CN102706863B - There is self-cleaning function and without the Electrochemiluminescprocess process pick-up unit of additional interference - Google Patents
There is self-cleaning function and without the Electrochemiluminescprocess process pick-up unit of additional interference Download PDFInfo
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- CN102706863B CN102706863B CN201210141894.7A CN201210141894A CN102706863B CN 102706863 B CN102706863 B CN 102706863B CN 201210141894 A CN201210141894 A CN 201210141894A CN 102706863 B CN102706863 B CN 102706863B
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Abstract
The present invention relates to and a kind ofly there is self-cleaning function and without the Electrochemiluminescprocess process pick-up unit of additional interference, belong to analytical test field.The Electrochemiluminescprocess process glass-carbon electrode detected in involved device is very easily subject to the adsorption fouling of the organic species that electrolysis produces, and this case is intended to solve this problem.The structure of this case device comprises electrolytic cell and is inserted in working electrode in electrolytic cell, to electrode and contrast electrode, emphasis is, ultrasonic transducer is equiped with in the bottom of electrolytic cell or side, simultaneously, entangle contrast electrode with the ultrasonic energy absorber of the pen cap shape of micropore material or test tube shape, make it disturb from ultrasound wave.This case, without under the prerequisite of additional interference, is carried out instant cleaning with low-power, high-frequency ultrasound wave to the described electrode in electrolytic cell, is contained the adsorption fouling process of described electrode thus.
Description
Technical field
The present invention relates to and a kind ofly there is self-cleaning function and without the Electrochemiluminescprocess process pick-up unit of additional interference, belong to analytical test field.
Background technology
In applied analysis detection means, electrogenerated chemiluminescence is a kind of new detection technique grown up on chemiluminescence basis, the system containing chemiluminescent substance by electrode pair applies certain voltage or electric current, make luminescent substance be stimulated and transition return ground state and send photon, therefore electrochemiluminescence has the excellent selectivity of galvanochemistry and chemiluminescent highly sensitive advantage.Electrogenerated chemiluminescence technology is in life analysis, environmental monitoring, the aspects such as food analysis have a wide range of applications, the feature main manifestations excellent based on it is: its selectivity of (1) electrogenerated chemiluminescence technology is high, electrogenerated chemiluminescence is combined with electrochemical and chemiluminescence two parts, because the current potential of the redox reaction that different materials occurs is different, show on cyclic voltammetry curve to be exactly that redox peak appears in different potentials, response curve can be had for different materials according to the change of spike potential like this.(2) highly sensitive, chemiluminescent high sensitivity is equally applicable to electrogenerated chemiluminescence, and the redox reaction produced in the middle of magazine does not have the interference of external light source, by the detection of photomultiplier, realizes highly sensitive detection.(3) experimental instrument and equipment is simple, operates photomultiplier and signal output system that this experimental technique only needs corresponding electrochemical workstation and sensed light signal, easy to operate.(4) consuming time short, response efficiency is high, completes the time that cyclic voltammetry scan only needs 3-5 minute.
But, working electrode in device involved by this electrochemiluminescdetection detection and the adsorption fouling of organic species that electrolysis produces very easily is subject to electrode and auxiliary electrode, especially when adopting glass-carbon electrode as working electrode, described adsorption fouling is even more serious, and described adsorption fouling can cause the rapid decay of working electrode and auxiliary electrode performance; Therefore, how while carrying out electrochemiluminescdetection detection operation, effectively, immediately clean described working electrode and auxiliary electrode, a technical matters urgently to be resolved hurrily is just become.
Summary of the invention
Problem to be solved by this invention is, researches and develops a kind ofly while carrying out Electrochemiluminescprocess process detection, can immediately carry out the novel Electrochemiluminescprocess process pick-up unit of the self-cleaning running of electrode, and this self-cleaning running should not bring negative interference.
