CN201335817Y - Dissolved oxygen microelectrode - Google Patents
Dissolved oxygen microelectrode Download PDFInfo
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- CN201335817Y CN201335817Y CNU2008202284332U CN200820228433U CN201335817Y CN 201335817 Y CN201335817 Y CN 201335817Y CN U2008202284332 U CNU2008202284332 U CN U2008202284332U CN 200820228433 U CN200820228433 U CN 200820228433U CN 201335817 Y CN201335817 Y CN 201335817Y
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- electrode
- dissolved oxygen
- platinum filament
- outer sleeve
- tip
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Abstract
The utility model discloses a dissolved oxygen microelectrode, which comprises an external sleeve filled with a post- membrane electrolyte, wherein one end of the external sleeve is in a tip shape which is filled with a silicone rubber membrane; an induction cathode made of a platinum wire, an Ag / AgCl internal reference electrode and a silver protection cathode are arranged at the center of the external sleeve, and the distance between the tips of the silver protection cathode and the platinum wire is 50um to 200um; and epoxy resin is closed between the external sleeve and a capillary glass tube, and the leading wires of the platinum wire induction cathode, the Ag / AgCl internal reference electrode and the silver protection cathode are respectively welded on the corresponding wiring terminals of electrode plugs. The dissolved oxygen microelectrode has small volume, high resolution, short response time, high sensitivity, wide scope of application, simple preparation method and low cost, can rapidly determine the dissolved oxygen of micro-environment in activated sludge flocs or biofilms, and has broad application prospects in the microstudy of environmental microbiology, biological wastewater treatment and other fields.
Description
Technical field
The utility model relates to a kind of microelectrode and preparation thereof, particularly a kind of dissolved oxygen micro electrode.
Background technology
Water body environment is closely bound up with human life, and the quality of water quality is having a strong impact on the healthy of people.The content of DO in the water body environment (dissolved oxygen DO) is one of important indicator of contaminated degree of water body and ecologic environment quality, other index is closely related in it and the water such as BOD, COD, is culture fishery, waterworks, the requisite monitoring project of sewage treatment plant and water quality monitoring department.In environmental monitoring, measuring in the water the classic methods of DO is iodimetric titration, but iodimetric titration is fixed to the interference that the whole non-on-line determination process of titration is subject to multiple factor from sampling.Particularly for the mensuration of extreme anoxic or anaerobic water sample, classical titrimetry can draw higher even wrong conclusion.And microelectrode has high resolution and sensitivity, can solve this difficult problem effectively.
In addition, utilize the high resolving power of oxygen microelectrode can also measure water-bed photosynthesis.Carsten etc. determine the gross photosynthesis of microalgae by the minimizing speed of measuring oxygen concentration in bottom, the deep-sea light disappearance back 4s.If initially reducing speed with oxygen represents photosynthesis rate, the maximum rate of measuring with the oxygen microelectrode is higher by 32% than the value that classic method records.The research of Yoshiyuki etc. also shows, when light intensity reaches 1050 μ mol photons/m/s, the 0.5mm place can record the net photosynthesis amount on the sediment top layer, and when light intensity reached 1900 μ mol photons/m/s, the 1.0mm place can record the gross photosynthesis amount on the sediment top layer.Along with light intensity increases, net photosynthesis speed and respiration also increase thereupon.In light reaction and dark reaction, the concentration of oxygen in the METHOD FOR CONTINUOUS DETERMINATION sediment different levels shows that photosynthesis changes rapidly with the change of light intensity, and oxygen concentration is stable in 200s.
The oxygen microelectrode also has a wide range of applications in aerobe is handled.In the aerobe processing procedure of sewage, exist the anaerobism microcell in active sludge or the biological membrane.But traditional method lacks accurate instrument, can only measure the dissolved oxygen concentration in the aeration tank, and powerless to the oxygen distribution situation in active sludge and the biological membrane microcell.Oxygen microelectrode tip can reach 1 μ m, can be deep into active sludge inside, measures the oxygen concentration of different levels, thereby determines that oxygen concentration is to the influence of nitrification and denitrification in single-activity mud flco.Anaerobic processes in Andreas etc. the have utilized different microelectrode simultaneous determinations single-activity mud flco are studied the back to 6 active sludge flcos and are found that wherein anaerobic zone does not appear in 4 flcos in aeration process, so denitrification rate is very slow; Denitrification rate is but very fast in other 2 flcos, and its reason may be that the density of these 2 flcos will cause the appearance of anaerobic zone obviously greater than preceding 4 flcos.Hisashi Sato etc. studies show that, the penetration depth of oxygen in flco depends on the oxygen concentration in the pond, the nitrated aerobic district that occurs in, nitrated speed increases with oxygen concentration, when oxygen concentration reaches 40 μ M, it is stable that rate of nitrification keeps, and when oxygen concentration during at 10 μ M～35 μ M scopes, nitrification and denitrification takes place simultaneously in aerating activated sludge.Hisashi Sato etc. utilizes O
2, NH
4 +, NO
2 -, NO
3 -Combine with the pH microelectrode and to have carried out the macroscopic view and the micro-analysis of nitrification and denitrification in the membrane aeration biomembrane reactor.
