CN1458519A - Microscopic electrochemical analyzer - Google Patents
Microscopic electrochemical analyzer Download PDFInfo
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- CN1458519A CN1458519A CN03122933A CN03122933A CN1458519A CN 1458519 A CN1458519 A CN 1458519A CN 03122933 A CN03122933 A CN 03122933A CN 03122933 A CN03122933 A CN 03122933A CN 1458519 A CN1458519 A CN 1458519A
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Abstract
The microscopic electrochemical analyzer includes power supply unit, optical microscope, electrolytic bath, video camera, computer, control software with matched with image display and editing functions. The optical microscope is connected via standard CS interface with CCD camera, the CCD camera and the computer are connected via video card, the CCD camera transmits its data to software for control and amplified display in the display, and the electrolytic bath is connected to the outer power supply to constitute the work bath for electrochemical immigration and electrochemical reaction. By means of biological microscopic technology and electrochemical immigration and electrochemical reaction technology, the present invention constitutes the instrument capable of continuous observing, photographing and analyzing electric immigration, reverse emulsion and electrochemical reaction in various polar and non-polar systems and amplifying microscopic dynamic process.
Description
Technical field
The present invention relates to a kind of to oil phase (nonpolar phase)---the device that the electric detachment process of water (polarity phase) system is analyzed particularly relates to a kind of micro-electrochemical analyser.
Background technology
At present, in the process of research crude oil high-tension electricity desalination/electrical dewatering, experiment for each concrete technological parameter all will be analyzed its last salt content/liquid water content, these analyses are often wasted time and energy, and for a kind of specific crude oil, determine its electro-desalting/electrical dewatering optimal processing parameter often to carry out tens to experiments up to a hundred time, need the time more than one month at least.The handled crude oil kind of China's most refinery is changeable, so be difficult to accomplish the specific aim of technological parameter, causes electro-desalting/electrical dewatering poor effect, directly influences the safety of refining process unit.
At this kind situation, the present invention proposes this method that technological experiment and evaluation are dynamic observed and analyze, by observe oil/moisture under the various different technology conditions from microprocess, analyze the quality of various different technology conditions, this method rapidly, intuitively can solve the problem of technology of electric de-salting device in petroleum refining industry.
Summary of the invention
The present invention uses the principle of biology microscope technology, high-tension electricity chemical transport, digital vedio recording technology, has designed and has set up one and be enclosed within electromigration, the breaking that can observe, make a video recording, analyze various polarity phase/nonpolar phase system under the multiple current field condition continuously, the instrument that reaches the electrochemical reaction micro dynamic course.
A kind of micro-electrochemical analyser of the present invention, comprise supply unit, optical microscope, electrolytic cell, video camera, store the computing machine of the control program that cooperates the image demonstration at least, the video card of one data-switching, optical microscope links to each other by standard C S interface with ccd video camera, ccd video camera links to each other by video card with computing machine, after ccd video camera carries out programmed control with data transmission in the computing machine, real-time storage is on the storer of computing machine, and the variation of electrolytic cell internal reaction is shown enlarged on the display of computing machine, the external multifunctional power supply device of electrolytic cell constitutes electrochemical migration, the work pool of electrochemical reaction.
Described micro-electrochemical analyser, its high pressure resistant electrolytic cell is made of the used neutral density glass slide glass of biological microscope, electrode, high-frequency and high-voltage lead and High-Voltage Insulation band, electrode places on the slide glass and adopts the epoxy adhesive close adhesion, the both positive and negative polarity of electrode connects positive and negative high-frequency and high-voltage lead respectively, and the high-frequency and high-voltage lead other end is connected on the output terminal of multifunctional power supply device.
Micro-electrochemical analyser of the present invention, image digitization with various micro dynamic course is stored continuously, the function of editor, computing machine or TV set demonstration, make people's eyes can be very easily on microscope amplifies 10～1500 times computer screen, observe and analyze the transient behavior process of multiple high-tension electricity chemical transport (under the current field condition of E=1～5000V/cm) and electrochemical reaction more intuitively, rapidly, continuously, make the observation of electrochemical research and analysis enter into micron-sized field.
