CN103499623B - A kind of combined type N 2o selects microelectrode and preparation method thereof - Google Patents
A kind of combined type N 2o selects microelectrode and preparation method thereof Download PDFInfo
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- CN103499623B CN103499623B CN201310395421.4A CN201310395421A CN103499623B CN 103499623 B CN103499623 B CN 103499623B CN 201310395421 A CN201310395421 A CN 201310395421A CN 103499623 B CN103499623 B CN 103499623B
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Abstract
The invention discloses a kind of combined type N
2o selects microelectrode and preparation method thereof, and microelectrode comprises: microelectrode main body and outer tubular cone-shaped glass sleeve pipe, and be provided with Ag/AgCl anode in microelectrode main body, Ag protects negative electrode and Pt negative electrode, three accesses micro voltage meter separately; Be marked with electrolytic solution after film in microelectrode main body, in outer tubular cone-shaped glass sleeve pipe, be marked with adsorption selection liquid; Outer tubular cone-shaped glass overlaps the sealing of effective epoxy resin sealant; Microelectrode main body and the pellosil sealing-in of outer tubular cone-shaped glass sleeve bottom; Microelectrode main body and rear two distance between two tips of cone-shaped glass sleeve pipe socket are 100-180 μm; The tip diameter of electrode body is 30-50 μm; The tip diameter of outer tubular cone-shaped glass sleeve pipe is 50-70 μm.Method comprises: assembling microelectrode main body; Assembling outer tubular cone-shaped glass sleeve pipe; Assembling combined type N
2o selects microelectrode.The present invention has that resolution is high, highly sensitive, the advantage of signal stabilization, can in-site detecting biological membrane, N in the mud flco beds of precipitation
2o space distribution rule.
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 feature.
Microsensor can be divided into separate type and combined type two kinds usually.Separate type is working electrode and reference/to electrode separation, and two kinds of electrodes need to be placed in identical electrolysis system simultaneously and just can complete mensuration.Combined type is exactly by working electrode and reference/be integrated within an electrode electrode.Compared to separated electrode, Combined type electric have test flexible, by sample environment with measure place and disturb the advantages such as little, electrochemical signals is stablized, 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 wastewater biological denitrificaion process.It is reported, because of N in sewage disposal system
2the greenhouse effect that O release produces account for sewage disposal system release all gas and produce 26% of total greenhouse effect, in nitrogen transition process the N that discharges in air
2o can cause the destruction to atmospheric environment largely.Therefore, N in nitrogen transition process is explored
2o is mechanism of production what, and carries out N
2o minimizing controls have great importance and be worth.
Summary of the invention
For N in current existing nitrogen transition process
2the defect that O study mechanism technological means exists and deficiency, the object of the invention is to, provide a kind of combined type N
2o selects microelectrode and preparation method thereof, and this microelectrode has working electrode and contrast electrode and is incorporated within an electrode electrode, discloses N from the angle of microcosmic
2the mechanism of production of O and controlling soil moist.It has, and resolution is high, highly sensitive, the advantage of signal stabilization, can in-site detecting biological membrane, N in the mud flco beds of precipitation
2o 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 the outer tubular cone-shaped glass sleeve pipe that a microelectrode main body and are 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 runs through along its inner chamber and have Ag to protect negative electrode, Pt negative electrode and Ag/AgCl anode, and three stretches out from the cylindrical end face of microelectrode main body and is connected with micro voltage meter; Described microelectrode main body cylinder shape end face epoxy resin fixed closed, cone point pellosil is closed; Described outer tubular cone-shaped glass sleeve pipe one end is taper, and the other end is cylindrical; Its inner chamber is full of adsorption selection liquid, and its cone point pellosil is closed, and the tapering point of its cylindrical end face and microelectrode main body socket-connects, 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 μm.
After the film that described microelectrode body lumen is full of, 1:1 is formulated by volume by the NaOH of KCl and 0.2mol/L of 2mol/L for electrolytic solution.