This case is solved the problem by following scheme, the device that the program provides a kind ofly has self-cleaning function and without the Electrochemiluminescprocess process pick-up unit of additional interference, the structure of this device comprises electrolytic cell, and, be installed in below electrolytic cell or the photomultiplier of side, described electrolytic cell is installed within magazine, and, working electrode, and, to electrode, and, contrast electrode, described is sheet to electrode, column or thread platinum electrode or gold electrode, described contrast electrode is Ag/AgCl electrode or mercurous chloride electrode, described working electrode is glass-carbon electrode, described working electrode and the working end of electrode and contrast electrode is positioned to the inside of described electrolytic cell, this electrolytic cell is that its opening end profile is square, rectangle, the cup-shaped vessel of circular or oval indent, emphasis is, the structure of this device comprises ultrasonic transducer, the installation position of this ultrasonic transducer is the bottom position of lateral location at this electrolytic cell or electrolytic cell, and, ultrasonic energy absorber, this its profile of ultrasonic energy absorber is pen cap shape or test tube shape, the inside of electrolytic cell should be positioned in its one end closed of ultrasonic energy absorber in pen cap shape or test tube shape, the inner chamber of this ultrasonic energy absorber is goed deep in its working end of described contrast electrode, this its material of ultrasonic energy absorber is micropore material, described micropore material is micropore ceramics, fine-celled foam glass, fine-celled foam aluminium, microporous silicon rubber, expanded microporous polytetra fluoroethylene-EPTEE or micropore Kynoar.
Described micropore ceramics, fine-celled foam glass, fine-celled foam aluminium, microporous silicon rubber, expanded microporous polytetra fluoroethylene-EPTEE and micropore Kynoar etc. poromerics, all have commercially available; Selected poromerics can be bought simply cut, punching, make required form.
Described glass-carbon electrode one word, its art-recognized meanings, in Electrochemiluminescprocess process field, is known.
Described ultrasonic transducer is device higher-order of oscillation electric signal being converted to high frequency mechanical oscillation, and itself art-recognized meanings of described ultrasonic transducer one word is known at ultrasound wave professional skill field.
This case device can also comprise higher-order of oscillation electric signal generator certainly, this higher-order of oscillation electric signal generator can be connected with described ultrasonic transducer via higher-order of oscillation electric signal transmission cable, this higher-order of oscillation electric signal generator forms ultrasound emission mechanism together with the described ultrasonic transducer linked together with it via higher-order of oscillation electric signal transmission cable, and the ultrasound emission power of this ultrasound emission mechanism is between 1 milliwatt and 20 watts.Adopt lower power, help avoid the described electrode of damage, and be conducive to avoiding interference electrochemiluminescdetection detection.
The art-recognized meanings of described higher-order of oscillation electric signal generator one word is known at ultrasound wave professional skill field.
The structure of this case device, can also comprise some annexes, described annex such as: faint light measuring instrument, this faint light measuring instrument can be connected with described photomultiplier; And registering instrument, this registering instrument can be connected with described faint light measuring instrument.
Described annex is again such as: electrochemical operation station arrangement, and this electrochemical operation station arrangement can be connected with described working electrode and auxiliary electrode and contrast electrode.
Described electrochemical workstation can certainly be integrated with that faint light detects, record and the electrochemical workstation of data processing module.
Described annex is also such as: for clamping electrode clamping, the fixed support of working electrode and auxiliary electrode and contrast electrode; Etc..
Described faint light measuring instrument and the term such as described registering instrument and electrochemical operation station arrangement are expressed, and for instrumental analytical chemistry field, its art-recognized meanings is known.
Ultrasonic cavitation is the very strong effect of one, and low-frequency ultrasonic waves is comparatively strong to the surface impacts of objective workpiece, and the cavitation of this low-frequency ultrasonic waves is not too applicable to for the meticulous pick-up unit as this case; Along with the raising of ultrasonic frequency, cavitation weakens the damage of objective workpiece gradually until can ignore; Therefore, the preferred ultrasonic frequency being suitable for this case device is not random frequency.
As mentioned above, for avoiding ultrasonic cavitation to the damage on working electrode and auxiliary electrode surface, and avoid bringing out sonoluminescence, the hyperacoustic preferred frequency that this ultrasound emission mechanism launches at least should at more than 40KHz; Its scope of hyperacoustic preferred frequency that this ultrasound emission mechanism launches is between 40KHz and 12MHz.
In more meticulous aspect, for avoiding the surperficial ultrasound injury of described working electrode and auxiliary electrode, and, avoid more subtly bringing out sonoluminescence, this ultrasound emission mechanism launch hyperacoustic further preferred frequency at least should at more than 80KHz; Hyperacoustic further preferred its scope of frequency that this ultrasound emission mechanism launches is between 80KHz and 12MHz.
Liquid at the bottom of different electrolytic cells and different electrochemiluminescdetection detection analytic targets, different to hyperacoustic susceptibility of different capacity and frequency, for avoiding ultrasound wave to the interference analyzed, according to liquid at the bottom of concrete electrolytic cell and concrete detection analytic target, progressively can adjust, determine required ultrasonic frequency and power.