Present employed dissolved oxygen electrode, volume is big, and the response time is long, and sensitivity is generally not high, and complex operation, and also rests on macroscopical basis mostly.For at present also powerless in the water environment microcell, particularly biological wastewater treatment process as the variation of dissolved oxygen DO in active sludge, the inner infinitesimal environment of biological membrane.Therefore, develop a kind of new dissolved oxygen micro electrode for dissolved oxygen concentration in various mud, the sediment interior microscopic zone in the research water body, and in the biological wastewater treatment process, the concentration change situation of dissolved oxygen DO in the inner infinitesimal of active sludge or the biological membrane zone, thereby further inquire into biological sewage treatment mechanism, optimization process technology, significant.
Summary of the invention
At defective or deficiency that above-mentioned prior art exists, the purpose of this utility model is, a kind of novel dissolved oxygen micro electrode is provided, and this dissolved oxygen micro electrode most advanced and sophisticated superfine can fast measuring active sludge flco or the dissolved oxygen DO of the interior infinitesimal environment of biological membrane.
In order to realize above-mentioned task, the utility model is taked following technical solution:
A kind of dissolved oxygen micro electrode is characterized in that, this dissolved oxygen micro electrode comprises that is filled with an electrolytical outer sleeve behind the film, and outer sleeve is made by soda-lime glass, and the one end is tip-shape, and the tip is marked with silicone rubber membrane; The induction negative electrode of being made by platinum filament is equipped with in the centre of described outer sleeve, and described platinum filament has one section platinum filament to expose outside glass capillary being positioned at the outer sleeve point, and the exposed platinum filament back that is corroded is gold-plated; Inner contrast electrode of Ag/AgCl and silver protection negative electrode also are housed in the outer sleeve; wherein; the induction negative electrode is connected with the inner contrast electrode of Ag/AgCl; the silver guard electrode is inserted separately; the tip of silver guard electrode is 50 μ m～200 μ m apart from the tip of platinum filament; by the epoxy resin sealing, the lead-in wire of platinum filament induction negative electrode, the inner contrast electrode of Ag/AgCl and silver protection negative electrode is welded in respectively on the corresponding binding post of electrode plug between outer sleeve and the glass capillary.
The dissolved oxygen micro electrode volume of the utility model preparation is little, resolution is high, the response time is short, highly sensitive, applied widely, the preparation method is simple, and is with low cost.Microexamination in fields such as environmental microbiology and biological sewage treatment has a wide range of applications.
Description of drawings
Fig. 1 is the synoptic diagram that dissolved oxygen micro electrode and computing machine are united use.Label is wherein represented respectively: 1, PC: the sectional view that is used to show mensuration; 2, A/D converter (model is ADC-216USB), 3, power controller (model is MC-232), 4, current amplifier (model is PA2000), 5, miniature manipulater (model is MM33), 6, micro-step motor (MMS), 7, microcontroller support (model is LS-18), 8, dissolved oxygen micro electrode, 9, testing sample, the line between per two parts is concentric cable.
Fig. 2 is the structural map of dissolved oxygen micro electrode, and label is wherein represented respectively: 10. soda-lime glass (schott8418 glass), 11, filamentary silver, 12, electrolytic solution behind the film; 13, epoxy resin, 14, glass capillary, 15, the Ag/AgCl silk, 16, platinum filament.
Fig. 3 is the structural representation at dissolved oxygen micro electrode tip.Label is wherein represented respectively: 11, filamentary silver, 16, platinum filament, 17, spun gold, 18, silicone rubber membrane.
The utility model is described in further detail below in conjunction with accompanying drawing.
