectrode main body 501 back-end sealings.Ag protection negative electrode 505, Ag/AgCl anode 507 and Pt negative electrode 506 access respectively the micro voltage meter separately.The microelectrode main body 501 assembled is that taper, the other end are that cylindrical outer tubulose cone-shaped glass sleeve pipe 502 cylindrical ends penetrate from an end, and examining under a microscope microelectrode main body 501 is 100-180 μ m with the tip of outer tubular cone-shaped glass sleeve pipe 502.To outside, adsorption liquid 503 is selected in the interior injection of tubular tapered glass bushing 502, and uses epoxy resin connecting sealed microelectrode main body 501 and outer tubular cone-shaped glass sleeve pipe 502.Be socketed on the outer tubular cone-shaped glass sleeve pipe 502 of microelectrode main body 501 bottoms by epoxy resin 504 sealant sealings; Microelectrode main body 501 and outer tubular cone-shaped glass sleeve pipe 502 bottoms are respectively by pellosil 509 sealing-ins.
Wherein, the tip diameter of microelectrode main body 501 tapers is 30-50 μ m; After the film that its inner chamber is full of, 1:1 is formulated by volume by the KCl of 2mol/L and the NaOH of 0.2mol/L for electrolytic solution 508.
Outer tubular cone-shaped glass sleeve pipe 502 cone point diameters are 50-70 μ m; The ascorbic acid salt solusion that the selection adsorption liquid (503) that its inner chamber is full of is 11.5-12.5 for the pH value.
After microelectrode main body 501 and 502 sockets of outer tubular cone-shaped glass sleeve pipe, two distance between two tips are 100-180 μ m.
The diameter of Pt negative electrode 506 is that 0.1mm, purity are 99.99%; The diameter of Ag protection negative electrode 505 is that 0.2mm, purity are 99.99%; Epoxy resin 508 thickness are 5-6mm.
Above-mentioned combined type N
2o selects microelectrode to make in the following manner:
The first step, assembling microelectrode main body
1) make tapered glass tube blank post: by two automatic coupling voltage regulator series connection, with miniature manipulater, glass tube is fixed on to the heater coil middle part; The glass tube lower end is connected to heavy burden with adhesive plaster; After opening power, coil heats is melted glass tube, when glass tube falls down soon, turns off rapidly power supply, completes for the first time and draws; Glass tube tip after drawing for the first time again, is fixed on the middle part of heater coil upward, after opening power, when glass tube falls down soon, rapidly a step voltage increased, and rapid powered-down, complete for the second time and draw; With sand paper, its tip is polished flat after drawing completes, make tapered glass tube blank post;
2) tapered glass tube blank post tip is cut flat: with blade, the most advanced and sophisticated rib thorn of the blank post that drawn place is cut smoothly, obtaining tip diameter is 30-50 μ m tapered glass tube;
3) assemble tubular tapered glass tube electrode: the tapered glass tube tip is sealed with pellosil, the sealing degree of depth is 20-30 μ m, to filling with electrolytic solution after film in tubular tapered glass tube, Pt negative electrode and Ag protection negative electrode are inserted into to tip from the cylindrical end face of tubular tapered glass tube respectively, the Pt cathode point is front, Ag protection negative electrode is rear, and the two distance is controlled at 80-100 μ m; Finally insert the Ag/AgCl anode, obtain tubular tapered glass tube electrode;
4) the fixing and sealing of microelectrode main body circular end surface: use the cylindrical end face of the tubular tapered glass tube electrode of epoxy resin sealing, complete Pt negative electrode, Ag are protected to the fixing of negative electrode and Ag/AgCl anode, obtain the microelectrode main body;
Second step, assembling outer tubular cone-shaped glass sleeve pipe
1) make outer tubular cone-shaped glass sleeve pipe blank post: by two automatic coupling voltage regulator series connection, with miniature manipulater, glass tube is fixed on to nickel alloy heater coil middle part; The glass tube lower end is connected to heavy burden with adhesive plaster; After opening power, coil heats is melted glass tube, when glass tube falls down soon, turns off rapidly power supply, completes for the first time and draws; With sand paper, its tip is polished flat after drawing completes, make outer tubular cone-shaped glass sleeve pipe blank post;
2) outer tubular cone-shaped glass sleeve pipe blank post tip is cut flat: with blade, the most advanced and sophisticated rib thorn of the blank post that drawn place is cut smoothly, obtaining tip diameter is 50-70 μ m outer tubular cone-shaped glass sleeve pipe;
3) outer tubular cone-shaped glass casing length is cut to 3-3.5cm, its tip is sealed with pellosil, and injects and be full of the selection adsorption liquid to its inside, makes outer tubular cone-shaped glass sleeve pipe;
The 3rd step, assembling combined type N
2o selects microelectrode
1) microelectrode main body tapering point is inserted from outer tubular cone-shaped glass sleeve pipe cylinder end face, and to keep under the microscope the two distance between two tips be 100-180 μ m;
2) with epoxy resin, microelectrode main body and the outer tubular cone-shaped glass sleeve pipe place of socket-connecting are sealed, complete combined type N
2o selects the making of microelectrode.
