CN101644693A - BDD electrode-based COD rapid determination device - Google Patents
BDD electrode-based COD rapid determination device Download PDFInfo
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- CN101644693A CN101644693A CN200910189911A CN200910189911A CN101644693A CN 101644693 A CN101644693 A CN 101644693A CN 200910189911 A CN200910189911 A CN 200910189911A CN 200910189911 A CN200910189911 A CN 200910189911A CN 101644693 A CN101644693 A CN 101644693A
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Abstract
The invention discloses a BDD electrode-based rapid COD measuring device which comprises an electrochemical analysis unit, wherein the electrochemical analysis unit comprises an electrolytic cell provided with a working electrode, a reference electrode and a counter electrode, and the working electrode is a BDD electrode. The electrochemical analysis unit also comprises a fixed support rod and a supporting plate connected with the fixed support rod, the electrolytic cell is arranged on the supporting plate, and the upper end of the electrolytic cell is provided with an electrolytic cell cover connected with the fixed support rod; the supporting plate is provided with a magnetic stirrer, and the bottom of the electrolytic cell is provided with a magnetic bar; the side wall of the lower part of the electrolytic cell is provided with a liquid carrying port, and the other side wall of the lower part of the electrolytic cell is provided with a vent. The device is easy to operate, short in time consumption and rapid in signal response; no toxic substance is discharged during and after the test, and the problem of secondary pollution is avoided; the BDD electrode can completely oxidize organic pollutants in water; the mechanical strength is high, pollution resistance and corrosion resistance are realized, and the material is environment-friendly; can realize the rapid, automatic and continuous operation of COD determination.
Description
Technical field
The present invention relates to a kind of COD pick-up unit, more particularly refer to COD fast measuring device based on the BDD electrode.
Background technology
COD, i.e. chemical oxygen demand (COD) is an important indicator of weighing the water body organic contamination, also is that China the Eleventh Five-Year Plan period requires one of leading indicator that total amount reduces discharging.The standard method that the COD of country measures is the potassium dichromate circumfluence method.It is accurate that potassium dichromate method has measurement result, high repeatability and other advantages, but its shortcoming is a method complexity, consuming time, the medicine consumption is big, and uses poisonous chromium, mercury reagent, causes secondary pollution etc.
At the deficiency of classic method, in the face of the needs in market, many advanced technologies constantly are incorporated in the COD detection system, make the COD detection method develop to automatic, intelligence, online direction.For example, ultrasonic auxiliary resolution method, spectrophotometric method is singly swept polarography, photocatalytic oxidation and galvanochemistry ampere method or the like.Up to the appearance of electrochemical method, allow people see the dawn that fundamentally improves all shortcomings of classic method.Electrochemical method does not need costliness, toxic reagent; Method of testing is easy, quick; Be easy to combine with the flow injection technology, thus the automaticity of raising assay method.But electrochemical method also has weak point, for example to containing solid-state or measured deviation may appear in colloid organic wastewater.And the main problem that exists at present is also untapped a kind of suitable electrode material that goes out.In research in the past, used electrode material, the electrochemical oxidation ability that has is not high, the not enough environmental protection of the material that has itself.Therefore, electrochemical method is that present COD measures one of primary study direction in the research, is the key issue of being badly in need of solution and excavate suitable electrode material.
Selection of electrode materials is most important.Electrode is as the core original paper that detects, and its oxidability and stability are directly connected to the quality of measurement effect.
The representative electrode that is used for electrochemical process survey COD on the existing market is compared as follows:
1.AgO/CuO check the shortcoming of electrode: oxidability is not high;
2.PbO2 the shortcoming of electrode: the erosion of not anti-chlorine, have the risk of heavy metal ion stripping to the ferric ion sensitivity, in acidity or alkaline medium, the Interference Detection signal also causes secondary pollution to environment.
The inventor develops a kind of new fast measuring device based on the defective of above-mentioned prior art.
