• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    In the present invention, by placing the electrode and the washing nozzle capable of simultaneously performing the measurement agitation function for the measurement of trace elements in one cell at the same time, has a structurally compact configuration, according to the surface state of the electrode In order to solve the problem that the potential is changed, the electrode support cover 210 having the mounting holes 211, 212, and 213 formed so that the reference electrode 401 and the auxiliary electrode 402 are installed on the upper portion, and the lower portion of the support cover. A cell assembly 200 comprising a cell 220 disposed in the cell 220 to provide an enclosed space, an assembly disk 230 disposed below the cell, and a base block 240 having a square block shape for supporting the assembly disk. Wow; A glass carbon electrode assembly 100 inserted into a mounting hole of the electrode support cover 210 to simultaneously perform a role of an agitator and a role of an electrode; A washing nozzle 222 disposed at the center of the cell pedestal 221 of the cell 220; There is provided a glass carbon electrode system including a nozzle control circuit unit 307 for controlling the nozzle operating device 500 for spraying the cleaning liquid toward the glass carbon electrode assembly 100 through the cleaning nozzle 222.
    公开号:KR20040041233A
    申请号:KR1020020069395
    申请日:2002-11-09
    公开日:2004-05-17
    发明作者:전병성；이재춘
    申请人:강영진；
    IPC主号:
    专利说明:

    Glass Carbon Electrode System {GLASSY CARBON ELECTRODE SYSTEM}
    [13] The present invention relates to a glass carbon electrode system, and more particularly, to a glass carbon electrode system capable of completely washing an electrode with a washing nozzle, and simultaneously using a trace element measuring function and a measuring object stirring function. .
    [14] In general, polarography, which is generally used for quantitative qualitative analysis of various trace components, uses a principle in which voltage-current characteristics are proportional to the type and concentration of analyte.
    [15] Polarography is an electrochemical method for analyzing solutions consisting of oxidizing or reducing substances, called voltammetry, and was developed in 1922 by the Czech chemist Jaroslav Herovsky.
    [16] Jaroslav Herovsky put the solution to be analyzed into a glass cell containing two electrodes, with mercury dripping from the capillary of one electrode made of glass capillary. To be stored.
    [17] In the prior art dropping mercury electrode system in which such an electrode system is practically used, as shown in FIG. 1, mercury 8 in the mercury storage container 1 is dropped at the end of the glass capillary tube as the opening / closing valve 3 is opened. A dropping mercury electrode 2, a reference electrode 5, and a platinum auxiliary electrode 6, which are dropped and subsequently dropped into the cell 8, are provided inside the cell 8 in which the sample solution is contained.
    [18] Here, the mercury storage container (1) is configured to adjust the height to control the drop rate of the mercury drop, the on-off valve (3) to adjust the opening and closing time to ensure that the appropriate size of the mercury drops hanging on the capillary bottom It is configured to be.
    [19] The dropping mercury electrode 2, the reference electrode 5, and the platinum auxiliary electrode 6 are connected in series with an electric circuit and an ammeter which can control 0V to 2V.
    [20] Normally, when the dropping mercury electrode is connected to the cathode of the polarization voltage, the voltage slightly increases and the current corresponding to this voltage can be detected by an ammeter. The current flowing in the dropping mercury electrode is very small until it is applied a voltage large enough to reduce the material to be analyzed. When the applied voltage increases above this threshold, the current initially increases rapidly, but gradually reaches a certain value and remains constant to some degree as the voltage increases further. The threshold voltage needed to rapidly increase the current is a characteristic of the material to be reduced, which is the value that identifies (qualitatively analyzes) the material. Under appropriate conditions, the specific limiting current is controlled by the rate at which the reducing material diffuses to the surface of the mercury, and the magnitude of the limiting current is consistent with the measurement of the concentration of the reducing material (quantitative analysis). The limiting current may be obtained by oxidizing the oxidizing material when the dropping electrode is the anode. If the solution contains several substances that are reduced or oxidized at different voltages, the voltage-current curve shows an increase in discrete currents (polar graph wave) and a limiting current for each. Therefore, this method is useful for detecting or determining several substances at the same time, and can detect or determine substances even at relatively very small concentrations of 1 ppm to 1,000 ppm.
