CN101726523B - Ampere detection electrode positioned on temperature modulating column end and manufacturing method thereof - Google Patents
Ampere detection electrode positioned on temperature modulating column end and manufacturing method thereof Download PDFInfo
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- CN101726523B CN101726523B CN 200910251267 CN200910251267A CN101726523B CN 101726523 B CN101726523 B CN 101726523B CN 200910251267 CN200910251267 CN 200910251267 CN 200910251267 A CN200910251267 A CN 200910251267A CN 101726523 B CN101726523 B CN 101726523B
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Abstract
The invention relates to an ampere detection electrode positioned on a temperature modulating column end and a manufacturing method thereof. The ampere detection electrode comprises a detection electrode and a heating device, wherein the detection electrode is a conductive body; the heating device comprises a heating coil and a DC heating power supply; and the heating coil is formed by winding two bent parallel lead wires on the detection electrode and is connected with the DC heating power supply. The invention can easily realize the modulation of the temperature of the electrode by controlling heating current, completely eliminate the interference of a magnetic field on ampere detection and enhance the signal to noise ratio and the detection sensitivity and achieve great high repeatability and stability; in addition, the heating way has simple structure and easy miniaturization.
Description
Technical field
The present invention relates to a kind of ampere detection electrode positioned on temperature modulating column end and production method thereof of realizing with the isolation technics coupling.This electrode can not only be eliminated heating current to the interference of ampere detection signal, greatly strengthens detection sensitivity, has simultaneously high stability and reappearance.
Background technology
At the analytical chemistry separation technology field, detecting device is the important component part of tripping device.Detecting device commonly used has fluorescence detector (such as ultraviolet one visible light detector, differential refraction detector, fluorescence detector etc.), electrochemical detector, mass spectrum, nuclear magnetic resonance, flame ion detection, photodiode array etc. at present.Electrochemical detector has the advantages such as dead volume is little, fast response time, cost is low, highly sensitive, selectivity is good, convenient, flexible, with it and isolation technics coupling, has a wide range of applications in the analytical chemistry research field.The styletable Amperometric is present most widely used electrochemical detection method.
But at present styletable ampere detection method in the application aspect the isolation technics owing on sensitivity, stability, range of application, also there being some urgent problems.In Capillary Electrophoresis, micro-fluidic chip and capillary electric chromatogram field, because it is the method that detects according to the electric current that electroactive material produces when the working electrode surface generation redox reaction that ampere detects, separate high pressure detection system is had very large interference, so the styletable detection has been applied to eliminating the impact of separation electric field on the terminal cylinder Electrochemical Detection.Although the styletable detection can be eliminated the electric field aspect and have great advantage, also there are two shortcomings in it.First electrode is carrying out in ampere testing process continuously and since electrode surface to reactant with and the suction-operated of product, thereby make electrode generation passivation greatly reduce sensitivity and the reappearance of electrode detection.It two is that styletable detects as a kind of from the post detecting pattern, because detection material spreads after flowing out kapillary, so that its ampere detection efficiency is lower, thereby has further affected the sensitivity of electrode detection.
In the liquid chromatography field, usually run into when most protein, lipoid and surfactant that electrode response answers stable and detect lower limit and do not reach the difficulties such as requirement, this is because macromolecular substances or its reaction product have been adsorbed onto the ammeter face, makes electrode surface contaminated and deactivate.Compound in many biologies and the environment is owing to having higher overpotential at solid electrode, so do not have electrochemical response in general potential range simultaneously.Therefore, directly carry out Electrochemical Detection for these compounds and generally need to adopt higher current potential, the interference that this will inevitably produce larger background current and concurrent has affected the detectability of analyzing.
Therefore how to improve electrode sensitivity, strengthen stability, the application at separation field is extremely important for electrochemical detector to reduce overpotential.