Summary of the invention
The objective of the invention is to provides for overcoming the deficiencies in the prior art that a kind of detection is more accurate, detection time is shorter, the more stable free of contamination again COD determinator of performance.It is working electrode that this device adopts the BDD electrode, and the BDD electrode is a kind of eco-friendly electrode material, and BDD (boron-doped diamond) electrode has that electrochemical window is wide, background current is low, good stability, characteristics that resistance to corrosion is strong.The deviation of contrast national standard method is in 5%, and only be 2-3 minute detection time, and is accurately stable fast, environmental protection.
The technology of the present invention content is: based on the COD fast measuring device of BDD electrode, it comprises the electrochemical analysis unit, and described electrochemical analysis unit comprises and is provided with working electrode, contrast electrode and to the electrolytic cell of electrode, described working electrode is the BDD electrode.
Further technology contents of the present invention is: described electrochemical analysis unit also comprises fixing pole and the supporting plate that connects with fixing pole, and described electrolytic cell is located on the supporting plate, and the electrolytic cell upper end is provided with the electrolytic cell that connects with fixing pole and covers; Described supporting plate is provided with magnetic stirring apparatus, and described electrolytic cell bottom is provided with magnetic bar; The lower sides of electrolytic cell is provided with the carrier fluid mouth, and another sidewall of bottom is provided with drain; Described electrolytic cell covers and is equipped with aforesaid working electrode, contrast electrode and to electrode.
Further technology contents of the present invention is: also comprise data acquisition unit and control module, the carrier fluid mouth of described electrochemical analysis unit is connected with sampling pipe and purge pipe; Described sampling pipe is provided with sampling pump, and described purge pipe is provided with scavenging pump; Described data acquisition unit comprises data acquisition processing circuit, and described control module comprises controller, and described data acquisition processing circuit is provided with working electrode, contrast electrode with to the test side that electrode connects, and is provided with the communication terminal that connects with controller; Described controller is provided with the control end that connects with sampling pump, scavenging pump.
Further technology contents of the present invention is: described sampling pipe comprises sample liquid pipe and supporting electrolyte pipe; Described sample liquid pipe is provided with the sample liquid valve, and described supporting electrolyte pipe is provided with the supporting electrolyte valve, and described sample liquid valve, supporting electrolyte valve all connect with the control end of controller.
Further technology contents of the present invention is: described purge pipe comprises cleaning fluid pipe and supporting electrolyte pipe; Described scavenging pump comprises cleaning liquid pump and supporting electrolyte pump.
Further technology contents of the present invention is: the described carrier fluid mouth outside also is provided with the heater block that connects with controller, and described purge pipe, sampling pipe pass heater block and connect with the carrier fluid mouth.
Further technology contents of the present invention is: described electrolytic cell upper portion side wall is provided with overflow vent; Described electrolytic cell is the vertebral body shape; Described working electrode, contrast electrode and electrode is arranged in is fixed in the rubber band that electrolytic cell covers; Described electrolytic cell covers and also is provided with pore; Described BDD electrode is to be the membrane electrode of substrate with the titanium sheet.
The present invention compared with prior art has the following advantages:
1. apparatus of the present invention operation is simple and easy, weak point consuming time, and signal response is rapid;
2. do not have the noxious material discharging in the test process and after finishing, do not produce the secondary pollution problem;
3.BDD the hydroxyl radical free radical that electrode surface produces is the strong oxidizer of a kind of high redox potential (2.8V), its oxidation-reduction potential is considerably beyond ozone (2.1V) and dichromate ion (1.4V), can complete oxidation water in organic contaminant;
4.BDD membrane electrode is substrate with the titanium sheet, the physical strength height, and antipollution, anticorrosive, environment-friendly material;
5. realized that COD measures automatically, operation continuously, promoted environmental protection, original position better, in the development of line style COD test macro.
The beneficial effect of apparatus of the present invention with promoting people's green environment monitoring theory, can further promote the understanding of people to environmental protection, promotes the development of environmental protection cause.
Below in conjunction with the drawings and specific embodiments the present invention is further described.
Description of drawings
Fig. 1 is the COD fast measuring device specific embodiment structural drawing that the present invention is based on the BDD electrode.