Micro-electrochemical analyser of the present invention, to oil phase (nonpolar phase)---the various electric separation method of water (polarity phase) system, carried out extensive studies, can very photograph various micron-sized oil/water droplets clearly, gathering under various high-voltage electric field effects---the dynamic overall process of---separation---sedimentation of growing up, can system, research and analysis organism/water fast, motion conditions under various high-voltage electric field migration and separation process parameters, research for electrochemical method, detect and analyze, and the rapid screening of electrochemical industry technology, estimate, improve and raising, determining of optimum process condition provides important method and means.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is electrolytic cell vertical view of the present invention and front elevation.
Fig. 3 is a power device structure block diagram of the present invention.
Among the figure: 1. slide glass 2. electrodes 3. liquid 4. lines of anti-high-frequency and high-voltage the 5. bonding agents 6. optical microscope 7.CCD video cameras 8. video cards 9. computing machines 10. high pressure resistant electrolytic cells to be analyzed
Embodiment
The present invention is further illustrated below in conjunction with drawings and Examples.
See also shown in Figure 1, a kind of micro-electrochemical analyser of the present invention, by supply unit, electrolytic cell 10, optical microscope 6, CCD (promptly digital) video camera 7, video card 8 and computing machine 9 are formed, optical microscope 6 links to each other by standard C S interface with ccd video camera 7, ccd video camera 7 links to each other by video card 8 with computing machine 9, ccd video camera 7 carries out data transmission to be presented on the display after the software control in computing machine 9, micro cell 10 external power supply devices constitute electrochemical migration, the work pool of electrochemical reaction, this micro cell 10 has the specific function of anti-high-voltage breakdown.
In the present invention, micro cell 10 is made of the used neutral density glass slide glass 1 of biological microscope, copper electrode 2, high-frequency and high-voltage lead 4, copper electrode 2 places on the slide glass 1 and adopts epoxy adhesive 5 close adhesion, the both positive and negative polarity of copper electrode 2 connects positive and negative high-frequency and high-voltage lead 4 respectively, and high-frequency and high-voltage lead 4 other ends are connected on the output terminal of multifunctional power.
In the present invention, microimaging comprises optical microscope 6 and ccd video camera 7, and optical microscope 6 has the standard C S interface that connects ccd video camera 7, and is equipped with special-purpose long-focal length lens and high projector.Ccd video camera 7 adopts sharpness more than 420 lines, and the output standard is P system or N system, and the video camera with low illuminance.Ccd video camera 7 links to each other with computing machine 9 by video line 8, and the galvanochemistry dynamic process image with being taken the photograph converts digital signal to, is sent to computing machine and storage or processing, shows by graphoscope again.
Micro-electrochemical analyser of the present invention, its sequence of operation is:
(a) liquid 3 to be analyzed is splashed in the micro cell 10, be placed on the objective table of microscope 6;
(b) open multifunctional power, regulate output waveform, close multifunctional power;
(c) open computing machine 9, and open Control Software;
(d) regulate microscope 6 and video camera 7, make clear being presented on the computer display of micro-image of the analytic liquid 3 in the micro cell 10, and begin shooting;
(e) multifunctional power output is loaded on the micro cell 10, observes and write down the case of iontophoresis in the micro cell 10;
(f) as the case may be with actual requirement, regulate multifunctional power output voltage and waveform, regulate microscope 6 and video camera 7;
(g) computing machine 9 real time record, storage, reservation view data;
(h) experiment finishes, successively powered-down, video camera, microscope.
For example: oil/W Em natural or artificial preparation is splashed between the electrode in little high pressure resistant electrolytic cell 10, and be placed on the objective table of optical microscope 6; Open multifunctional power, the adjusting waveform is a triangular wave, closes multifunctional power; Open computing machine 9, and open Control Software; Adjusting optical microscope 6 and the ccd video camera 7 clear observation electrochemical reactions of energy also are presented on the display of computing machine; Multifunctional power is applied electric field, frequency is that 5000Hz output is loaded on the micro cell 10, can see clearly in display that the little water droplet that has amplified in more than the 1000 times of oil under the effect of electric field force, attracts each other, forms the process of water chain, collision, distortion, gathering, sedimentation.
Carry out concrete oil/moisture from the time, can according to oil/moisture from difficulty or ease, suitably strengthen or weaken electric field, or change waveform, peak pulse duration.