    [21] Thus, in the case of using a fixed electrode such as platinum as a working electrode in graphy, the mercury electrode is mainly used because the potential of the working electrode varies depending on the surface state of the electrode. When mercury electrodes are used, mercury droplets grow and new surfaces are continuously exposed to the analyte, resulting in more reproducible voltage-current characteristics than using fixed surfaces.
    [22] As described above, the conventional dropping mercury electrode using the capillary phenomenon has a problem in that the mercury column is frequently broken by the impact. When the measurement is carried out while the mercury drop is suspended at the end of the capillary tube, the mercury drop drops due to the impact or other causes.
    [23] In particular, during the reduction reaction, the contamination inside the capillary proceeds, and mercury droplets do not hang at the end of the capillary tube and often fall off, and thus cannot be stably measured. In addition, the size of the mercury electrode, which is the most important variable in the measurement, changes greatly every time the electrode is produced, making accurate measurement difficult.
    [24] Accordingly, the present applicant has developed and registered the mercury electrode system of the Korean patent No. 265023 No. 265023 in 2000 to solve this problem.
    [25] This patent can be stably fixed to the mounting groove formed on the upper end of the capillary tube accurately measured mercury using a precision injector in the above-mentioned general voltammetry, it was characterized by a stable measurement of trace elements.
    [26] After that, the applicant can use the trace element measurement function and the measuring material stirring function at the same time in the product production step, and can detect several substances at the same time, including the pH measurement of relatively simple water quality, and the product capable of continuous repeated automatic measurement Invented.
    [27] In the prior art, when the fixed electrode is used, there is a problem in that the potential of the working electrode varies depending on the surface state of the electrode. As a result, a kit for cleaning a separate fixed electrode is used. As a result, the configuration of the compact cell is complicated.
    [28] Accordingly, an object of the present invention is to arrange the glass carbon electrode and the cleaning nozzle simultaneously in one cell, which can simultaneously perform the measurement agitation function for the measurement of trace elements, has a structurally compact configuration, the surface state of the electrode It is to provide a glass carbon electrode system that solves the problem that the potential of the working electrode is changed in accordance with.
    [1] 1 is a schematic view showing a part of a dropping mercury electrode system according to the prior art,
    [2] Figure 2 is a perspective view for explaining the configuration of a glass carbon electrode system according to an embodiment of the present invention,
    [3] 3 is an exploded perspective view of the glass carbon electrode shown in FIG.
    [4] 4 is a cross-sectional view for explaining the coupling relationship and the operating relationship of the glass carbon electrode system shown in FIG.
    [5] ♣ Explanation of symbols for main part of drawing ♣
    [6] 100: glass carbon electrode assembly 200: cell assembly
    [7] 210: electrode base cover 220: cell
    [8] 221: cell support 222: cleaning nozzle
    [9] 230: assembly disk 240: base
    [10] 300: electronic circuit system 307: nozzle control circuit
    [11] 401: reference electrode 402: auxiliary electrode
    [12] 500: nozzle operating device 600: supply recovery device
    [29] An object of the present invention described above is to provide a reference electrode, an electrode support cover having a mounting hole so that the auxiliary electrode is installed on the top, a cell disposed under the support cover to provide a closed space, and disposed below the cell. A cell assembly comprising an assembled disk and a base having a square block shape for supporting the assembly disk; A glass carbon electrode assembly inserted into a mounting hole of the electrode support cover to simultaneously perform a role of an agitator and a role of an electrode; A washing nozzle disposed at the center of the cell pedestal of the cell; This cleaning nozzle is achieved by a glass carbon electrode system comprising a nozzle control circuit for controlling a nozzle operating device for spraying the cleaning liquid toward the glass carbon electrode assembly.