Described outer tubular cone-shaped glass sleeve pipe cone point diameter is 50-70 μm.
The ascorbic acid salt solusion of the adsorption selection liquid that described outer tubular cone-shaped glass cannula cavity is full of to be pH value be 11.5-12.5.
After described microelectrode main body and cone-shaped glass sleeve pipe are socketed, two distance between two tips are 100-180 μm.
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) tapered glass tube blank post is made: by two automatic coupling voltage regulator series connection, be fixed in the middle part of heater coil with miniature manipulater by glass tube; Glass tube lower end adhesive plaster is connected to heavy burden; After opening power, coil heats melts glass tube, when glass tube falls down soon, turns off power supply rapidly, completes first time drawing; Glass tube tip after being drawn first time again, is fixed on the middle part of heater coil upward, after opening power, when glass tube falls down soon, is increased by voltage order one rapidly, and rapid powered-down, complete 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: cut smooth with blade by most advanced and sophisticated for the blank post drawn rib thorn place, obtaining tip diameter is 30-50 μm of tapered glass tube;
3) tubular tapered glass tube electrode is assembled: closed by tapered glass tube tip pellosil, the closed degree of depth is 20-30 μm, electrolytic solution after film is filled in tubular tapered glass tube, negative electrode is protected to be inserted into tip from the cylindrical end face of tubular tapered glass tube respectively on Pt negative electrode and Ag, Pt cathode point is front, Ag protects negative electrode rear, and the two distance controlling is at 80-100 μm; Finally insert Ag/AgCl anode, obtain tubular tapered glass tube electrode;
4) microelectrode body circular end face is fixing and closed: the cylindrical end face using epoxy resin sealing tubular tapered glass tube electrode, completes fixing Pt negative electrode, Ag protection negative electrode and Ag/AgCl anode, obtains microelectrode main body;
Second step, assembling outer tubular cone-shaped glass sleeve pipe
1) outer tubular cone-shaped glass sleeve pipe blank post is made: by two automatic coupling voltage regulator series connection, be fixed in the middle part of nickel alloy heater coil with miniature manipulater by glass tube; Glass tube lower end adhesive plaster is connected to heavy burden; After opening power, coil heats melts glass tube, when glass tube falls down soon, turns off power supply rapidly, completes first time drawing; With sand paper, its tip is polished flat after drawing completes, obtained outer tubular cone-shaped glass sleeve pipe blank post;
2) outer tubular cone-shaped glass sleeve pipe blank post tip is cut flat: cut smooth with blade by most advanced and sophisticated for the blank post drawn rib thorn place, obtaining tip diameter is 50-70 μm of outer tubular cone-shaped glass sleeve pipe;
3) outer tubular cone-shaped glass casing length is cut to 3-3.5cm, its tip pellosil is closed, and injects to its inside and be full of adsorption selection liquid, i.e. obtained outer tubular cone-shaped glass sleeve pipe;
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 both keeping under the microscope, distance between two tips is 100-180 μm;
2) with epoxy resin, microelectrode main body and the outer tubular cone-shaped glass sleeve pipe place of socket-connecting are closed, namely 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: glass capillary Pt silk being put into heavy burden, be fixed in the middle part of nickel alloy heater coil with miniature manipulater, make glass capillary melt and be wrapped up completely by Pt silk under gravity by heater coil, then scrape off with blade the glass rib wrapped up at Pt silk tip and sting to make Pt silk expose;
2) corrosion and cleaning Pt silk: will cut the Pt silk after putting down as anode, carbon-point, as negative electrode, is put into KCN solution corrode with 7V power supply after being connected; After corrosion, cleaning, obtains the Pt silk after excessive erosion;
3) Pt silk is electroplated: using the Pt silk after excessive erosion as anode, carbon-point, as negative electrode, is connected to be placed in saturated chlorauric acid solution with 2V power supply and electroplates 20-30s, obtained Pt negative electrode.