Temperature modulation is by heating current working electrode to be heated to make electrode can at high temperature carry out work.The temperature of electrode can accurately be modulated by the size of regulating electric current.At high temperature, the diffusion layer viscosity of electrode surface greatly reduces, and convection current strengthens, and the electrolyte mass transfer rate improves can reduce the oxidation potential of detection material on electrode simultaneously, and this has improved the ampere detection signal strength greatly, has guaranteed simultaneously the cleaning of electrode surface.
Thermode is applied to separation field as the styletable ampere detector, is expected to solve the shortcoming that the above-mentioned electrochemical detector of mentioning exists.Existing thermode type of heating is to utilize high-frequency alternating current that working electrode is heated (Zhang Lan; Song Ziwang; Chen Guonan. Capillary Electrophoresis-thermal technology makes electrode-ampere pick-up unit and thermal technology's working electrode preparation method [P]. Chinese patent: CN101140259,2008-03-12.).Because the ampere detection signal of tripping device electrochemical detector generally is in the nA rank, the heating alternating current has very large interference to the ampere detection signal, and this has limited the application of thermode technology in the end of electrophoretic capillary column ampere detects.
In order to eliminate the heating alternating current to the interference of ampere detection signal, the present invention proposes the two-wire winding method and utilize DC current to come heating electrode.Utilize the present invention, electrode temperature can accurately be controlled, and when improving sensitivity, can eliminate heating current to the impact of ampere detection signal and greatly strengthen the stability of detecting device.
Summary of the invention
The purpose of this invention is to provide a kind of ampere detection electrode positioned on temperature modulating column end, it can reduce heating current greatly to the interference of ampere detection signal, can also keep the high stability of detection signal and reappearance when greatly improving sensitivity.
For achieving the above object, the present invention adopts following scheme: a kind of ampere detection electrode positioned on temperature modulating column end is characterized in that: it is comprised of detecting electrode and heating arrangement; Described detecting electrode is an electric conductor, and described heating arrangement is comprised of heater coil and DC heating power supply, and described heater coil is to be converted into parallel two by wire to be wrapped on the described detecting electrode; One end of described heater coil is connected with the DC heating power supply.
Another purpose of the present invention provides a kind of manufacture method of said temperature modulation styletable ampere detecting electrode, and the method is not only simple and practical, and can greatly reduce heating current to the interference of ampere signal according to the detecting device of the method design.
For achieving the above object, the present invention adopts following scheme: the manufacture method of a kind of above-mentioned thermode-styletable ampere detector is characterized in that may further comprise the steps:
(1) provide a kind of electric conductor as detecting electrode and the wire that is used for making heater coil;
(2) wire is converted into parallel two and is wrapped on the detecting electrode, form two heater coils that the current return opposite direction is side-by-side.
(3) output terminal of heater coil with a direct current heating power supply linked to each other.The electrode and the heater coil that wind are put into a pipe box, utilize epoxide-resin glue and described thick conductor to fix.
Described electrodes conduct body, heater coil scribble insullac with the surface of wire.
The invention has the beneficial effects as follows and can be easy to realize control to electrode temperature by the control heating current, can eliminate the interference that magnetic field is detected ampere fully, and this type of heating is simple in structure, easily microminiaturized.
Description of drawings
Fig. 1 is detector electrode structure schematic diagram of the present invention.
Fig. 2 is detecting electrode Distribution of Magnetic Field schematic diagram of the present invention.
In the accompanying drawing:
1, detecting electrode 2, epoxide-resin glue 3, heater coil 4, sleeve pipe 5, working electrode surface
6, heater coil connects the terminals 7 of direct supply, the terminals that working electrode connects electrochemical workstation
Embodiment
The present invention will be further described below in conjunction with drawings and Examples.
As shown in Figure 1, the invention provides a kind of ampere detection electrode positioned on temperature modulating column end, it is characterized in that: it is comprised of detecting electrode 1 and heating arrangement; Described detecting electrode 1 is a conductor that scribbles insullac, and described heating arrangement is comprised of heater coil 3 and DC heating power supply, and described heater coil 3 is to be converted into parallel two by a conductor that scribbles insullac to be wrapped on the described detecting electrode; One end of described heater coil (being the terminals 6 that heater coil connects direct supply) is connected with the DC heating power supply; The described detecting electrode surface that twines is arranged with sleeve pipe 4, and described sleeve pipe 4 is fixed by epoxide-resin glue 2 and detecting electrode.