    [30] Hereinafter, the glass carbon electrode system according to the preferred embodiment of the present invention will be described in detail with reference to FIGS. 2 to 4.
    [31] 2 is a perspective view for explaining the configuration of a glass carbon electrode system according to an embodiment of the present invention, Figure 3 is an exploded perspective view of the glass carbon electrode shown in Figure 2, Figure 4 is shown in Figure 2 It is a cross-sectional view for explaining the coupling relationship and the operating relationship of the glass carbon electrode system.
    [32] As shown in FIG. 2, in the glass carbon electrode system of the present invention, the glass carbon electrode assembly 100 having a stirrer, the cell assembly 200, the electronic circuit system 300 for measurement and control, and the reference electrode 401 are provided. And an auxiliary electrode 402 is provided.
    [33] The glass carbon electrode assembly 100 operates as a motor inside to serve as a stirrer and mounts a glass carbon electrode on a rotating shaft equipped with a stirring blade, thereby simultaneously serving as a fixed electrode and a fixed electrode. Parts.
    [34] The cell assembly 200 has a semi-elliptic electrode base cover 210 and a cell 220 formed of a glass to plastic material having a high corrosion resistance and acid resistance, which is disposed under the semi-elliptic electrode support cover 210 to provide a closed space. The disk 230, and the base 240 of the rectangular block shape for supporting the assembly disk.
    [35] Here, the electrode support cover 210 has mounting holes 211, 212, 213 vertically penetrated to mount the glass carbon electrode assembly 100, the reference electrode 401, and the auxiliary electrode 402 in a vertical or inclined manner. ), And has connection ports 214 and 215 to which hoses are connected to inject pure water (distilled water), electrolyte, sample, standard sample, and the like.
    [36] In addition, the cell 220 is supported by a circular cell pedestal 221 at the bottom, and is screwed into the upper seating groove of the assembly disk 230. In the inner center of the cell pedestal 221, a cleaning nozzle (222: cleaning nozzle) is protruded, and the discharge hole 223 is formed to be recessed. The washing nozzle 222 is connected to the nozzle operating device 500 (see FIG. 4) through the inlet 241 of the base 240 to wash the surface of the glass carbon electrode bar with a high pressure washing liquid (pure water). . The discharge hole 223 is provided with a recovery passage supply pump and a vacuum to supply and recover gas (nitrogen) to liquid (sample, standard sample, distilled water, and electrolyte) used for measurement through the outlet 231 of the assembly disk 230. It is connected to a supply recovery device 600 having a pump (not shown).
    [37] In addition, the assembly disk 230 is fixed to the upper surface of the base portion 240 by screwing, and one side of the base portion 240 is fixed to the fixing bolt hole so that the cell assembly 200 is detachably attached to the installation surface. 290 are forming.
    [38] On the other hand, the electronic circuit system 300 is an automatic control algorithm for the operation of the glass carbon electrode assembly 100 to be described in detail below, the trace element measurement operation, the cleaning operation, and supply control of the sample, electrolyte, pure water, nitrogen It is equipped with a component analysis algorithm and performs a component analysis in proportion to the type and concentration of analyte with a measured voltage-current value.
    [39] As shown in FIG. 3, the glass carbon electrode assembly 100 includes a cylindrical upper and lower housings 110 and 111, which can be disassembled and assembled with threads, and a motor 120 mounted inside the housing. A shaft connecting member 130 of an inert polymer (PEEK) material, which is secured by fitting to the rotating shaft 121 of the motor and serves as insulation, and such a shaft connecting member 130 is inserted into the shaft and can be freely rotated. The electrode connector 140 having an axial hole 141 of a size, and is mounted inside the electrode connector and screwed to the lower portion of the shaft connecting member 130, thereby serving as a contact electrode and a rotational force transmitting member. At the same time, the drive shaft 150 made of stainless material, the bearing 160 fitted to the drive shaft, and the fluorine screwed to the lower end of the drive shaft and are actually in contact with the standard sample, electrolyte, pure water, and sample. Hollow teflon bar 170 of a resin material, and the glass carbon electrode bar 180 is inserted into the lower axis of the Teflon bar 170, and electrically connected to the drive shaft 150.