Embodiment
Referring to Fig. 2 and Fig. 3, according to a kind of dissolved oxygen micro electrode of the technical solution of the utility model preparation, comprise an outer sleeve 10 that is filled with electrolyte 12 behind the film, outer sleeve 10 is made by soda-lime glass, and the one end is tip-shape, and its tip is less than 50 μ m.The tip is marked with silicone rubber membrane 18; The induction negative electrode of being made by platinum filament 16 is equipped with in the centre of described outer sleeve 10, and described platinum filament 16 has one section platinum filament to expose outside glass capillary 14 being positioned at outer sleeve 10 points, and the exposed platinum filament back that is corroded is gold-plated; Inner contrast electrode of Ag/AgCl and silver protection negative electrode also are housed in the outer sleeve 10; wherein; the induction negative electrode is connected with the inner contrast electrode of Ag/AgCl; the silver guard electrode is inserted separately; the tip of silver guard electrode is 50 μ m～200 μ m apart from the tip of platinum filament 16; by epoxy resin 13 sealings, the lead-in wire of platinum filament induction negative electrode, the inner contrast electrode of Ag/AgCl and silver protection negative electrode is welded in respectively on the corresponding binding post of electrode plug between outer sleeve 10 and the glass capillary 14.
The tip of above-mentioned platinum filament 16 is corroded to 25 μ m, and gold-plated length is 10-20 μ m.Silver protection negative electrode is made for most advanced and sophisticated superfine filamentary silver, filamentary silver outer wrap glass, the 50 μ m that are corroded of its most advanced and sophisticated 1cm place.The length of silicone rubber membrane is 10 μ m～20 μ m.
The purity of described platinum filament 16 is 99.99%, and outer sleeve is 8418 soda-lime glass.
Above-mentioned dissolved oxygen micro electrode is made in the following manner:
1, the platinum filament 16 of a diameter 0.1mm, purity 99.99% is put into glass capillary 14, this glass capillary 14 is fixed on the heater coil centre position, opening power is regulated transformer, makes glass capillary 14 fusings and it is wrapped up platinum filament 16 under action of gravity.
2, an end 2cm of platinum filament 16 is long glass is removed, and makes one section platinum filament expose out, is anode with this exposed platinum filament, and other gets a carbon-point and makes negative electrode, all places saturated KCN solution (saturation degree 71.6%) to form the loop.
3, in saturated potassium cyanide solution, about the about 20s of electrolysis, the length place of platinum filament one end 1cm can eroded to the about 25 μ m of diameter under the alternating voltage of 7V, under the voltage of 2V, continue the corrosion several seconds again, can obtain thinner tip.The alcohol flushing of the sulfuric acid of water, 10% concentration, 70% concentration successively after platinum filament 16 corrosion.
4, be anode with platinum filament 16, spun gold 17 is made negative electrode, places saturated chlorauric acid solution to electroplate about 30s in most advanced and sophisticated corrosion place of platinum filament under the 1.5V DC voltage, and gold-plated length is about 10-20 μ m.
After above-mentioned steps 1 to 4 is finished, promptly make the induction negative electrode;
5, the filamentary silver 11 of getting a diameter 0.2mm is made the protection negative electrodes, and with filamentary silver 11 outer wrap upper glasses, glass is removed at 1cm place at one end by heater coil, again the filamentary silver of removing behind the glass 11 is corroded into 50 μ m in saturated potassium cyanide solution tip.
6, a soda-lime glass (Schott8418 glass) is vertically fixed on the miniature manipulater, by heater coil and adjusting transformer, heating twice can draw an end of Schott8418 glass for tip-shape, most advanced and sophisticated diameter is several microns, as the outer sleeve 10 of oxygen microelectrode 8.
7, polish with the tip of fine sandpaper outer sleeve 10, be coated in silicone rubber membrane 18 on the microslide uniformly again, then the tip of outer sleeve 10 is dipped on microslide gently, observe under Stereo microscope, making the length of the silicone rubber membrane 18 that injects to the tip is 10-20 μ m.Placing 24h solidifies silicone rubber membrane 18.
8, get the KCl saturated solution, make anode with filamentary silver 11, carbon-point is done negative electrode, under 1.5 volts the DC voltage on filamentary silver 11 plating AgCl make inner contrast electrode (anode).
9, electrolytic solution 12 behind the preparation film, electrolytic solution is by 1MKCl, 0.3MK behind the film
2CO
3With 0.2M KHCO
3Mixed liquor form, volume ratio is 2: 2: 1.
10, in outer sleeve 10, inject electrolytic solution 12 behind the film; to respond to negative electrode and inner contrast electrode again couples together and inserts in the outer sleeve 10; silver-colored guard electrode is inserted separately in the outer sleeve 10; silver guard electrode tip is 50-200 μ m apart from the platinum filament tip, uses epoxy sealing between glass capillary and the outer sleeve.