Wherein, the making of Pt negative electrode comprises the following steps:
1) wrap up and cut flat Pt silk: the glass capillary of the Pt silk being put into to heavy burden, be fixed in nickel alloy heater coil middle part with miniature manipulater, make the glass capillary fusing and under Action of Gravity Field, the Pt silk wrapped up fully by heater coil, then with blade, scraping off the glass rib wrapped up at Pt silk tip and sting so that the Pt silk exposes;
2) corrosion with clean the Pt silk: will cut Pt silk after flat as anode, carbon-point is as negative electrode, and puts into KCN solution after the 7V power supply is connected and corroded; Clean after corrosion, obtain the Pt silk after excessive erosion;
3) electroplate the Pt silk: by the Pt silk after excessive erosion, as anode, carbon-point, as negative electrode, is connected to be placed in saturated chlorauric acid solution with the 2V power supply and electroplates 20-30s, makes the Pt negative electrode.
The making of Ag protection negative electrode comprises the following steps:
1) wrap up and cut flat Ag silk: the glass capillary of the Ag silk being put into to heavy burden, be fixed in nickel alloy heater coil middle part with miniature manipulater, make the glass capillary fusing and under Action of Gravity Field, the Ag silk wrapped up fully by heater coil, then scrape off with blade the glass rib thorn wrapped up at Ag silk tip, the Ag silk is exposed;
2) corrosion with clean the Ag silk: will cut Ag silk after flat as anode, carbon-point is as negative electrode, and puts into KCN solution after the 5V power supply is connected and electroplated, and after electroplating, cleans, and makes Ag and protects negative electrode.
The method for making of Ag/AgCl anode is: using the Ag silk as anode, carbon-point is negative electrode, electroplate 5s with being positioned in saturated KCl solution after the 5V power supply is connected, make the Ag/AgCl anode.
Combined type N shown in Figure 3, as to adopt the present invention to prepare
2when O selects microelectrode to be detected, at first pass through fixedly stepper motor 7 of operator's console 1, and the miniature manipulater 6 of MC-232 is tightly clamped to the combined type N assembled
2o selects microelectrode 5, and by combined type N
2o selects microelectrode 5 to be connected with stepper motor 7, then by combined type N
2o selects microelectrode 5 to put into the matrix 4(water sample to be measured be arranged on operator's console 1 heelpiece 2), be provided with net 3 isolation in water sample; Combined type N
2o selects microelectrode 5 to be connected with PHM210 micro voltage meter 8, PHM210 micro voltage meter 8 is connected with ADC-216USB converter 9, stepper motor 7 is connected with MC-232 microcontroller 10, and then MC-232 microcontroller 10 is connected with PC computer 11 respectively with ADC-216USB converter 9 again.In the mensuration system, combined type N
2o selects the response signal of microelectrode to be passed to PHM210 micro voltage meter 8 by external micro voltage line, signal is passed to ADC-216USB converter 9 and is converted to digital signal again after the micro voltage meter amplifies, converter is passed to signal PC computer 11 again, by Unisense Profix3.09 software, signal is recorded to preservation automatically.
The above is only to the present invention is directed to certain combined type N
2the embodiment that O selects microelectrode to make, not do any restriction to the present invention, every according to the technology of the present invention to any simple modification made for any of the above embodiments, change and equivalent structure variation, all still belong in the protection domain of technical solution of the present invention.
