CN101435794A - pH selectivity micro-electrode and preparing method thereof - Google Patents
pH selectivity micro-electrode and preparing method thereof Download PDFInfo
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- CN101435794A CN101435794A CNA2008102327351A CN200810232735A CN101435794A CN 101435794 A CN101435794 A CN 101435794A CN A2008102327351 A CNA2008102327351 A CN A2008102327351A CN 200810232735 A CN200810232735 A CN 200810232735A CN 101435794 A CN101435794 A CN 101435794A
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Abstract
The invention discloses a pH selective microelectrode and a preparation method thereof. The pH selective microelectrode comprises a conical glass bushing, an after-membrane electrolyte is filled in a cavity of the conical glass bushing, a tip part of the conical glass bushing is injected with a hydrogen ion selective liquid membrane, an Ag/AgCl wire is arranged in the conical glass bushing, and an epoxy resin is used to fix the Ag/AgCl wire and seal the conical glass bushing at a mouth part of the conical glass bushing. The diameter of the tip of the pH selective microelectrode is between 1 and 10mu m, the linear response range, namely the pH value is between 4 and 10, and the slope is -59.945mV/pH. The response time of the microelectrode is short and is generally less than 5s, and the pH selective microelectrode has the advantages of small volume, simple production and low cost.
Description
Technical field
The present invention relates to a kind of microelectrode and preparation thereof, particularly a kind of pH selectivity micro-electrode and preparation method thereof.
Technical background
Serious environmental is polluted and is made wastewater treatment come into one's own day by day, and denitrogenation is as an important step of wastewater treatment, and pH has material impact to nitration denitrification, so discussion of denitrogenation mechanism and process optimization all be unable to do without the mensuration of pH.For a long time, owing to lack proper tools, people measure the pH of microscopic fields and rest on macroscopical basis, and the research of the variation of pH in the microcosmos area is lacked corresponding means of testing.
Summary of the invention
Defective or deficiency at above-mentioned prior art exists the objective of the invention is to, and a kind of pH selectivity micro-electrode and preparation method thereof is provided, and the pH selectivity micro-electrode that the present invention makes is applicable to measures pH variation in active sludge or the biological membrane interior microscopic zone.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of pH selectivity micro-electrode, comprise a cone-shaped glass sleeve pipe, it is characterized in that, electrolytic solution after in the chamber of cone-shaped glass sleeve pipe, being filled with film, the point of cone-shaped glass sleeve pipe is marked with the hydrogen ion selective liquid film, the Ag/AgCl silk is installed in the cone-shaped glass sleeve pipe, at the oral area of cone-shaped glass sleeve pipe with epoxy resin fixedly Ag/AgCl silk and sealing cone-shaped glass sleeve pipe.
The preparation method of above-mentioned pH microelectrode is characterized in that, comprises the following steps:
(1) draw the cone-shaped glass sleeve pipe: glass tube is fixed on the centre position of heater coil, and heating freely falls it, with the tip of glass tube up, is fixed on the clip again, and heating makes the diameter of its point in desired scope once more.
(2) silanization: 30min in the silane agent is immersed at the tip that will draw good cone-shaped glass sleeve pipe in fuming cupboard, is placed in the glass container then and places chamber type electric resistance furnace to toast 1h, make remain on the cone-shaped glass sleeve pipe silane agent volatilization fully.
(3) electrolytic solution behind the injection film: electrolytic solution behind the film is injected it respectively in the cone-shaped glass sleeve pipe of silanization with the 1mL syringe behind 0.45 μ m filtering with microporous membrane, and in the pressurization of the rear end of cone-shaped glass sleeve pipe, make electrolytic solution be filled to the point of cone-shaped glass sleeve pipe, to discharge gas wherein;
(4) suck the hydrogen ion selective liquid film: under binocular microscope, with the tip of syringe with hydrogen ion selective liquid film suction taper glass bushing, the length of suction is 5mm;
(5) the Ag/AgCl silk is inserted behind the film in the electrolytic solution until point near the cone-shaped glass sleeve pipe, then with epoxy resin at the fixing Ag/AgCl silk and seal the cone-shaped glass sleeve pipe of the mouth of pipe of cone-shaped glass sleeve pipe, and make Ag/AgCl silk one end expose the cone-shaped glass sleeve pipe.
PH selectivity micro-electrode of the present invention, for the effective instrument that provides is provided the pH that measures microcosmos area, this pH selectivity micro-electrode volume is little, most advanced and sophisticated superfine, can realize online, original position, nondestructive mensuration, can be used for studying pH in the various mud of water body, the sediment interior microscopic zone, and in the biological wastewater treatment process, hydrionic concentration change situation in the inner infinitesimal of active sludge or the biological membrane zone, thereby further optimization process technology.
Description of drawings
Fig. 1 is the structural representation of pH selectivity micro-electrode, and label wherein is respectively: 1, cone-shaped glass sleeve pipe; 2, electrolytic solution behind the film; 3, Ag/AgCl silk; 4, epoxy resin; 5, hydrogen ion selective liquid film;
Fig. 2 is the mensuration linear response range figure of pH selectivity micro-electrode.
