CN102445488A - Multiparameter water quality heavy metal automatic online monitor based on anodic stripping voltammetry - Google Patents
Multiparameter water quality heavy metal automatic online monitor based on anodic stripping voltammetry Download PDFInfo
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- CN102445488A CN102445488A CN2011102789456A CN201110278945A CN102445488A CN 102445488 A CN102445488 A CN 102445488A CN 2011102789456 A CN2011102789456 A CN 2011102789456A CN 201110278945 A CN201110278945 A CN 201110278945A CN 102445488 A CN102445488 A CN 102445488A
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Abstract
The invention relates to a multiparameter water quality heavy metal automatic online monitor based on the anodic stripping voltammetry. The monitor is characterized in that: the monitor comprises an electrochemical detection device, a control system, and a liquid charging device, a reaction device and a liquid discharging device which are respectively connected with the control system; the liquid charging device and the liquid discharging device, which jointly comprise peristaltic pumps, a precise syringe pump and six connection solenoid valves, are connected with the reaction device through pipelines to send a solution to the reaction device or discharge the solution from the reaction device; and the reaction device which is formed by inserted electrodes and an electrolytic cell with a stir bar provided therein is connected with the electrochemical detection device and can timely obtain effective data. By adopting the anodic stripping voltammetry in the invention, the simultaneous determination of multiple parameters can be realized, the reagent consumption is less, the apparatus is simple, the determination lower limit can be reduced by 2-3 orders of magnitude, and the chroma and the turbidity have no influences on the monitor, so the monitor can be used for the analysis of surface water and purified water.
Description
Technical field
The present invention relates to a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument, be applicable to the environmental water quality monitoring field based on anodic stripping voltammetry.
Background technology
In recent years, the heavy metal pollution incident takes place frequently, and since two thousand nine China has recurred more than 30 particularly serious heavy metal pollution incident.In the face of heavy metal pollution situation occurred frequently, Chinese Government will administer heavy metal pollution and formally bring into schedule.The overall goal and the policy direction of heavy metal pollution control during the clear and definite China " 12 " of " 12 " planning.The minister of Chinese Ministry of Environmental Protection Zhou Shengxian once mentioned when accepting " Chinese environmental newspaper " interview; The target of " 12 " heavy metal pollution control is to invest 75,000,000,000 yuan through state plan in the five-year, sets up fairly perfect heavy metal pollution and prevents and treats system, accident emergency system and environment and health risk assessment system.Heavy metal pollution detection and monitoring system play the vital role of assessment and early warning as the important component part of this system, and country also can increase input aspect coherent detection and the monitoring instrument naturally.Thereby heavy metal pollution detection of China and monitoring instrument are estimated and can rapidly be increased in recent years.
At present, China domestic producer or minority that can autonomous production heavy metal automatic on-line monitoring instrument can have the few of real mature technology.Existing homemade heavy metal automatic on-line monitoring instrument adopts AAS mostly, and this method cost is low, and belongs to the chemical analysis method of comparative maturity; Be easy to comparatively speaking realize that still, this method reagent consumption is big; Can not eliminate the influence of colourity and turbidity, can not realize monitoring simultaneously multiparameter, and the mensuration lower limit can not meet the demands sometimes; If, can reduce the detection lower limit, but complex operation with other concentration and separation technology couplings.Yet, adopt anodic stripping voltammetry just can overcome the above problems, this method adopts three-electrode system; Install easy; Reagent dosage is few, and it is low to measure lower limit, and colourity and turbidity are noiseless; Can monitor multiple parameter simultaneously, can be described as the method that relatively has superiority that a kind of water quality heavy metal detects.But anodic stripping voltammetry really will be used for the on-line monitoring of water quality heavy metal, also faces some new problems, and for example measurement range is narrow, the electrode poor reproducibility, and feed liquor precision, electrolytic cell structure etc. requires high.
Summary of the invention
For addressing the above problem, the present invention provides a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry.
Technical scheme of the present invention is: a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry; It comprises electrochemical detection device, control system and the feeding device that links to each other with control system respectively, reaction unit and pumping equipment; Said feed liquor, pumping equipment comprise peristaltic pump, precise injection pump and six solenoid valves; Link to each other with reaction unit through pipeline; And solution sent into or discharges reaction unit, and said reaction unit is made up of the electrolytic cell that inserts electrode and built-in stirrer, and it links to each other with electrochemical detection device and also can in time obtain valid data.