Claims (10)
1. a combined type N
2o selects microelectrode, and this microelectrode comprises a microelectrode main body (501) and an outer tubular cone-shaped glass sleeve pipe (502) that is socketed on its lower end, it is characterized in that, described microelectrode main body (501) one ends are taper, and the other end is cylindrical; Its inner chamber is full of electrolytic solution (508) after film, and is penetrated with Ag protection negative electrode (505), Pt negative electrode (506) and Ag/AgCl anode (507) along its inner chamber, and the three stretches out with the micro voltage meter and is connected from the cylindrical end face of microelectrode main body (501); Cylindrical epoxy resin (504) fixed closed for end face of described microelectrode main body (501), pellosil sealing (509) for cone point; Described outer tubular cone-shaped glass sleeve pipe (502) one ends are taper, and the other end is cylindrical; Its inner chamber is full of selects adsorption liquid (503), and it is pellosil (509) sealing for cone point, and the tapering point of its cylindrical end face and microelectrode main body (501) socket-connects, epoxy resin for socket place (504) sealing.
2. combined type N as claimed in claim 1
2o selects microelectrode, it is characterized in that, the tip diameter of described microelectrode main body (501) taper is 30-50 μ m.
3. combined type N as claimed in claim 1
2o selects microelectrode, it is characterized in that, after the film that described microelectrode main body (501) inner chamber is full of, 1:1 is formulated by volume by the KCl of 2mol/L and the NaOH of 0.2mol/L for electrolytic solution (508).
4. combined type N as claimed in claim 1
2o selects microelectrode, it is characterized in that, described outer tubular cone-shaped glass sleeve pipe (502) cone point diameter is 50-70 μ m.
5. combined type N as claimed in claim 1
2o selects microelectrode, it is characterized in that, the ascorbate that the selection adsorption liquid (503) that described outer tubular cone-shaped glass sleeve pipe (502) inner chamber is full of is 11.5-12.5 for the pH value.
6. combined type N as claimed in claim 1
2o selects microelectrode, it is characterized in that, after described microelectrode main body (501) and cone-shaped glass sleeve pipe (502) socket, two distance between two tips are 100-180 μ m.
7. a combined type N
2o selects the preparation method of microelectrode, it is characterized in that, comprises the steps:
The first step, assembling microelectrode main body
1) make tapered glass tube blank post: by two automatic coupling voltage regulator series connection, with miniature manipulater, glass tube is fixed on to the heater coil middle part; The glass tube lower end is connected to heavy burden with adhesive plaster; After opening power, coil heats is melted glass tube, when glass tube falls down soon, turns off rapidly power supply, completes for the first time and draws; Glass tube tip after drawing for the first time again, is fixed on the middle part of heater coil upward, after opening power, when glass tube falls down soon, rapidly a step voltage increased, and rapid powered-down, complete for the second time and draw; With sand paper, its tip is polished flat after drawing completes, make tapered glass tube blank post;
2) tapered glass tube blank post tip is cut flat: with blade, the most advanced and sophisticated rib thorn of the blank post that drawn place is cut smoothly, obtaining tip diameter is 30-50 μ m tapered glass tube;
3) assemble tubular tapered glass tube electrode: the tapered glass tube tip is sealed with pellosil, the sealing degree of depth is 20-30 μ m, to filling with electrolytic solution after film in tubular tapered glass tube, Pt negative electrode and Ag protection negative electrode are inserted into to tip from the cylindrical end face of tubular tapered glass tube respectively, the Pt cathode point is front, Ag protection negative electrode is rear, and the two distance is controlled at 80-100 μ m; Finally insert the Ag/AgCl anode, obtain tubular tapered glass tube electrode;
4) the fixing and sealing of microelectrode main body circular end surface: use the cylindrical end face of the tubular tapered glass tube electrode of epoxy resin sealing, complete Pt negative electrode, Ag are protected to the fixing of negative electrode and Ag/AgCl anode, obtain the microelectrode main body;
Second step, assembling outer tubular cone-shaped glass sleeve pipe