Referring to Fig. 1, the use of the dissolved oxygen micro electrode 8 of the utility model preparation is: dissolved oxygen micro electrode 8 inserts in the testing sample 9, dissolved oxygen micro electrode 8 is fixed on the microcontroller support (model is LS-18) 7 by miniature manipulater 5 (model is MC-232) and is adjusted to suitable position, miniature manipulater 5 is controlled by micro-step motor 6 (model is MM33), it can realize several microns of every moved further, and its power is controlled by the power controller 3 that links to each other with PC 1 (model is MC-232).The electric signal of dissolved oxygen micro electrode 8 responses amplifies in current amplifier (model is PA2000) 4 by cable, in A/D converter (model is ADC-216USB) 2 input PCs 1, demonstrates the continuous variation of signal on PC 1 then.
The dissolved oxygen micro electrode volume of the utility model preparation is little, resolution is high, the response time is short, highly sensitive, applied widely, the preparation method is simple, and is with low cost.Microexamination in fields such as environmental microbiology and biological sewage treatment has a wide range of applications.
Claims (7)
1, a kind of dissolved oxygen micro electrode is characterized in that, this dissolved oxygen micro electrode comprises an outer sleeve (10) that is filled with electrolyte (12) behind the film, and outer sleeve (10) is made by soda-lime glass, and the one end is tip-shape, and the tip is marked with silicone rubber membrane (18); The induction negative electrode of being made by platinum filament (16) is equipped with in the centre of described outer sleeve (10), and described platinum filament (16) has one section exposed platinum filament outside glass capillary (14) being positioned at outer sleeve (10) point, and the exposed platinum filament back that is corroded is gold-plated; Inner contrast electrode of Ag/AgCl and silver protection negative electrode also are housed in the outer sleeve (10); wherein; the induction negative electrode is connected with the inner contrast electrode of Ag/AgCl; the silver guard electrode is inserted separately; the tip of silver guard electrode is 50 μ m～200 μ m apart from the tip of platinum filament (16); by epoxy resin (13) sealing, the lead-in wire of platinum filament induction negative electrode, the inner contrast electrode of Ag/AgCl and silver protection negative electrode is welded in respectively on the corresponding binding post of electrode plug between outer sleeve (10) and the glass capillary (14).
2, dissolved oxygen micro electrode as claimed in claim 1 is characterized in that, the tip of described platinum filament (16) is corroded to 25 μ m, and gold-plated length is 10-20 μ m.
3, dissolved oxygen micro electrode as claimed in claim 1 is characterized in that, described silver protection negative electrode is made for most advanced and sophisticated superfine filamentary silver, filamentary silver outer wrap glass, the 50 μ m that are corroded of its most advanced and sophisticated 1cm place.
4, dissolved oxygen micro electrode as claimed in claim 1 is characterized in that, the length of described silicone rubber membrane is 10 μ m～20 μ m.
5, dissolved oxygen micro electrode as claimed in claim 1 is characterized in that, electrolytic solution behind the described film (12) is by 1MKCl, 0.3MK
2CO
3With 0.2M KHCO
3Mixed liquor form, its volume ratio is 2: 2: 1.
6, dissolved oxygen micro electrode as claimed in claim 1 is characterized in that, the tip of described outer sleeve (10) is less than 50 μ m.
7, dissolved oxygen micro electrode as claimed in claim 1 is characterized in that, the purity of described platinum filament (16) is 99.99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008202284332U CN201335817Y (en) | 2008-12-25 | 2008-12-25 | Dissolved oxygen microelectrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008202284332U CN201335817Y (en) | 2008-12-25 | 2008-12-25 | Dissolved oxygen microelectrode |
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| Publication Number | Publication Date |
|---|---|
| CN201335817Y true CN201335817Y (en) | 2009-10-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNU2008202284332U Expired - Fee Related CN201335817Y (en) | 2008-12-25 | 2008-12-25 | Dissolved oxygen microelectrode |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101408526B (en) * | 2008-11-14 | 2012-07-04 | 西安建筑科技大学 | Dissolved oxygen micro electrode and preparing method thereof |
-
2008
- 2008-12-25 CN CNU2008202284332U patent/CN201335817Y/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101408526B (en) * | 2008-11-14 | 2012-07-04 | 西安建筑科技大学 | Dissolved oxygen micro electrode and preparing method thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091028 Termination date: 20111225 |