In addition, the invention provides a kind of manufacture method of said temperature modulation styletable ampere detecting electrode, it is characterized in that may further comprise the steps:
(1), provides a kind of electric conductor as detecting electrode and be used for making the wire of heater coil;
(2), wire be converted into parallel two be wrapped on the thick conductor, form two heater coils that the loop opposite direction is side-by-side;
(3), the output terminal of heater coil with a direct current heating power supply linked to each other; Cancel out each other in the magnetic field that described heater coil produces.
At last the electrode and the heater coil that wind are put into a pipe box, utilize epoxide-resin glue and described thick conductor to fix.
Concrete, please continue with reference to shown in Figure 1:
1, the diameter of at first getting a long 10cm is the copper enameled wire (working electrode) of 360 μ m, its two ends are fixed, and keep that the copper enameled wire all is in straight configuration in the whole manufacturing process, then will twine one section copper enameled wire of upper heater coil with absolute ethyl alcohol clear clean.
2, get the copper enameled wire of the 75 μ m of an about long 50cm, it is converted into two parallel lines (line does not disconnect) from middle position, then the end with break in the middle of it is fixed on the copper enameled wire of 360 μ m with 502 glue first, again with the uniform wound in parallel of copper enameled wire of the 75 μ m copper enameled wire at 360 μ m, being wound to loop length is 2cm, the tension of the coil of whole winding is close and be fixed with 502 glue at last.
3, the copper enameled wire (working electrode) that winds 360 μ m of heater coil in the step 2 is wound with heater coil electrode clean partly with the absolute ethyl alcohol handle first clean, insert diameter and be in 900 microns the plastic casing, and fix the centre that makes its working electrode position be in sleeve pipe, evenly pour into the epoxide-resin glue that mixes in the sleeve pipe again, after at room temperature placing 0.5-2 hour, more whole sleeve pipe is put into 45-75 degree constant temperature oven heating 3-6 hour.
4, the working electrode other end and heater coil lead-in wire is removed insullac and and wire bonds good, respectively as the lead-in wire that connects electrochemical workstation and direct supply, to polish with sand paper in its test side with the good electrode of epoxy resin cure, the detecting electrode workplace is exposed and heater coil does not expose, put into the ultrasonic 5-20min of intermediate water, taking-up is dried for subsequent use.
As shown in Figure 2, Fig. 2 is the induced field schematic diagram that the sub-heater coil of the present embodiment produces when applying direct current, as can be seen from the figure, the coil that two-wire twines applies two magnetic fields that produce opposite direction behind the electric current, can so that the magnetic field of whole heater coil is cancelled, near the magnetic field of electrode surface be disappeared like this.
The above only is preferred embodiment of the present invention, and all equalizations of doing according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Claims (7)
1. ampere detection electrode positioned on temperature modulating column end, it is characterized in that: it is comprised of detecting electrode and heating arrangement; Described detecting electrode is an electric conductor, and described heating arrangement is comprised of heater coil and DC heating power supply, and described heater coil is to be converted into parallel two by wire to be wrapped on the described detecting electrode; The two ends of described heater coil are connected with the DC heating power supply.
2. ampere detection electrode positioned on temperature modulating column end according to claim 1, it is characterized in that: the described detecting electrode surface that twines is arranged with pipe box, and described pipe box is fixed by epoxide-resin glue and detecting electrode.
3. ampere detection electrode positioned on temperature modulating column end according to claim 1 and 2, it is characterized in that: described detecting electrode is an electric conductor, and electrode material comprises metallic conductor, carbonaceous conductor, polynary composite conductor, semiconductor.
4. ampere detection electrode positioned on temperature modulating column end according to claim 1 and 2, it is characterized in that: described heater coil is that a wire coiling forms.