The oil product that has can add emulsion breaker when separating, analyser of the present invention can be observed the phenomenon that oil/aqueous systems of being added with different emulsion breakers is separated respectively under electric field, evaluates the quality of emulsion breaker.
Micro-electrochemical analyser each several part of the present invention had both had independence, have simultaneously well mutual coordination function again, realize microscopic observation, demonstration, the process analysis of the transient behavior process of multiple electrochemical migration, the emulsification of organic and inorganic phase, electrochemical reaction jointly.
Optical microscope
Optical microscope has the standard C S interface that connects ccd video camera, micro-enlargement factor scope: 10～1500 times, be equipped with special-purpose long-focal length lens and high projector.
Ccd video camera
Ccd video camera adopts sharpness more than 420 lines, and the output standard is P system or N system, and the video camera with low illuminance,
Computing machine and software.
The CCD camera head links to each other with microcomputer by video line, and the high-tension electricity chemistry dynamic process image with being taken the photograph converts digital signal to, is sent to computer stored or processing, shows by microcomputer monitor again.Though it is very big that this microscope camera system, is mainly considered institute's memory image and film file for the requirement of microcomputer, so all very high to technical requirement configurations such as the hard-disc storage amount of computing machine and travelling speed.
The view data switching software, being specifically designed to the image that ccd video camera is photographed gathers, and convert digital signal to, be input in the computing machine, require time response fast, can in time carry out the collection and the projection of galvanochemistry image, special software has instantaneous shooting and image editing function.
The major technique characteristics and the index of multifunctional power supply device output in the present invention:
Electric field signal output: the electric current and the voltage of high-voltage alternating, high voltage direct current, high voltage ac/dc, high frequency, high frequency direct current superposition electric field;
High-frequency signal waveform: pulsating wave, triangular wave, square wave, zigzag wave;
High-frequency signal peak pulse duration: can regulate continuously in 0～50% scope;
High-frequency electric field frequency: 400～50000Hz, scalable continuously;
Output voltage: 0～10000V, adjustable continuously;
Output current: 0～5.0A;
Output power: 100～3000VA.
Fig. 2 is the vertical view and the front elevation of micro cell, it is with multifunctional power supply device, constitute the work pool part of high-tension electricity chemical transport, electrochemical reaction, have the novelty design of specific functions such as high pressure resistant puncture, discharge, constitute micro-electrochemical analyser with microimaging and data handling system.
Micro cell 10 operating voltage: 0～10000 volt AC field, DC electric field, alternating current-direct current electric field, and the high-frequency and high-voltage electric field of 400～50000Hz, 0～10000V;
Electric field intensity: 0～5000V/cm;
Voltage or electric current can be regulated continuously, and high-tension electricity puncture phenomenon can not take place, and system is high pressure resistant stable and reliable;
Micro cell design and composed as follows:
(1) because micro cell 10 will be placed under the microscope camera system and observe, therefore chooses the pond body infrastructure component of the used neutral density glass slide glass of biological microscope as the micro cell system.
(2) the little copper bar of two high conductions of intercepting is as the positive and negative electrode of micro cell.Choose the special lead of anti-high-frequency and high-voltage that two length suitably contain the multiply copper cash, with the welding of two copper electrodes, then that copper sheet is smooth with sand papering respectively, make its can with the microslide close adhesion, without any the slit.
(3) use High Performance Insulation glue, two copper electrodes are bonded on the microslide, must guarantee to make two electrodes parallel as far as possible.For satisfying the needs of different researchs, make the electrode of different spacing.The exposed part of electrode both sides, the potpourri sealing with epoxy resin and hardening agent prevents that oil sample overflows in the experimentation.
That the high-frequency and high-voltage electro-desalting/electrical dewatering technology of electrolytic cell 10 has is energy-conservation 30%, save time 50%, separation efficiency improves 50～90%.
Microscope 6 among the present invention, be on the basis of traditional optical microscope, adopt the special-purpose object lens of the long depth of field, the distance of camera lens and analyzed sample can be more than 5mm, thus make camera lens and sample strip insulating property, prevent that the atmospherical discharges and the breakdown performance of high-voltage electric field strengthen greatly.