Described Ag protects the making of negative electrode to comprise the following steps:
1) wrap up and cut flat Ag silk: glass capillary Ag silk being put into heavy burden, be fixed in the middle part of nickel alloy heater coil with miniature manipulater, glass capillary is made to melt and be wrapped up completely by Ag silk under gravity by heater coil, then scrape off the glass rib thorn wrapped up at Ag silk tip with blade, Ag silk is exposed;
2) corrosion and cleaning Ag silk: will cut the Ag silk after putting down as anode, carbon-point, as negative electrode, is put into KCN solution electroplate with 5V power supply after being connected, cleaning after plating, obtained Ag protection negative electrode.
The method for making of described Ag/AgCl anode is: be negative electrode using Ag silk as anode, carbon-point, is positioned in saturated KCl solution and electroplates 5s, obtained Ag/AgCl anode with 5V power supply after being connected.
Compared with prior art, the present invention has that volume is light and handy, stable performance, highly sensitive, accuracy good, respond advantage rapidly.Can to suspended state mud and the inner N of biological membrane
2o produces and measures with the spatial distribution characteristic of migration.To be commonly employed potentiality and space in environmental monitoring and biological denitrificaion study mechanism field.
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 mensuration schematic diagram.
In figure, 501. microelectrode main bodys; 502. cone-shaped glass sleeve pipes; 503. adsorption selection liquid; 504. epoxy resin; 505.Ag protects negative electrode; 506.Pt negative electrode; 507.Ag/AgCl anode; Electrolytic solution after 508. films; 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; The miniature manipulater of 6.MM33; 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, give combined type N
2o selects the structure of microelectrode; comprise microelectrode main body 501, cone-shaped glass sleeve pipe 502, Ag protect negative electrode 505, Ag/AgCl anode 507, the Pt negative electrode 506 after KCN solution corrosion, adsorption selection liquid (pH value is the ascorbic acid salt solusion of 11.5-12.5) 503, epoxy resin 504, pellosil 509 after the film in microelectrode main body in electrolytic solution (composition is KCI1mol/L, NaOH0.1mol/L) 508, 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 end, and microelectrode main body 501 one end is taper, and the other end is cylindrical; Be placed in microelectrode main body 501 Ag protect negative electrode 505, Ag/AgCl anode 507 and the Pt negative electrode 506 after KCN solution corrosion; then to electrolytic solution 508 after injectable membrane in microelectrode main body 501, and epoxy resin 504 is used to fix at microelectrode main body 501 back-end sealing.Ag protects negative electrode 505, Ag/AgCl anode 507 and Pt negative electrode 506 to access micro voltage meter respectively separately.The microelectrode main body 501 assembled is taper from one end, the other end is that cylindrical outer tubulose cone-shaped glass sleeve pipe 502 cylindrical end penetrates, and examining under a microscope microelectrode main body 501 with the tip of outer tubular cone-shaped glass sleeve pipe 502 is 100-180 μm.Externally injection adsorption selection liquid 503 in tubular tapered glass bushing 502, and use 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 bottom by epoxy resin 504 sealant sealing; Respectively by pellosil 509 sealing-in bottom microelectrode main body 501 and outer tubular cone-shaped glass sleeve pipe 502.
Wherein, the tip diameter of microelectrode main body 501 taper is 30-50 μm; After the film that its inner chamber is full of, 1:1 is formulated by volume by the NaOH of KCl and 0.2mol/L of 2mol/L for electrolytic solution 508.
Outer tubular cone-shaped glass sleeve pipe 502 cone point diameter is 50-70 μm; The adsorption selection liquid (503) that its inner chamber is full of for pH value be the ascorbic acid salt solusion of 11.5-12.5.
After microelectrode main body 501 and outer tubular cone-shaped glass sleeve pipe 502 are socketed, two distance between two tips are 100-180 μm.