The present invention is described in further detail below in conjunction with accompanying drawing.
Embodiment
Referring to Fig. 1, pH selectivity micro-electrode of the present invention comprises a taper outer sleeve pipe 1, and Ag/AgCl silk 3 is installed in this glass tube, the point of taper outer sleeve pipe 1 is marked with hydrogen ion selective liquid film 5, is filled with electrolytic solution 2 behind the film in the chamber of taper outer sleeve pipe 1; With epoxy resin 4 fixedly Ag/AgCl silk and outer glass sleeve pipe.
Taper outer sleeve pipe 1 is a mono-layer tube, and to make tip length be 1～10 μ m.
This pH selectivity micro-electrode, linear response range are pH=4～10, and slope is-59.945mV/pH.Electrode response time is short, is generally less than 5s, and volume is little, making is simple, cheap.
The preparation method of pH selectivity micro-electrode comprises the following steps:
(1) draw cone-shaped glass sleeve pipe 1: glass tube is fixed on the centre position of heater coil, and heating freely falls it, with the tip of glass tube up, is fixed on the clip again, and heating makes its tip diameter in desired scope once more.
(2) silanization: 30min in the silane agent is immersed at the tip that will draw good cone-shaped glass sleeve pipe in fuming cupboard, is placed in the glass container then and places chamber type electric resistance furnace to toast 1h, make remain on the glass cone-shaped glass sleeve pipe silane agent volatilization fully.
(3) electrolytic solution behind the injection film: electrolytic solution behind the film 2 is injected it respectively in the cone-shaped glass sleeve pipe 1 of silanization with the 1mL syringe behind 0.45 μ m filtering with microporous membrane, and in the pressurization of the rear end of cone-shaped glass sleeve pipe 1, make electrolytic solution be full of cone-shaped glass sleeve pipe (until point), to discharge gas wherein.
(4) suck hydrogen ion selective liquid film (LIX): under binocular microscope, with the tip of syringe with hydrogen ion selective liquid film 5 suction taper glass bushings 1, the liquid film length of suction is about 5mm.
(5) Ag/AgCl silk 3 is inserted behind the films in the electrolytic solution 2 until point near cone-shaped glass sleeve pipe 1, with epoxy resin 4 at the mouth of pipe of cone-shaped glass sleeve pipe fixedly Ag/AgCl silk 3 and sealing cone-shaped glass sleeve pipe 1, and make an end of Ag/AgCl silk 3 expose cone-shaped glass sleeve pipe 1, as indicator electrode.
The preparation process of Ag/AgCl silk 3 is as follows:
1. get a suitably long filamentary silver, with sand papering to remove its surperficial oxide layer;
2. get a precious metal or carbon-point and receive on the negative electrode of power supply, the filamentary silver of polishing is received on the anode of power supply, under the DC voltage of 1.5V, in saturated potassium chloride solution, electroplate 2s and promptly can be made into the Ag/AgCl silk.
Electrolytic solution is the KH of 0.04mol/L behind the above-mentioned film
2PO
4, 0.023mol/L the NaCl of NaOH, 0.015mol/L constitute (pH is transferred to 7).The hydrogen ion selective liquid film is that 0.5g Alamine 304 (tridodecylamine), 0.035g sodium tetraphenylborate (sodium tetraphenylborate) are dissolved in the 5mL2-nitrobenzophenone Octyl Ether (2-nitrophenyl octyl ether) and make.
Calibration curve method is the most frequently used a kind of analytical approach of pH selectivity micro-electrode.The pH selectivity micro-electrode of the present invention's preparation adopts calibration curve method, prepares a series of pH value solution with the pH standard buffer solution, measures its potential value respectively, in order to estimate electrode performance.The result shows that the linear response range of this pH selectivity micro-electrode is pH=4～10, and regression coefficient reaches 0.9991, and slope is-59.945mV/pH, as shown in Figure 2.Electrode response time is short, is generally less than 5s.
Claims (9)
1. pH selectivity micro-electrode, comprise a cone-shaped glass sleeve pipe (1), it is characterized in that, electrolytic solution (2) after in the chamber of cone-shaped glass sleeve pipe (1), being filled with film, the point of cone-shaped glass sleeve pipe (1) is marked with hydrogen ion selective liquid film (5), Ag/AgCl silk (3) is installed, at the oral area of cone-shaped glass sleeve pipe (1) epoxy resin (4) fixedly Ag/AgCl silk (3) and sealing cone-shaped glass sleeve pipe (1) in the cone-shaped glass sleeve pipe (1).
2. pH selectivity micro-electrode as claimed in claim 1 is characterized in that, described cone-shaped glass sleeve pipe (1) is a mono-layer tube.
3. pH selectivity micro-electrode as claimed in claim 1 is characterized in that, the tip length of described cone-shaped glass sleeve pipe (1) is 1 μ m～10 μ m.