    [40] Here, the motor 120 is connected to the power supply unit of the electronic circuit system to be described later through the power supply line, and serves to rotate and stop the rotating shaft 121 at high speed according to a control signal. The motor 121 forms a bolt fastening flange 122 and is fixed to an upper surface of the electrode connector 140.
    [41] The electrode connector 140 has three semicircular vertical grooves 141, 142, and 143 which are radially disposed at a center angle of 120 ° and extend in the longitudinal direction, and are connected to the lower ends of these three vertical grooves, and the circumferential direction of the electrode connector One horizontal groove 144 extending in the circumferential surface is formed.
    [42] At the point where the vertical grooves 141, 142, 143 and the horizontal groove 144 meet each other, contact mounting holes 145 and 146 are formed to penetrate the axial hole 141 of the electrode connector 140, respectively.
    [43] The contacts 147 are inserted into the three installation holes 145 and 146, respectively, to support the drive shaft 150 with a predetermined elastic force to transmit the probe current to the electronic circuit system through the wire. To this end, the contacts 147 are fixed to a stainless steel coil spring and two stainless steel balls disposed at both ends thereof, and a stainless steel ball which overcomes the elastic force and is inserted into and fixed to the installation holes 145 and 146. It consists of pins.
    [44] The electrode connector 140 is mounted on the lower housing 111 by inserting the vertical grooves 141, 142, and 143 into the guide protrusion formed in the inner diameter of the lower housing 111.
    [45] Meanwhile, the Teflon bar 170 surrounding the end of the driving shaft 150 and the glass carbon electrode bar 180 is flame retardant and has excellent heat resistance, and exhibits excellent resistance to all chemicals, fluorine gas, chlorine trifluoride, and molten alkali. It is stable against all chemicals except metals, is not eroded by all acids, alkalis, oxidizing agents and organic solvents, and has good electrical insulation and excellent high frequency characteristics, so it is very suitable for the glass carbon electrode system of the present invention. In the case of using the fixed electrode at, the potential of the working electrode can be minimized depending on the surface state of the electrode. In fact, the glass carbon electrode bar 180 is all wrapped around the outer circumferential surface by the Teflon bar 170, but because the lower end exposed to the outside completely washed with a washing nozzle to be described below, a precise probe can be made .
    [46] Meanwhile, a plurality of mounting grooves 115 are formed in the lower seating portions 114 of the lower housings 110 and 111, and a plurality of O-rings 112 and 113 are fastened to these grooves, respectively, so that these O-rings 112, 113 serves to seal the inside of the cell 220 when the glass carbon electrode assembly 100 is mounted.
    [47] In addition, the motor 120, the shaft connecting member 130, the electrode connector 140, the drive shaft 150, the bearing 160, and the Teflon bar 170 are disposed in the upper and lower housings 110 and 111 in the above-described order. ) And the glass carbon electrode bar 180 are assembled, the upper and lower housings 110 and 111 are screwed together. In this case, the teflon bar 170 protrudes through the axial hole of the lower seating portion 114 of the lower housing 111. The protruding Teflon bar 170 is fixed to the stirring blade 190 is fit fitting.
    [48] As shown in FIG. 4, the glass carbon electrode assembly 100 and the other electrodes 401 and 402 are mounted to the electrode support cover 210 of the cell assembly 200 and have voltages of + 5V, + 12V, and ± 15V. A measurement control circuit section 304 having an analog-to-digital converter 302 and a digital-to-analog converter 303 for supplying a current signal for measuring trace elements in an electronic circuit system 300 operating as a power supply 301; And a motor drive control circuit section 305 for supplying power and power required for driving the motor.