The diameter of Pt negative electrode 506 is 0.1mm, purity is 99.99%; The diameter of Ag protection negative electrode 505 is 0.2mm, purity is 99.99%; Epoxy resin 508 thickness is 5-6mm.
Above-mentioned combined type N
2o selects microelectrode to make in the following manner:
The first step, assembling microelectrode main body
1) tapered glass tube blank post is made: by two automatic coupling voltage regulator series connection, be fixed in the middle part of heater coil with miniature manipulater by glass tube; Glass tube lower end adhesive plaster is connected to heavy burden; After opening power, coil heats melts glass tube, when glass tube falls down soon, turns off power supply rapidly, completes first time drawing; Glass tube tip after being drawn first time again, is fixed on the middle part of heater coil upward, after opening power, when glass tube falls down soon, is increased by voltage order one rapidly, and rapid powered-down, complete 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: cut smooth with blade by most advanced and sophisticated for the blank post drawn rib thorn place, obtaining tip diameter is 30-50 μm of tapered glass tube;
3) tubular tapered glass tube electrode is assembled: closed by tapered glass tube tip pellosil, the closed degree of depth is 20-30 μm, electrolytic solution after film is filled in tubular tapered glass tube, negative electrode is protected to be inserted into tip from the cylindrical end face of tubular tapered glass tube respectively on Pt negative electrode and Ag, Pt cathode point is front, Ag protects negative electrode rear, and the two distance controlling is at 80-100 μm; Finally insert Ag/AgCl anode, obtain tubular tapered glass tube electrode;
4) microelectrode body circular end face is fixing and closed: the cylindrical end face using epoxy resin sealing tubular tapered glass tube electrode, completes fixing Pt negative electrode, Ag protection negative electrode and Ag/AgCl anode, obtains microelectrode main body;
Second step, assembling outer tubular cone-shaped glass sleeve pipe
1) outer tubular cone-shaped glass sleeve pipe blank post is made: by two automatic coupling voltage regulator series connection, be fixed in the middle part of nickel alloy heater coil with miniature manipulater by glass tube; Glass tube lower end adhesive plaster is connected to heavy burden; After opening power, coil heats melts glass tube, when glass tube falls down soon, turns off power supply rapidly, completes first time drawing; With sand paper, its tip is polished flat after drawing completes, obtained outer tubular cone-shaped glass sleeve pipe blank post;
2) outer tubular cone-shaped glass sleeve pipe blank post tip is cut flat: cut smooth with blade by most advanced and sophisticated for the blank post drawn rib thorn place, obtaining tip diameter is 50-70 μm of outer tubular cone-shaped glass sleeve pipe;
3) outer tubular cone-shaped glass casing length is cut to 3-3.5cm, its tip pellosil is closed, and injects to its inside and be full of adsorption selection liquid, i.e. obtained outer tubular cone-shaped glass sleeve pipe;
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 both keeping under the microscope, distance between two tips is 100-180 μm;
2) with epoxy resin, microelectrode main body and the outer tubular cone-shaped glass sleeve pipe place of socket-connecting are closed, namely 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: glass capillary Pt silk being put into heavy burden, be fixed in the middle part of nickel alloy heater coil with miniature manipulater, make glass capillary melt and be wrapped up completely by Pt silk under gravity by heater coil, then scrape off with blade the glass rib wrapped up at Pt silk tip and sting to make Pt silk expose;
2) corrosion and cleaning Pt silk: will cut the Pt silk after putting down as anode, carbon-point, as negative electrode, is put into KCN solution corrode with 7V power supply after being connected; After corrosion, cleaning, obtains the Pt silk after excessive erosion;
3) Pt silk is electroplated: using the Pt silk after excessive erosion as anode, carbon-point, as negative electrode, is connected to be placed in saturated chlorauric acid solution with 2V power supply and electroplates 20-30s, obtained Pt negative electrode.