Ultrasonic energy absorber in this case structure makes it from hyperacoustic interference for the protection of contrast electrode, maintains contrast electrode current potential and stablize.
The poromerics in any aperture has certain absorption to shake the function of ripple; The preferred value of this its micropore size of micropore material of this case is less than 1.0 millimeters.
The described ultrasonic energy absorber of any wall thickness all has that certain ultrasound wave is cleared up, absorption function; This case is somebody's turn to do in pen cap shape or the preferred value of its wall thickness of ultrasonic energy absorber of test tube shape is between 0.3 centimetre and 3.0 centimetres.
Only with regard to poromerics to the absorption of higher-order of oscillation wave energy, clear up function and principle, for the professional of field of acoustics, be known.
As mentioned above, for liquid at the bottom of different Electrochemiluminescprocess process detected objects and electrolytic cell, should carefully adjust, ultrasonic frequency needed for selection and power, but, when previous work is not in place, when selected ultrasonic frequency and power are not enough appropriate, to such an extent as to induce the sonoluminescence of some strength, also be not enough worried, as long as deduct blank comparison value in analyte detection process, a kind of electrogenerated chemiluminescence with the instant self-cleaning function of electrode is automatically converted under this situation of this device of this case, electrochemiluminescence double excitation Conjoint Analysis pick-up unit.
The advantage of this case is, this case device can while carrying out Electrochemiluminescprocess process detection, through the sound wave transmission of liquid at the bottom of electrolytic cell, utilize high-frequency, the operative end surface of lower powered ultrasound wave to the working electrode be placed in electrolytic cell and auxiliary electrode continues, instant cleaning action, in this way, immediately the organic impurities of electrolysis oxidation-reduction reaction generation is avoided to the adsorption fouling of described electrode surface, make described electrode can remain the pure and fresh state of electrode surface in whole described analyte detection process, prevent the rapid decay of electrode performance.Certainly, based on the design feature of this case device, Electrochemiluminescprocess process detect start before and after terminating, the described ultrasound emission mechanism that this case device also can utilize it to carry, launches the cleaning in advance for electrolytic cell and electrode and ending cleaning easily.This device of this case also can convert a kind of electrogenerated chemiluminescence, the electrochemiluminescence double excitation Conjoint Analysis pick-up unit with the instant self-cleaning function of electrode easily to.
On the other hand, be the ultrasonic energy absorber of pen cap shape or test tube shape described in this case utilizes, weaken, suppress ultrasound wave to the integrated interference of described contrast electrode, maintain described contrast electrode current potential by this and stablize.
Accompanying drawing explanation
Fig. 1 is this case embodiment schematic diagram, the rough form of expressed the is core structure portion of this device.
In figure, 1 is magazine, and 2 is the cables connecting contrast electrode, 3 is the cables connecting working electrode, and 4 is the cables connecting auxiliary electrode, and 5 is higher-order of oscillation electric signal transmission cables, 6 is auxiliary electrodes, and this auxiliary electrode is also known as to electrode, and 7 is working electrodes, this case working electrode refers in particular to glass-carbon electrode, and 8 is ultrasonic transducers, and 9 is electrolytic cells, 10 schematically represent it is photomultiplier, 11 is bases, and 12 is in pen cap shape or the ultrasonic energy absorber of test tube shape, and 13 is contrast electrodes.
Embodiment
In this case embodiment that Fig. 1 shows, the structure of device comprises electrolytic cell 9, and, be installed in the photomultiplier 10 below electrolytic cell 9, this photomultiplier 10 both can be end window type photomultiplier, this photomultiplier 10 also can be side window type photomultiplier, in legend, this photomultiplier 10 is the bottoms being installed in electrolytic cell 9, but, this photomultiplier 10 also can be installed in the side of electrolytic cell 9, described electrolytic cell 9 is installed within magazine 1, and, working electrode 7, and, to electrode 6, and, contrast electrode 13, described is sheets to electrode 6, column or thread platinum electrode or gold electrode, described contrast electrode 13 is Ag/AgCl electrode or mercurous chloride electrode, described working electrode 7 is glass-carbon electrodes, described the working electrode 7 and working end of electrode 6 and contrast electrode 13 is positioned to the inside of described electrolytic cell 9, this electrolytic cell 9 is that its opening end profile is square, rectangle, the cup-shaped vessel of circular or oval indent, emphasis is, the structure of this device comprises ultrasonic transducer 8, in legend, the installation position of this ultrasonic transducer 8 is the lateral location at this electrolytic cell 9, but, the installation position of this ultrasonic transducer 8 can certainly allow to be the bottom at electrolytic cell 9, and, ultrasonic energy absorber 12, this its profile of ultrasonic energy absorber 12 is pen cap shape or test tube shape, the inside of electrolytic cell 9 should be positioned in its one end closed of ultrasonic energy absorber 12 in pen cap shape or test tube shape, the inner chamber of this ultrasonic energy absorber 12 is goed deep in described its working end of contrast electrode 13, this its material of ultrasonic energy absorber 12 is micropore material, described micropore material is micropore ceramics, fine-celled foam glass, fine-celled foam aluminium, microporous silicon rubber, expanded microporous polytetra fluoroethylene-EPTEE or micropore Kynoar.