    [49] In addition, the electronic circuit system 300 connects the supply recovery device control circuit section 306 and the nozzle control circuit section 307 to the supply recovery device 600 and the nozzle operating device 500, respectively.
    [50] Here, the nozzle operating device 500 is provided with a pump (not shown) which is a pressure generating means, which pumps the pure water of the washing liquid container 501 to a high pressure cleaning nozzle according to a control signal of the nozzle control circuit unit 307. 222.
    [51] Hereinafter, the operation relationship of the glass carbon electrode system of the present invention will be described.
    [52] First, in order to analyze the trace elements, the potential difference is measured by the glass carbon electrode bars 180 of the glass carbon electrode assembly 100 controlled by the electronic circuit system 300 by injecting the sample and the standard sample into the cell in order. The result of the calculation is computed by a computer for analysis of results (not shown).
    [53] In more detail, the supply recovery device 600 performs a drain procedure according to the control signal of the supply recovery device control circuit unit 306. In the recovery procedure, first, the recovery of the pre-used preservation solution is started, and then the motor drive control circuit unit 305 rotates the rotating shaft of the motor of the glass carbon electrode assembly 100 in accordance with the control signal, thereby stirring blade 190 ) Rotates the storage solution while rotating at high speed, and the storage solution thus stirred is completely removed from the inside of the cell by the supply and recovery device 600, and the rotating shaft of the motor is stopped.
    [54] Then, the supply recovery device 600 injects fresh pure water and electrolyte into the cell to clean the inside of the cell again.
    [55] Then, in order to completely remove the air remaining in the cell, the supply recovery device 600 introduces nitrogen into the cell according to the control signal of the control circuit unit 306 and performs the above-described recovery procedure once more.
    [56] In this state, the electronic circuit system 300 starts the blank measurement procedure via the measurement control circuit section 304. At this time, the potential difference in the vacuum state is measured through the glass carbon electrode bar 180 mounted on the shaft connecting member, the drive shaft and the Teflon bar in the direction of the rotation axis of the motor, and the measurement control circuit 304 is an analog-to-digital converter 302 The result of the blank state is obtained by converting to digital data at. Thereafter, the nozzle control circuit unit 307 operates the nozzle operating device 500 to clean the end of the glass carbon electrode bar 180 by spraying pure water from the washing nozzle 222, and then to the supply recovery device 600. Recovery procedure is performed.
    [57] Next, the electronic circuit system 300 performs a sample measurement procedure through the measurement control circuit unit 304. In the sample measurement procedure, first, the sample is input into the cell by the feed recovery device 600, and then nitrogen is introduced to remove air. Thereafter, the measurement control circuit 304 measures the potential difference of the sample through the glass carbon electrode bar 180, and performs the same as above, and obtains the result of the sample in the same manner as before. Then, as before, the end of the glass carbon electrode bar 180 is washed and the recovery procedure is performed.
    [58] The electronic circuit system 300 then performs a standard sample measurement procedure via the measurement control circuitry 304. In the standard sample measurement procedure, first, the standard sample is input into the cell by the supply recovery device 600, and then nitrogen is introduced to remove air. Thereafter, the measurement control circuit unit 304 measures the potential difference of the sample through the glass carbon electrode bar 180. As described above, the result of obtaining the standard sample and the cleaning and recovery procedures of the glass carbon electrode bar 180 are performed. do.
    [59] The results of the blanks obtained in this manner, and the results of the samples and the standard samples are transmitted to the computer, and the computer receives the results and performs the malleability analysis.
    [60] According to the present invention described above, it is possible to configure a compact cell in accordance with the provision of a glass carbon electrode assembly that performs the role of a stirrer and an electrode at the same time, quantitative qualitative analysis without using a conventional dropping or dropping mercury electrode There is an effect of providing a glass carbon electrode system that can be performed.