Preferably: described control system adopts embedded integrated industrial PC as main control unit; Control user interaction unit, data transmission unit, pump valve advance drainage system control module and electrochemical detection device, and responsible user interactions, regularly measurement, control pump valve advance discharge opeing and electrochemical detection device work, data processing and upload; Adopt PLC to advance the drainage system control module as pump valve, be responsible for testing process advance discharge opeing, pipeline cleans; Adopt the control module of single-chip microcomputer, be responsible for anodic stripping voltammetry analysis, and send the result main control unit of monitor to water sample as electrochemical detection device.
Preferably: said reaction unit is one and inserts three electrode electrolytic cell, is the right cylinder stirring pool, and the electrolytic cell side is respectively equipped with three electrode mounting holes, inlet opening, outage and air hole; The built-in stirrer of electrolytic cell cooperates with the motor of the electrolytic cell back side with strong magnets, to realize the stirring of solution.
Preferably: described electrolytic cell is that a volumes is the right cylinder stirring pool of 30mL, and the front panel of electrolytic cell can be opened, and seals through silica gel sealing ring between front panel and the integral body.
Preferably: said feed liquor system divides two-way to carry out, and one the tunnel for measuring the sample introduction of agents useful for same, combines to realize that another road is the sample introduction of standard solution with a peristaltic pump through one six solenoid valve, realizes through a high-precision syringe pump; Said drainage system is realized through a peristaltic pump.
Beneficial effect of the present invention is: the present invention is based on anodic stripping voltammetry; The ultimate principle of this method is to treat under negative current potential that earlier measured ion reduces with enrichment to working electrode; CONTROLLED POTENTIAL makes ionic oxide formation stripping to be measured to positive scanning direction then, thereby obtains a stripping peak; Its spike potential and peak size are respectively by element kind and concentration of element decision, thus the realization qualitative and quantitative analysis.Therefore; This method itself has the incomparable advantage of additive method; For example owing to passed through enrichment in advance so to measure lower limit low, utilize out the spike potential difference can carry out multiparameter mensuration etc. simultaneously, the present invention measures when utilizing this advantage to realize in the water quality various heavy element just.
Feed liquor of the present invention system divides two-way to carry out; One the tunnel for measuring the sample introduction of agents useful for same, combines to realize that another road is the sample introduction of standard solution with a peristaltic pump through one six solenoid valve; Realize through a high-precision syringe pump, this syringe pump accurately sample introduction to 0.5uL.The drainage system of instrument is realized through a peristaltic pump.
Electrolytic cell of the present invention is the right cylinder stirring pool of a volumes 30mL.The side is respectively equipped with three electrode mounting holes, inlet opening, outage and air hole.The front panel of electrolytic cell can be opened, and is convenient to carry out the I&M of electrode, seals through silica gel sealing ring between front panel and the integral body.The built-in stirrer of electrolytic cell cooperates with the motor of the electrolytic cell back side with strong magnets, to realize the stirring of solution.
Integral body control of the present invention adopts embedded integrated industrial PC as main control unit, and responsible user interactions, regularly measurement, control pump valve advance drainage system and electrochemical analyser work, data processing and upload; The PLC that adopts Siemens Company advances the control module of drainage system as pump valve, be responsible for testing process advance discharge opeing, pipeline cleans; Adopt the control module of the MSP430 series monolithic of TI company, be responsible for anodic stripping voltammetry analysis, and send the result main control unit of monitor to water sample as electrochemical analyser.
The present invention can reach 0-5mg/L to the sensing range of heavy metal, and has multistage measurement range selection.Monitor in use can be specified range, perhaps uses the automatic switching range function.When selecting the automatic switching range function; Monitor can be according to the content of beary metal in the water sample; Through changing the ratio of water sample and end liquid, change the enrichment time in the anode process in leaching, the modes such as gear that change the electrochemical monitoring appearance realize the automatic switchover of range.