1) make outer tubular cone-shaped glass sleeve pipe blank post: by two automatic coupling voltage regulator series connection, with miniature manipulater, glass tube is fixed on to nickel alloy heater coil middle part; The glass tube lower end is connected to heavy burden with adhesive plaster; After opening power, coil heats is melted glass tube, when glass tube falls down soon, turns off rapidly power supply, completes for the first time and draws; With sand paper, its tip is polished flat after drawing completes, make outer tubular cone-shaped glass sleeve pipe blank post;
2) outer tubular cone-shaped glass sleeve pipe blank post tip is cut flat: with blade, the most advanced and sophisticated rib thorn of the blank post that drawn place is cut smoothly, obtaining tip diameter is 50-70 μ m outer tubular cone-shaped glass sleeve pipe;
3) outer tubular cone-shaped glass casing length is cut to 3-3.5cm, its tip is sealed with pellosil, and injects and be full of the selection adsorption liquid to its inside, makes outer tubular cone-shaped glass sleeve pipe;
The 3rd step, assembling combined type N
2o selects microelectrode
1) microelectrode main body tapering point is inserted from outer tubular cone-shaped glass sleeve pipe cylinder end face, and to keep under the microscope the two distance between two tips be 100-180 μ m;
2) with epoxy resin, microelectrode main body and the outer tubular cone-shaped glass sleeve pipe place of socket-connecting are sealed, complete combined type N
2o selects the making of microelectrode.
8. combined type N as claimed in claim 7
2o selects the preparation method of microelectrode, it is characterized in that, the making of described Pt negative electrode comprises the following steps:
1) wrap up and cut flat Pt silk: the glass capillary of the Pt silk being put into to heavy burden, be fixed in nickel alloy heater coil middle part with miniature manipulater, make the glass capillary fusing and under Action of Gravity Field, the Pt silk wrapped up fully by heater coil, then with blade, scraping off the glass rib wrapped up at Pt silk tip and sting so that the Pt silk exposes;
2) corrosion with clean the Pt silk: will cut Pt silk after flat as anode, carbon-point is as negative electrode, and puts into KCN solution after the 7V power supply is connected and corroded; Clean after corrosion, obtain the Pt silk after excessive erosion;
3) electroplate the Pt silk: by the Pt silk after excessive erosion, as anode, carbon-point, as negative electrode, is connected to be placed in saturated chlorauric acid solution with the 2V power supply and electroplates 20-30s, makes the Pt negative electrode.
9. combined type N as claimed in claim 7
2o selects the preparation method of microelectrode, it is characterized in that, the making of Ag protection negative electrode comprises the following steps:
1) wrap up and cut flat Ag silk: the glass capillary of the Ag silk being put into to heavy burden, be fixed in nickel alloy heater coil middle part with miniature manipulater, make the glass capillary fusing and under Action of Gravity Field, the Ag silk wrapped up fully by heater coil, then scrape off with blade the glass rib thorn wrapped up at Ag silk tip, the Ag silk is exposed;
2) corrosion with clean the Ag silk: will cut Ag silk after flat as anode, carbon-point is as negative electrode, and puts into KCN solution after the 5V power supply is connected and electroplated, and after electroplating, cleans, and makes Ag and protects negative electrode.
10. combined type N as claimed in claim 7
2o selects the preparation method of microelectrode, it is characterized in that, the method for making of Ag/AgCl anode is: using the Ag silk as anode, carbon-point is negative electrode, electroplate 5s with being positioned in saturated KCl solution after the 5V power supply is connected, make the Ag/AgCl anode.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103868964A (en) * | 2014-03-12 | 2014-06-18 | 西安建筑科技大学 | Compound H2S microelectrode and preparation method thereof |
| CN114609219A (en) * | 2022-03-07 | 2022-06-10 | 南京师范大学 | Microelectrode for monitoring inorganic nitrogen ion concentration in real time and preparation method and application thereof |
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| CN103868964A (en) * | 2014-03-12 | 2014-06-18 | 西安建筑科技大学 | Compound H2S microelectrode and preparation method thereof |
| CN114609219A (en) * | 2022-03-07 | 2022-06-10 | 南京师范大学 | Microelectrode for monitoring inorganic nitrogen ion concentration in real time and preparation method and application thereof |
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| CN103499623B (en) | 2015-12-23 |
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