Ccd video camera 7 among the present invention adopts the video camera of 30～300 hardwood/seconds, and the special-purpose view data software decoding card of employing, data processing adopts the computer system that operation is fast, storage is big, display performance is good, designs and set up the microimaging and the data processing display system of function admirable.
Micro-electrochemical analyser of the present invention can also be used to observing that other is nonpolar---polarity two-phase system, the gathering under the effect of electric field force or the phenomenon of separation.
Micro-electrochemical analyser of the present invention, can not only clearly observe organic phase---the situations such as shape, size and distribution of the various micron order water droplets of aqueous phase, can also be with the micron order water droplet, electromigration under multiple current field condition, electrofocusing, grow up, a series of continuous dynamic processes such as sedimentation, micro-, quick shooting, data storage and note, and by computing machine high-fidelity display, continuous demonstration, show and carry out view data and handle.
Electrochemical analyser of the present invention can be to the analysis and optimization of technological process such as the high-voltage alternating electrical dewatering that recovers the oil in the petroleum industry, high voltage direct current electrical dewatering, emulsion breaker competition and parameter.
Electrochemical analyser of the present invention also can be to the analysis and optimization of technological processs such as the alternating current desalination in the petroleum refining industry, direct current desalination, alterating and direct current desalination, emulsion breaker competition, oil product electrofining and parameter.
Electrochemical analyser of the present invention also can separate with inorganic electricity mutually organic phase in the bionic biologics, the analysis and optimization of electrofining technological process and parameter.Or the like.
Micro-electrochemical analyser of the present invention, to oil phase (organic phase)---the various electric separation method of aqueous systems, carried out extensive studies, can very photograph various micron-sized oil/water droplets clearly, gathering under various electric field actions---the dynamic overall process of---separation---sedimentation of growing up, can system, research and analysis organism/water fast, motion conditions under various electric field migration and separation process parameters, research for electrochemical method, detect and analyze, and the rapid screening of electrochemical industry technology, estimate, improve and raising, determining of optimum process condition provides important method and means.
The micro dynamic course of electromigration and electrochemical reaction under the various high-voltage electric field effects can be observed, be detected, take, store, show to micro-electrochemical analyser of the present invention continuously, such as: the electro-deposition of electroplating process, the electrophoresis process of organic additive, the dynamic link of organic polymer under electric field action, the growth of cell with change or the like, can be widely used in the determining and improve etc. of scientific research, analysis, detection, manufacture of multiple industrial circles such as petrochemical complex, bioengineering, medical industry.The micro-electrochemical analysis system of utilize setting up has been studied the micro dynamic course of oil/water power migration, determines to provide approach accurately and fast for the electro-desalting optimal processing parameter.
Claims (9)
1, a kind of micro-electrochemical analyser, comprise high-voltage power apparatus, optical microscope, electrolytic cell, it is characterized in that: also comprise ccd video camera (7), store the computing machine (9) of the control program that cooperates image demonstration and editting function at least, the video card of one data-switching (8), the same ccd video camera of optical microscope (6) (7) links to each other by standard C S interface, ccd video camera (7) links to each other by video card (8) with computing machine (9), after ccd video camera (7) carries out programmed control with data transmission in the computing machine (9), be stored in constantly on the storer of computing machine, and the variation of high pressure resistant electrolytic cell (10) internal reaction is shown enlarged on the display of computing machine, the external multifunctional high-voltage power supply device of high pressure resistant electrolytic cell (10) constitutes electrochemical migration, the work pool of electrochemical reaction.
2, micro-electrochemical analyser according to claim 1, it is characterized in that: described electrolytic cell (10) is made of the used neutral density glass slide glass (1) of biological microscope, electrode (2), high-frequency and high-voltage lead (4), electrode (2) places slide glass (1) to go up and adopt epoxy adhesive (5) close adhesion, the both positive and negative polarity of electrode (2) connects positive and negative high-frequency and high-voltage lead (4) respectively, and high-frequency and high-voltage lead (4) other end is connected on the output terminal of multifunctional high-voltage power supply device.