Described micropore ceramics, fine-celled foam glass, fine-celled foam aluminium, microporous silicon rubber, expanded microporous polytetra fluoroethylene-EPTEE and micropore Kynoar etc. poromerics, all have commercially available; Selected poromerics can be bought simply cut, punching, make required form.
In this legend, do not draw the higher-order of oscillation electric signal generator be connected with ultrasonic transducer 8 via higher-order of oscillation electric signal transmission cable 5; The faint light measuring instrument be connected with photomultiplier 10 is not drawn yet; Further, the registering instrument be connected with this faint light measuring instrument is not drawn; This legend is not drawn via cable 2,3,4 and contrast electrode 13 and working electrode 7 and the electrochemical operation station arrangement that is connected electrode 6 yet; The electrode clamping for clamping each electrode, fixed support is not drawn in this legend yet, etc.
Ultrasonic transducer 8 in legend can be connected with higher-order of oscillation electric signal generator via higher-order of oscillation electric signal transmission cable 5, comprise higher-order of oscillation electric signal generator and form ultrasound emission mechanism via the ultrasonic transducer 8 that higher-order of oscillation electric signal transmission cable 5 links together with it, its preferable range of ultrasound emission power of this ultrasound emission mechanism is between 1 milliwatt and 20 watts; Its preferable range of hyperacoustic frequency that this ultrasound emission mechanism launches is between 40KHz and 12MHz; The further preferred scope of hyperacoustic frequency that this ultrasound emission mechanism launches is between 80KHz and 12MHz.Arbitrary value within above-mentioned preferred value scope is all the operational parameter value that this case device allows to select; Certainly, the concrete operations parameter value of actual selection will do careful selection according to the concrete condition of concrete analysis object system.
The ultrasonic transducer installed in device certainly can not just one, and that is, the installing quantity of ultrasonic transducer can be more than one, such as: two, three, four, five, six etc.; The quantity of ultrasonic transducer will be selected according to actual needs; Generally speaking, a foot also.
Ultrasonic energy absorber 12 makes it disturb from ultrasound wave for the protection of contrast electrode 13, maintains contrast electrode 13 current potential by this and stablize.
The poromerics in any aperture has certain absorption to shake the function of ripple; The preferred value of this its micropore size of micropore material of this case is less than 1.0 millimeters.
The described ultrasonic energy absorber 12 of any wall thickness all has that certain ultrasound wave is cleared up, absorption function; This case is somebody's turn to do in pen cap shape or the preferred value of its wall thickness of ultrasonic energy absorber 12 of test tube shape is between 0.3 centimetre and 3.0 centimetres.
Contrast electrode 13 itself art-recognized meanings and CONSTRUCTED SPECIFICATION, for analyze professional domain personnel for, be known, therefore this case legend does not describe its CONSTRUCTED SPECIFICATION, only simply illustrates with straight line.
The embodiment of this case device is not limited to this case figure legends.