5. the manufacture method of an ampere detection electrode positioned on temperature modulating column end as claimed in claim 1 is characterized in that may further comprise the steps:
(1) provide a kind of electric conductor as detecting electrode and the wire that is used for making heater coil;
(2) described wire is converted into parallel two and is wrapped on the detecting electrode, form two heater coils that the current return opposite direction is side-by-side;
(3) output terminal of heater coil with a direct current heating power supply linked to each other; Cancel out each other in the magnetic field that described heater coil produces.
6. the manufacture method of ampere detection electrode positioned on temperature modulating column end according to claim 5 is characterized in that further comprising: the electrode and the heater coil that wind are put into a pipe box, utilize epoxide-resin glue and described electric conductor to fix.
7. according to claim 5 or 6 described ampere detection electrode positioned on temperature modulating column end manufacture methods, it is characterized in that: described electric conductor, heater coil scribble insullac with the surface of wire.
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| CN101726523B true CN101726523B (en) | 2013-04-03 |
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| CN102879447A (en) * | 2012-08-29 | 2013-01-16 | 闽江学院 | Preparation method for thermal control sulfhydryl ionic liquid modified electrode |
| CN104614429B (en) * | 2015-02-09 | 2017-07-04 | 福州大学 | The making of gold plated copper thermode and in temperature-controllable H2O2Application on sensor |
Citations (6)
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| GB1472358A (en) * | 1974-07-18 | 1977-05-04 | Balzers Patent Beteilig Ag | Device for the detection of gases and vapours |
| DE19543060A1 (en) * | 1995-11-07 | 1997-05-15 | Peter Prof Dr Gruendler | Electrochemical measurement on directly heated electrodes |
| CN101140259A (en) * | 2007-10-11 | 2008-03-12 | 福州大学 | Capillary electrophoresis-heat working electrode- ampere testing apparatus and heat working electrode preparation method |
| CN101162199A (en) * | 2007-11-19 | 2008-04-16 | 福州大学 | Heat controlled electric pole electrogenerated chemiluminescence testing apparatus and testing-pool preparation method |
| CN101368929A (en) * | 2008-09-24 | 2009-02-18 | 福州大学 | Temperature modulating electro-chemical electrode and its heating method |
| CN201844994U (en) * | 2009-12-01 | 2011-05-25 | 福州大学 | Temperature modulation end-column amperometric detection electrode |
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Patent Citations (6)
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|---|---|---|---|---|
| GB1472358A (en) * | 1974-07-18 | 1977-05-04 | Balzers Patent Beteilig Ag | Device for the detection of gases and vapours |
| DE19543060A1 (en) * | 1995-11-07 | 1997-05-15 | Peter Prof Dr Gruendler | Electrochemical measurement on directly heated electrodes |
| CN101140259A (en) * | 2007-10-11 | 2008-03-12 | 福州大学 | Capillary electrophoresis-heat working electrode- ampere testing apparatus and heat working electrode preparation method |
| CN101162199A (en) * | 2007-11-19 | 2008-04-16 | 福州大学 | Heat controlled electric pole electrogenerated chemiluminescence testing apparatus and testing-pool preparation method |
| CN101368929A (en) * | 2008-09-24 | 2009-02-18 | 福州大学 | Temperature modulating electro-chemical electrode and its heating method |
| CN201844994U (en) * | 2009-12-01 | 2011-05-25 | 福州大学 | Temperature modulation end-column amperometric detection electrode |
Non-Patent Citations (5)
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| Tadesse Zerihum 等.Electrically heated cylindrical microelectrodes. The reduction of dissolved oxygen on Pt.《Journal of electroanalytical chemistry》.1996,第404卷243-248. * |
| Zhenyu Lin等.A new electrochemiluminescent detection system equipped with an electrically controlled heating cylindrical microelectrode.《Analytica Chimica Acta 》.2006,第564卷226-230. * |
| 吴韶华等.木犀草素在直流加热单边热石墨柱电极上电化学行为及吸附溶出分析.《福州大学学报(自然科学版)》.2009,第37卷(第1期),128-132. * |
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