Ag protects the making of negative electrode to comprise the following steps:
1) wrap up and cut flat Ag silk: glass capillary Ag silk being put into heavy burden, be fixed in the middle part of nickel alloy heater coil with miniature manipulater, glass capillary is made to melt and be wrapped up completely by Ag silk under gravity by heater coil, then scrape off the glass rib thorn wrapped up at Ag silk tip with blade, Ag silk is exposed;
2) corrosion and cleaning Ag silk: will cut the Ag silk after putting down as anode, carbon-point, as negative electrode, is put into KCN solution electroplate with 5V power supply after being connected, cleaning after plating, obtained Ag protection negative electrode.
The method for making of Ag/AgCl anode is: be negative electrode using Ag silk as anode, carbon-point, is positioned in saturated KCl solution and electroplates 5s, obtained Ag/AgCl anode with 5V power supply after being connected.
Shown in Figure 3, adopt combined type N prepared by the present invention
2when O selects microelectrode to detect, first fix stepper motor 7 by operator's console 1, and miniature for MC-232 manipulater 6 is tightly clamped 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 in water sample and isolate; 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 more respectively with ADC-216USB converter 9.In 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 again and is converted to digital signal after micro voltage meter amplifies, converter again by signal transmission to PC computer 11, by UnisenseProfix3.09 software, signal is recorded preservation automatically.
The above is only the present invention is directed to certain combined type N
2the embodiment that O selects microelectrode to make, not does any restriction to the present invention, everyly changes any simple modification made for any of the above embodiments, change and equivalent structure according to the technology of the present invention, all still belongs in the protection domain of technical solution of the present invention.
Claims (6)
1. a combined type N
2o selects microelectrode, this microelectrode comprises the outer tubular cone-shaped glass sleeve pipe (502) that a microelectrode main body (501) and are socketed on its lower end, it is characterized in that, described microelectrode main body (501) one end is taper, and the other end is cylindrical; Its inner chamber is full of electrolytic solution (508) after film, and run through along its inner chamber and have Ag to protect negative electrode (505), Pt negative electrode (506) and Ag/AgCl anode (507), three stretches out from the cylindrical end face of microelectrode main body (501) and is connected with micro voltage meter; Described microelectrode main body (501) cylindrical end face epoxy resin (504) fixed closed, cone point pellosil (509) is closed; Described outer tubular cone-shaped glass sleeve pipe (502) one end is taper, and the other end is cylindrical; Its inner chamber is full of adsorption selection liquid (503), its cone point pellosil (509) is closed, the tapering point of its cylindrical end face and microelectrode main body (501) socket-connects, and socket place epoxy resin (504) is closed;
The tip diameter of described microelectrode main body (501) taper is 30-50 μm;
Described outer tubular cone-shaped glass sleeve pipe (502) cone point diameter is 50-70 μm.
2. 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 NaOH of KCl and 0.2mol/L of 2mol/L for electrolytic solution (508).
3. combined type N as claimed in claim 1
2o selects microelectrode, it is characterized in that, the adsorption selection liquid (503) that described outer tubular cone-shaped glass sleeve pipe (502) inner chamber is full of for pH value be the ascorbate of 11.5-12.5.
4. 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) are socketed, two distance between two tips are 100-180 μm.