Claims (1)
1. there is self-cleaning function and without the Electrochemiluminescprocess process pick-up unit of additional interference, the structure of this device comprises electrolytic cell, and, be installed in below electrolytic cell or the photomultiplier of side, described electrolytic cell is installed within magazine, and, working electrode, and, to electrode, and, contrast electrode, described is sheet to electrode, column or thread platinum electrode or gold electrode, described contrast electrode is Ag/AgCl electrode or mercurous chloride electrode, described working electrode is glass-carbon electrode, described working electrode and the working end of electrode and contrast electrode is positioned to the inside of described electrolytic cell, this electrolytic cell is that its opening end profile is square, rectangle, the cup-shaped vessel of circular or oval indent, and, ultrasonic transducer, the installation position of this ultrasonic transducer is the bottom position of lateral location at this electrolytic cell or electrolytic cell, and, higher-order of oscillation electric signal generator, this higher-order of oscillation electric signal generator is connected with described ultrasonic transducer via higher-order of oscillation electric signal transmission cable, this higher-order of oscillation electric signal generator forms ultrasound emission mechanism together with the described ultrasonic transducer linked together with it via higher-order of oscillation electric signal transmission cable, the ultrasound emission power of this ultrasound emission mechanism is between 1 milliwatt and 20 watts, hyperacoustic frequency that this ultrasound emission mechanism launches is between 80KHz and 12MHz, it is characterized in that, the structure of this device also comprises ultrasonic energy absorber, this its profile of ultrasonic energy absorber is test tube shape, its one end closed of ultrasonic energy absorber of being somebody's turn to do in test tube shape is positioned at the inside of electrolytic cell, the inner chamber of this ultrasonic energy absorber is goed deep in its working end of described contrast electrode, this its material of ultrasonic energy absorber is micropore material, described micropore material is micropore ceramics, fine-celled foam glass, fine-celled foam aluminium, microporous silicon rubber, expanded microporous polytetra fluoroethylene-EPTEE or micropore Kynoar, this its micropore size of micropore material is less than 1.0 millimeters, should be that its wall thickness of ultrasonic energy absorber of test tube shape is between 0.3 centimetre and 3.0 centimetres.
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| CN102944629A (en) * | 2012-10-25 | 2013-02-27 | 宁波大学 | Eluting device for sampling program for detecting polychlorinated biphenyl of trace of water body by gas chromatography-mass spectrometry |
| CN102967676A (en) * | 2012-10-25 | 2013-03-13 | 宁波大学 | Elution device for inspecting sampling process of polychlorinated biphenyl pollutant by using gas chromatography-mass spectrometer |
| CN102937632A (en) * | 2012-10-25 | 2013-02-20 | 宁波大学 | Elution device for environmental water polychlorinated biphenyl gas chromatography-mass spectrometer (GC-MS) analyzing and sampling procedure |
| CN102944630A (en) * | 2012-10-25 | 2013-02-27 | 宁波大学 | Device for GC-MS analyzing and sampling of elution procedure aiming to target object PCBs |
| CN106198625A (en) * | 2016-06-02 | 2016-12-07 | 东北电力大学 | One heavy metal species on-line monitoring system device in situ |
| CN108226229A (en) * | 2018-01-31 | 2018-06-29 | 江苏绿港现代农业发展有限公司 | A kind of water quality detection sensor self-cleaning device |
| CN114740061A (en) * | 2022-04-06 | 2022-07-12 | 中国科学院城市环境研究所 | Electrolytic cell for determining chemical oxygen demand |
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| US4033830A (en) * | 1976-03-17 | 1977-07-05 | The Foxboro Company | On-line amperometric analysis system and method incorporating automatic flow compensation |
| CN1146779C (en) * | 1998-04-28 | 2004-04-21 | 北京青谷科技有限公司 | Display screen touch point position parameter sensing device |
| WO2006007533A1 (en) * | 2004-07-01 | 2006-01-19 | Tracedetect, Inc. | Method for ultrasonic cleaning of a working electrode in electrochemical cell useful for automated trace metals measurement |
| US8298391B2 (en) * | 2007-07-11 | 2012-10-30 | Silveri Michael A | Amperometric sensor |
| CN100573108C (en) * | 2007-11-19 | 2009-12-23 | 福州大学 | Heat controlled electric pole electrogenerated chemiluminescence pick-up unit and detection cell preparation method |
| CN101907599B (en) * | 2010-07-21 | 2013-03-27 | 宇星科技发展(深圳)有限公司 | All-in-one heavy metal online analyzer |
| CN102042965B (en) * | 2010-11-18 | 2012-07-11 | 上海衡伟信息技术有限公司 | On-line broad-spectrum water quality analyzer |
| CN102175607B (en) * | 2011-01-19 | 2012-07-25 | 重庆大学 | Small-sized multifunctional sample detection room |
| CN102147373B (en) * | 2011-01-19 | 2012-06-27 | 重庆大学 | Multi-parameter water quality monitoring system based on micro-optical-electro-mechanical system (MOEMS) micro spectrometer |
| CN102070222A (en) * | 2011-03-08 | 2011-05-25 | 广州金川环保设备有限公司 | Method and device for pre-treating oil field sewage by ultrasonic oxidation united with electrochemical oxidation |
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