The reappearance of electrode of the present invention is mainly improved through cleaning process.Cleaning process comprises that feed liquor cleans automatically and galvanochemistry is cleaned two kinds; It mainly is to carry out whole pipeline with distilled water to clean that feed liquor cleans; It mainly is that three-electrode system is carried out constant potential scanning that galvanochemistry is cleaned, and between positive negative potential, switches, to realize the cleaning of working electrode surface.
At present, most of producers adopt AAS to realize the monitoring of heavy metal automatic on-line, compare with it; The present invention adopts anodic stripping voltammetry, can realize that multiparameter measures simultaneously, and reagent consumption is few; Install easy; Measure lower limit and can reduce by 2～3 one magnitude, and do not receive the influence of colourity and turbidity, can be used for the analysis of surface water and pure water.
Description of drawings
Fig. 1 provides a kind of one-piece construction synoptic diagram of the multi-parameter water quality heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry for the present invention.
Fig. 2 provides a kind of pipeline connecting figure of the multi-parameter water quality heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry for the present invention.
Fig. 3 provides a kind of system construction drawing of the multi-parameter water quality heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry for the present invention.
The experiment image that Fig. 4 provides a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry to be used for the embodiment gained for the present invention.
Embodiment
Below in conjunction with description of drawings embodiment of the present invention:
The present invention mainly is applicable to the automatic on-line monitoring of water quality heavy metal ion such as industrial waste water, sanitary sewage, surface water, potable water, below is that instance describes with unitary determination with automatic on-line monitoring continuously respectively.
Embodiment 1: monitoring in the time of copper in the industrial waste water, cadmium, plumbous three kinds of elements
Get the waste water of certain chemical cell manufacturer, through after the suitable pre-service, stored for future use.
As shown in Figure 1, the present invention mainly is made up of the conjuncted solenoid valve of display screen 1, electrolytic cell 2, precise injection pump 3, six 4, feed liquor peristaltic pump 5, discharge opeing peristaltic pump 6 and reagent box 7.
During the test beginning, with the distilled water suction line, carry out whole pipeline and clean, will pass through pretreated water sample suction line then, carry out the pipeline rinse by feed liquor peristaltic pump 5.In electrolytic cell 2, suck the 20mL water sample afterwards, and will test agents useful for same coating liquid, electrolyte suction electrolytic cell in proportion respectively, begin to adopt anodic stripping voltammetry to carry out electro-chemical test then; After treating that electro-chemical test is accomplished, waste liquid is through 6 emptyings of discharge opeing peristaltic pump, and then through feed liquor peristaltic pump 5 suction pure water and electrolyte; Carry out galvanochemistry and clean, suck pure water afterwards again, carry out whole pipeline and clean; The emptying waste liquid, whole mensuration process is accomplished, thereby obtains testing spectrogram; Find out the peak position and the peak size of every heavy metal species through built-in imgae processing software,, draw heavy metal concentration through contrasting with built-in typical curve.Experiment image (like Fig. 4) and final concentration value are shown on the display screen 1.
Embodiment 2: the continuous automatic on-line monitoring of cadmium element in the industrial waste water
Choosing certain Electroplate Factory is experimental point; After the installation, configure all location parameters, calibrate with standard solution then; Two good span calibration liquid carry out instance one described test to adopt configured in advance respectively; Record peak position and peak size are made a typical curve with the relation of peak height and concentration, with the parameter of curve input instrument of gained.Calibration has customized measuring period (every day 12 times) after accomplishing, and moves one month automatically.Experimental data can all be stored in the instrument, and all data of analysis-by-synthesis can find out that the present invention can satisfy the requirement of continuous automatic on-line monitoring.
The above be merely part embodiment of the present invention, but the present invention is not as limit; The present invention changes corresponding changes such as working electrode through making to change test agent, can measure nearly more than 30 kind of element; And, can measure more element along with the progress of assay method.
Claims (5)
1. multi-parameter water quality heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry; It is characterized in that: it comprises electrochemical detection device, control system and the feeding device that links to each other with control system respectively, reaction unit and pumping equipment; Said feed liquor, pumping equipment comprise peristaltic pump, precise injection pump and six solenoid valves; Link to each other with reaction unit through pipeline; And solution sent into or discharges reaction unit, and said reaction unit is made up of the electrolytic cell that inserts electrode and built-in stirrer, and it links to each other with electrochemical detection device and also can in time obtain valid data.