4. pH selectivity micro-electrode as claimed in claim 1 is characterized in that, electrolytic solution behind the described film (2) is by the KH of 0.04mol/L
2PO
4, the NaOH of 0.023mol/L and 0.015mol/L NaCl form, the pH value transfers to 7.
5. pH selectivity micro-electrode as claimed in claim 1 is characterized in that, described hydrogen ion selective liquid film is dissolved in by 0.5g Alamine 304 and 0.035g sodium tetraphenylborate in the 2-nitrobenzophenone Octyl Ether of 5mL to be made.
6. the preparation method of the described pH selectivity micro-electrode of claim 1 is characterized in that, comprises the following steps:
(1) draw the cone-shaped glass sleeve pipe: glass tube is fixed on the centre position of heater coil, and heating freely falls it, with the tip of glass tube up, is fixed on the clip again, and heating makes the diameter of its point in desired scope once more;
(2) silanization: 30min in the silane agent is immersed at the tip that will draw good cone-shaped glass sleeve pipe in fuming cupboard, is placed in the glass container then and places chamber type electric resistance furnace to toast 1h, make remain on the cone-shaped glass sleeve pipe silane agent volatilization fully;
(3) electrolytic solution behind the injection film: electrolytic solution behind the film is injected it respectively in the cone-shaped glass sleeve pipe of silanization with the 1mL syringe behind 0.45 μ m filtering with microporous membrane, and in the pressurization of the rear end of cone-shaped glass sleeve pipe, make electrolytic solution be filled to the point of cone-shaped glass sleeve pipe, to discharge gas wherein;
(4) suck the hydrogen ion selective liquid film: under binocular microscope, with the tip of syringe with hydrogen ion selective liquid film suction taper glass bushing, the length of suction is 5mm;
(5) the Ag/AgCl silk is inserted behind the film in the electrolytic solution until point near the cone-shaped glass sleeve pipe, then with epoxy resin at the fixing Ag/AgCl silk and seal the cone-shaped glass sleeve pipe of the mouth of pipe of cone-shaped glass sleeve pipe, and make Ag/AgCl silk one end expose the cone-shaped glass sleeve pipe.
7. method as claimed in claim 6 is characterized in that, the preparation process of described Ag/AgCl silk is as follows:
1) get the filamentary silver of an appropriate length, with sand papering to remove its surperficial oxide layer;
2) get a precious metal or carbon-point and receive on the negative electrode of power supply, the filamentary silver of polishing is received on the anode of power supply, under the DC voltage of 1.5V, in saturated potassium chloride solution, electroplate 2s and promptly can be made into the Ag/AgCl silk.
8. method as claimed in claim 6 is characterized in that, described hydrogen ion selective liquid film is dissolved in by 0.5g Alamine 304 and 0.035g sodium tetraphenylborate in the 2-nitrobenzophenone Octyl Ether of 5mL to be made.
9. method as claimed in claim 6 is characterized in that, electrolytic solution behind the described film (2) is by the KH of 0.04mol/L
2PO
4, the NaOH of 0.023mol/L and 0.015mol/L NaCl form, the pH value is adjusted to 7.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102327351A CN101435794A (en) | 2008-12-19 | 2008-12-19 | pH selectivity micro-electrode and preparing method thereof |
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| CNA2008102327351A CN101435794A (en) | 2008-12-19 | 2008-12-19 | pH selectivity micro-electrode and preparing method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103868965A (en) * | 2014-03-12 | 2014-06-18 | 西安建筑科技大学 | CO2 micro electrode and preparation method thereof |
| CN108896633A (en) * | 2018-04-20 | 2018-11-27 | 中国科学院生态环境研究中心 | A kind of high-precision pH microelectrode and preparation method thereof |
| CN114062463A (en) * | 2022-01-11 | 2022-02-18 | 南京智感环境科技有限公司 | Nondestructive measurement of microbial and environmental interface H+Microelectrode and preparation and determination methods thereof |
-
2008
- 2008-12-19 CN CNA2008102327351A patent/CN101435794A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103868965A (en) * | 2014-03-12 | 2014-06-18 | 西安建筑科技大学 | CO2 micro electrode and preparation method thereof |
| CN108896633A (en) * | 2018-04-20 | 2018-11-27 | 中国科学院生态环境研究中心 | A kind of high-precision pH microelectrode and preparation method thereof |
| CN108896633B (en) * | 2018-04-20 | 2020-06-30 | 中国科学院生态环境研究中心 | High-precision pH microelectrode and manufacturing method thereof |
| CN114062463A (en) * | 2022-01-11 | 2022-02-18 | 南京智感环境科技有限公司 | Nondestructive measurement of microbial and environmental interface H+Microelectrode and preparation and determination methods thereof |
| CN114062463B (en) * | 2022-01-11 | 2022-09-13 | 南京智感环境科技有限公司 | Nondestructive measurement of microbial and environmental interface H + Microelectrode and preparation and determination methods thereof |
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Open date: 20090520 |