3, micro-electrochemical analyser according to claim 1, it is characterized in that: described optical microscope (6) has the standard C S interface that connects ccd video camera (7), and special-purpose long-focal length lens and the high projector of outfit, ccd video camera (7) adopts sharpness more than 420 lines, the output standard is P system or N system, and the video camera with low illuminance.
4, micro-electrochemical analyser according to claim 1, it is characterized in that: ccd video camera (7) by video card (8) with the galvanochemistry dynamic process image of being taken the photograph, convert digital signal to, be sent to computing machine and storage or processing, show by the graphoscope amplification again.
5, micro-electrochemical analyser according to claim 1, it is characterized in that: it is observed 10～1500 times of optical microscope (6) that graphoscope amplifies the enlargement factor that shows, and can multistagely regulate, micro-and amplify, camera speed is fast, data processing is image conversion data special software to be matched composing images data professional treatment and demo system with computer system.
6, micro-electrochemical analyser according to claim 1 is characterized in that: multifunctional power supply device output performance index is,
Electric field signal output: high-voltage alternating, high voltage direct current, high voltage ac/dc, high frequency, high frequency direct current superposition
The electric current of electric field and voltage;
High-frequency signal waveform: pulsating wave, triangular wave, square wave, zigzag wave;
High-frequency signal peak pulse duration: can regulate continuously in 0～50% scope;
High-frequency electric field frequency: 400～50000Hz, scalable continuously;
Output voltage: 0～10000V, adjustable continuously;
Output current: 0～5.0A;
Output power: 100～3000VA.
7, micro-electrochemical analyser according to claim 1 is characterized in that: the technical feature of electrolytic cell (10) is,
Operating voltage: 0～10000 volt AC field, DC electric field, alternating current-direct current electric field, and 400～
The high-frequency and high-voltage electric field of 50000Hz, 0～10000V;
Electric field intensity: 0～5000V/cm;
8, micro-electrochemical analyser according to claim 1, it is characterized in that: microimaging, can clearly observe shape, the size of the various micron order drops of nonpolar phase-polarity in mutually and situation about distributing, can also be with the micron order water droplet, electromigration under multiple current field condition, electrofocusing, grow up, a series of continuous dynamic processes of sedimentation, micro-, quick shooting, data storage and note, and by computing machine high-fidelity display, continuous demonstration, show and carry out view data and handle.
9, micro-electrochemical analyser according to claim 2 is characterized in that: the high-frequency and high-voltage electro-desalting/electrical dewatering technology of electrolytic cell (10) have energy-conservation 30%, save time 50%, separation efficiency brings up to more than 50～90%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03122933 CN1209620C (en) | 2003-04-26 | 2003-04-26 | Microscopic electrochemical analyzer |
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| CN 03122933 CN1209620C (en) | 2003-04-26 | 2003-04-26 | Microscopic electrochemical analyzer |
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| CN1458519A true CN1458519A (en) | 2003-11-26 |
| CN1209620C CN1209620C (en) | 2005-07-06 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012074831A1 (en) * | 2010-12-02 | 2012-06-07 | General Electric Company | Static desalter simulator |
| CN102798735A (en) * | 2012-08-14 | 2012-11-28 | 厦门大学 | Pinpoint enhanced dark-field microscope, electrochemical testing device and leveling system |
| CN103344691A (en) * | 2013-06-19 | 2013-10-09 | 北京邮电大学 | Water-drop test system for electrochemical migration experiment |
-
2003
- 2003-04-26 CN CN 03122933 patent/CN1209620C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012074831A1 (en) * | 2010-12-02 | 2012-06-07 | General Electric Company | Static desalter simulator |
| CN103228767A (en) * | 2010-12-02 | 2013-07-31 | 通用电气公司 | Static desalter simulator |
| CN102798735A (en) * | 2012-08-14 | 2012-11-28 | 厦门大学 | Pinpoint enhanced dark-field microscope, electrochemical testing device and leveling system |
| CN103344691A (en) * | 2013-06-19 | 2013-10-09 | 北京邮电大学 | Water-drop test system for electrochemical migration experiment |
| CN103344691B (en) * | 2013-06-19 | 2015-06-10 | 北京邮电大学 | Water-drop test system for electrochemical migration experiment |
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| Publication number | Publication date |
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| CN1209620C (en) | 2005-07-06 |
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