2. a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument according to claim 1 based on anodic stripping voltammetry; It is characterized in that: described control system adopts embedded integrated industrial PC as main control unit; Control user interaction unit, data transmission unit, pump valve advance drainage system control module and electrochemical detection device, and responsible user interactions, regularly measurement, control pump valve advance discharge opeing and electrochemical detection device work, data processing and upload; Adopt PLC to advance the drainage system control module as pump valve, be responsible for testing process advance discharge opeing, pipeline cleans; Adopt the control module of single-chip microcomputer, be responsible for anodic stripping voltammetry analysis, and send the result main control unit of monitor to water sample as electrochemical detection device.
3. a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument according to claim 1 based on anodic stripping voltammetry; It is characterized in that: said reaction unit is one and inserts three electrode electrolytic cell; Be the right cylinder stirring pool, the electrolytic cell side is respectively equipped with three electrode mounting holes, inlet opening, outage and air hole; The built-in stirrer of electrolytic cell cooperates with the motor of the electrolytic cell back side with strong magnets, to realize the stirring of solution.
4. a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument according to claim 3 based on anodic stripping voltammetry; It is characterized in that: described electrolytic cell is that a volumes is the right cylinder stirring pool of 30mL; The front panel of electrolytic cell can be opened, and seals through silica gel sealing ring between front panel and the integral body.
5. a kind of multi-parameter water quality heavy metal automatic on-line monitoring instrument according to claim 1 based on anodic stripping voltammetry; It is characterized in that: said feed liquor system divides two-way to carry out; One the tunnel for measuring the sample introduction of agents useful for same; Combine to realize that through one six solenoid valve another road is the sample introduction of standard solution with a peristaltic pump, realize through a high-precision syringe pump; Said drainage system is realized through a peristaltic pump.
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Cited By (16)
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| CN102608191A (en) * | 2011-12-08 | 2012-07-25 | 青岛佳明测控仪器有限公司 | Electrochemistry on-line cleaning method for heavy metal on-line monitor working electrode |
| CN102998358A (en) * | 2012-12-28 | 2013-03-27 | 江苏德林环保技术有限公司 | Method and device for sequentially injecting lead in online detection of water quality |
| CN103076381A (en) * | 2012-12-31 | 2013-05-01 | 苏州汶颢芯片科技有限公司 | Anodic stripping voltammetric mechanism-based online automatic monitoring system for heavy metal ions in water |
| CN103344692A (en) * | 2013-06-27 | 2013-10-09 | 安徽大地熊新材料股份有限公司 | Method for detecting heavy metal ions in sewage |
| CN103364461A (en) * | 2013-04-22 | 2013-10-23 | 江苏天瑞仪器股份有限公司 | Online water heavy metal analyzer |
| CN103913490A (en) * | 2012-12-28 | 2014-07-09 | 株式会社堀场制作所 | Electrochemistry Analysis Method, Electrochemistry Analysis Device And Test Kit |
| CN104034760A (en) * | 2013-03-04 | 2014-09-10 | 上海宝钢工业技术服务有限公司 | Multifunctional tin plate surface characteristic testing device and use method thereof |
| CN105891294A (en) * | 2016-06-23 | 2016-08-24 | 中国科学院长春应用化学研究所 | Method for detecting heavy metal ions by electrochemical analysis |
| CN107356651A (en) * | 2017-08-28 | 2017-11-17 | 广州商辉怡业计算机科技有限公司 | Multi parameter water quality method and system |
| CN107655957A (en) * | 2017-09-20 | 2018-02-02 | 中冶华天南京工程技术有限公司 | A kind of device applied to villages and small towns river course heavy metal pollution on-line monitoring |