5. 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) tapered glass tube blank post is made: by two automatic coupling voltage regulator series connection, be fixed in the middle part of heater coil with miniature manipulater by glass tube; Glass tube lower end adhesive plaster is connected to heavy burden; After opening power, coil heats melts glass tube, when glass tube falls down soon, turns off power supply rapidly, completes first time drawing; Glass tube tip after being drawn first time again, is fixed on the middle part of heater coil upward, after opening power, when glass tube falls down soon, is increased by voltage order one rapidly, and rapid powered-down, complete 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: cut smooth with blade by most advanced and sophisticated for the blank post drawn rib thorn place, obtaining tip diameter is 30-50 μm of tapered glass tube;
3) tubular tapered glass tube electrode is assembled: closed by tapered glass tube tip pellosil, the closed degree of depth is 20-30 μm, electrolytic solution after film is filled in tubular tapered glass tube, negative electrode is protected to be inserted into tip from the cylindrical end face of tubular tapered glass tube respectively on Pt negative electrode and Ag, Pt cathode point is front, Ag protects negative electrode rear, and the two distance controlling is at 80-100 μm; Finally insert Ag/AgCl anode, obtain tubular tapered glass tube electrode;
4) microelectrode body circular end face is fixing and closed: the cylindrical end face using epoxy resin sealing tubular tapered glass tube electrode, completes fixing Pt negative electrode, Ag protection negative electrode and Ag/AgCl anode, obtains microelectrode main body;
Second step, assembling outer tubular cone-shaped glass sleeve pipe
1) outer tubular cone-shaped glass sleeve pipe blank post is made: by two automatic coupling voltage regulator series connection, be fixed in the middle part of nickel alloy heater coil with miniature manipulater by glass tube; Glass tube lower end adhesive plaster is connected to heavy burden; After opening power, coil heats melts glass tube, when glass tube falls down soon, turns off power supply rapidly, completes first time drawing; With sand paper, its tip is polished flat after drawing completes, obtained outer tubular cone-shaped glass sleeve pipe blank post;
2) outer tubular cone-shaped glass sleeve pipe blank post tip is cut flat: cut smooth with blade by most advanced and sophisticated for the blank post drawn rib thorn place, obtaining tip diameter is 50-70 μm of outer tubular cone-shaped glass sleeve pipe;
3) outer tubular cone-shaped glass casing length is cut to 3-3.5cm, its tip pellosil is closed, and injects to its inside and be full of adsorption selection liquid, i.e. obtained outer tubular cone-shaped glass sleeve pipe;
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 both keeping under the microscope, distance between two tips is 100-180 μm;
2) with epoxy resin, microelectrode main body and the outer tubular cone-shaped glass sleeve pipe place of socket-connecting are closed, namely complete combined type N
2o selects the making of microelectrode;
The making of described Pt negative electrode comprises the following steps:
1) wrap up and cut flat Pt silk: glass capillary Pt silk being put into heavy burden, be fixed in the middle part of nickel alloy heater coil with miniature manipulater, make glass capillary melt and be wrapped up completely by Pt silk under gravity by heater coil, then scrape off with blade the glass rib wrapped up at Pt silk tip and sting to make Pt silk expose;
2) corrosion and cleaning Pt silk: will cut the Pt silk after putting down as anode, carbon-point, as negative electrode, is put into KCN solution corrode with 7V power supply after being connected; After corrosion, cleaning, obtains the Pt silk after excessive erosion;
3) Pt silk is electroplated: using the Pt silk after excessive erosion as anode, carbon-point, as negative electrode, is connected to be placed in saturated chlorauric acid solution with 2V power supply and electroplates 20-30s, obtained Pt negative electrode;
Ag protects the making of negative electrode to comprise the following steps:
1) wrap up and cut flat Ag silk: glass capillary Ag silk being put into heavy burden, be fixed in the middle part of nickel alloy heater coil with miniature manipulater, glass capillary is made to melt and be wrapped up completely by Ag silk under gravity by heater coil, then scrape off the glass rib thorn wrapped up at Ag silk tip with blade, Ag silk is exposed;
2) corrosion and cleaning Ag silk: will cut the Ag silk after putting down as anode, carbon-point, as negative electrode, is put into KCN solution electroplate with 5V power supply after being connected, cleaning after plating, obtained Ag protection negative electrode.
6. combined type N as claimed in claim 5
2o selects the preparation method of microelectrode, and it is characterized in that, the method for making of Ag/AgCl anode is: be negative electrode using Ag silk as anode, carbon-point, is positioned in saturated KCl solution and electroplates 5s, obtain Ag/AgCl anode with 5V power supply after being connected.
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