    [61] In addition, in the glass carbon electrode assembly of the present invention, since the glassy carbon electrode is surrounded by a standard sample, electrolyte, pure water, and fluorine resin Teflon bar in contact with the samples, the surface state of the electrode generated from the existing fixed electrode Has the effect that can solve the problems caused by the change at once.
    [62] In addition, the glass carbon electrode system of the present invention can simplify the entire system of the trace element analysis device because it does not use mercury, and even beginners have the advantage of being safe and comfortable to use.
    [63] In addition, the glass carbon electrode system of the present invention is installed in a dropping mercury electrode near the washing nozzle, it can be easily used in the existing dropping mercury electrode system, it is a high-quality product that can realize more precise quantitative qualitative analysis There is an advantage that can be provided.
    [64] Although the technical idea of the glass carbon electrode system of the present invention described above has been described with the accompanying drawings, this is for illustratively describing the best embodiments of the present invention, but not for limiting the present invention. In addition, it is obvious that any person skilled in the art can make various modifications and imitations without departing from the scope of the technical idea of the present invention.
    权利要求:
    Claims (3)
    [1" claim-type="Currently amended] The electrode support cover 210 having the mounting holes 211, 212, and 213 formed thereon so that the reference electrode 401 and the auxiliary electrode 402 is installed on the upper portion thereof, and disposed below the support cover to provide a closed space. A cell assembly 200 comprising a cell 220, an assembly disc 230 disposed below the cell, and a base 240 having a square block shape for supporting the assembly disc;
    A glass carbon electrode assembly 100 inserted into a mounting hole of the electrode support cover 210 to simultaneously perform a role of an agitator and a role of an electrode;
    A washing nozzle 222 disposed at the center of the cell pedestal 221 of the cell 220;
    And a nozzle control circuit unit (307) for controlling the nozzle operating device (500) for spraying the cleaning liquid toward the glass carbon electrode assembly (100) through the cleaning nozzle (222).
    [2" claim-type="Currently amended] The method of claim 1,
    The glass carbon electrode assembly 100 includes a cylindrical upper and lower housings 110 and 111 that can be disassembled and assembled with a screw thread, a motor 120 mounted inside the housing, and a rotating shaft 121 of the motor. Axial connection member 130 made of an inert polymer (PEEK) material that is fixed by interference fit and serves as an insulation, and the shaft connection hole 130 of the size that can be freely rotated by being inserted into the shaft center The electrode connector 140 having a) and a screw shaft mounted to the inside of the electrode connector and screwed to the lower portion of the shaft connecting member 130, thereby driving a stainless steel drive shaft simultaneously serving as a contact electrode and a rotational force transmitting member. 150, a bearing 160 fitted to the drive shaft, and a fluororesin hollow type screwed to the lower end of the drive shaft and actually contacting a standard sample, an electrolyte, pure water, a sample, and the like. Teflon bar 170 and the glass carbon electrode bar 180 is inserted into the lower shaft center of the Teflon bar 170, and electrically connected to the drive shaft 150, the upper, lower housings 110 and 111 After assembling the glass carbon electrode system, characterized in that the stirring blades 190 are fixed to the Teflon bar 170 protruding through the axial hole of the lower seating portion 114 of the lower housing 111.
    [3" claim-type="Currently amended] The method according to claim 1 or 2,
    A plurality of seating grooves 115 are formed in the lower seating portions 114 of the lower housings 110 and 111, and O-rings 112 and 113 are fastened to the seating recesses 115, respectively. Glass Carbon Electrode System.
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    同族专利:
    公开号 | 公开日
    KR100485989B1|2005-05-03|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    法律状态:
    2002-11-09|Application filed by 강영진
    2002-11-09|Priority to KR10-2002-0069395A
    2004-05-17|Publication of KR20040041233A
    2005-05-03|Application granted
    2005-05-03|Publication of KR100485989B1
    优先权:
    申请号 | 申请日 | 专利标题
    KR10-2002-0069395A|KR100485989B1|2002-11-09|2002-11-09|Glassy carbon electrode system|
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