| CN107991365A (en) * | 2017-11-27 | 2018-05-04 | 宇星科技发展(深圳)有限公司 | A kind of on-line cleaning method for the heavy metal on-line computing model working electrode based on anodic stripping voltammetry |
| US9970899B2 (en) | 2016-07-15 | 2018-05-15 | Ketos, Inc. | Automated smart water quality monitor and analyzer and associated methods |
| CN109632888A (en) * | 2018-12-27 | 2019-04-16 | 广州安食通信息科技有限公司 | A kind of food heavy metal detector and food heavy metal detection method |
| CN110186989A (en) * | 2019-05-31 | 2019-08-30 | 中兴仪器（深圳）有限公司 | A kind of water quality heavy metal online analyzer |
| CN110208354A (en) * | 2019-04-02 | 2019-09-06 | 深圳市智创环保科技有限公司 | A kind of portable water quality in-line analyzer |
| CN112630277A (en) * | 2020-08-28 | 2021-04-09 | 广东工业大学 | Real-time solution detection equipment and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102608191A (en) * | 2011-12-08 | 2012-07-25 | 青岛佳明测控仪器有限公司 | Electrochemistry on-line cleaning method for heavy metal on-line monitor working electrode |
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| CN102998358A (en) * | 2012-12-28 | 2013-03-27 | 江苏德林环保技术有限公司 | Method and device for sequentially injecting lead in online detection of water quality |
| CN103913490B (en) * | 2012-12-28 | 2018-10-16 | 株式会社堀场制作所 | Electrochemical analysis method, electrochemical analysis device and reagent set |
| CN102998358B (en) * | 2012-12-28 | 2014-06-25 | 江苏德林环保技术有限公司 | Method and device for sequentially injecting lead in online detection of water quality |
| CN103913490A (en) * | 2012-12-28 | 2014-07-09 | 株式会社堀场制作所 | Electrochemistry Analysis Method, Electrochemistry Analysis Device And Test Kit |
| CN103076381A (en) * | 2012-12-31 | 2013-05-01 | 苏州汶颢芯片科技有限公司 | Anodic stripping voltammetric mechanism-based online automatic monitoring system for heavy metal ions in water |
| CN104034760A (en) * | 2013-03-04 | 2014-09-10 | 上海宝钢工业技术服务有限公司 | Multifunctional tin plate surface characteristic testing device and use method thereof |
| CN103364461A (en) * | 2013-04-22 | 2013-10-23 | 江苏天瑞仪器股份有限公司 | Online water heavy metal analyzer |
| CN103344692A (en) * | 2013-06-27 | 2013-10-09 | 安徽大地熊新材料股份有限公司 | Method for detecting heavy metal ions in sewage |
| CN105891294A (en) * | 2016-06-23 | 2016-08-24 | 中国科学院长春应用化学研究所 | Method for detecting heavy metal ions by electrochemical analysis |
| CN105891294B (en) * | 2016-06-23 | 2019-07-23 | 中国科学院长春应用化学研究所 | A kind of method of Applied Electrochemistry analytic approach detection heavy metal ion |
| US10436749B2 (en) | 2016-07-15 | 2019-10-08 | Ketos Inc. | Automated smart water quality monitor and analyzer and associated methods |
| US9970899B2 (en) | 2016-07-15 | 2018-05-15 | Ketos, Inc. | Automated smart water quality monitor and analyzer and associated methods |
| CN107356651A (en) * | 2017-08-28 | 2017-11-17 | 广州商辉怡业计算机科技有限公司 | Multi parameter water quality method and system |
| CN107655957B (en) * | 2017-09-20 | 2019-07-05 | 中冶华天南京工程技术有限公司 | A kind of device applied to villages and small towns river heavy metal pollution on-line monitoring |
| CN107655957A (en) * | 2017-09-20 | 2018-02-02 | 中冶华天南京工程技术有限公司 | A kind of device applied to villages and small towns river course heavy metal pollution on-line monitoring |
| CN107991365A (en) * | 2017-11-27 | 2018-05-04 | 宇星科技发展(深圳)有限公司 | A kind of on-line cleaning method for the heavy metal on-line computing model working electrode based on anodic stripping voltammetry |
| CN109632888A (en) * | 2018-12-27 | 2019-04-16 | 广州安食通信息科技有限公司 | A kind of food heavy metal detector and food heavy metal detection method |
| CN110208354A (en) * | 2019-04-02 | 2019-09-06 | 深圳市智创环保科技有限公司 | A kind of portable water quality in-line analyzer |
| CN110186989A (en) * | 2019-05-31 | 2019-08-30 | 中兴仪器（深圳）有限公司 | A kind of water quality heavy metal online analyzer |
| CN112630277A (en) * | 2020-08-28 | 2021-04-09 | 广东工业大学 | Real-time solution detection equipment and method |
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Application publication date: 20120509 |