Description of reference numerals
A electrochemical analysis unit B data acquisition unit
The C control module
1 fixing pole 11 nuts
12 nuts, 13 nuts
14 nuts
2 supporting plates, 3 magnetic stirring apparatuss
31 magnetic bars, 4 electrolytic cells
41A carrier fluid mouth A 41B carrier fluid mouth B
42 drains, 43 overflow vents
44 electrolytic solution, 5 electrolytic cells lid
51 pores, 6 rubber bands
61 working electrodes, 62 contrast electrodes
63 pairs of electrode 7 atmospheric valves
8 controllers, 80 heater blocks
81 sampling pipes, 82 purge pipes
810 sampling pumps, 811 supporting electrolyte valves
812 supporting electrolyte valves, 813 sample liquid valves
814 sample liquid pipes 815 are demarcated liquid valve
816 demarcate liquid line 821 cleaning liquid pumps
823 supporting electrolyte pumps, 822 cleaning fluid pipes
824 supporting electrolyte pipes
Embodiment
In order to more fully understand technology contents of the present invention, technical scheme of the present invention is further introduced and explanation below in conjunction with specific embodiment.
As shown in Figure 1, COD fast measuring device based on the BDD electrode, it comprises electrochemical analysis unit A, and electrochemical analysis unit A comprises and is provided with working electrode 61, contrast electrode 62 and to the electrolytic cell 4 (what adopt in the present embodiment is glassware) of electrode 63, working electrode 61 is the BDD electrode.The electrolytic cell lid 5 (what adopt in the present embodiment is plastic products) that electrochemical analysis unit A also comprises fixing pole 1, the supporting plate 2 that connects with fixing pole 1, is located at the electrolytic cell 4 on the supporting plate 2 and is located at electrolytic cell 4 upper ends and connects with fixing pole 1; Supporting plate 2 is provided with magnetic stirring apparatus 3, and magnetic stirring apparatus 3 is by the control system control of outside.Electrolytic cell 4 bottoms are provided with magnetic bar 30; The outside, bottom of electrolytic cell 4 is provided with the carrier fluid mouth, is provided with two at this implementation Shi Lizhong, carrier fluid mouth 41A and carrier fluid mouth 41B; Be equipped with working electrode 61, contrast electrode 62 on the electrolytic cell lid 5 and 63, three electrodes of electrode are connected with the observation circuit of outside respectively, export the testing result of COD.Fixedly pole 1 is a lead screw, and electrolytic cell lid 5 is the basket type structure, by nut 13 and 14 and fixing pole 1 adjustable thread connection.Supporting plate 2 by nut 11 and 12 and fixedly pole 1 be fixedly connected, regulate the height of electrolytic cell with this.Another outside, the bottom of electrolytic cell 4 is provided with drain 42, and upper outside is provided with overflow vent 43.Electrolytic cell 4 is the vertebral body shape, helps stirring fully and is beneficial to emptying, and not residual sample liquid is in order to avoid disturb next measurement result.Electrolytic cell Height Adjustable, the electrolytic cell lid adopts basket type, can be free movable.Working electrode 61, contrast electrode 62 and electrode 63 is arranged in is fixed in the rubber band 61 that electrolytic cell covers; Also be provided with pore 51 on the electrolytic cell lid 5.BDD electrode 61 is to be the membrane electrode of substrate with the titanium sheet.Drain 42 also is connected with atmospheric valve 7, and atmospheric valve 7 can adopt manual mode, also can adopt the electronic mode that connects with controller 8, and the latter can connect automatic emptying, atmospheric valve 7 preferred motorized valve structures.
Also comprise data acquisition unit B and control module C, the carrier fluid mouth 41A of electrochemical analysis unit A and 42B are connected with sampling pipe 81 and purge pipe 82 respectively; Sampling pipe 81 is provided with sampling pump 810, and purge pipe 82 is provided with scavenging pump (comprising cleaning liquid pump 821 and supporting electrolyte pump 823); Data acquisition unit B comprises data acquisition processing circuit 9, and control module C comprises controller 8, and data acquisition processing circuit 9 is provided with and working electrode 61, contrast electrode 62 and test side that electrode 63 is connected, is provided with the communication terminal that connects with controller 8; Controller 8 is provided with the control end that connects with sampling pump 810, cleaning liquid pump 821 and supporting electrolyte pump 823.Outside controller 8 decapacitation realize that the switching value/analog quantity to each pump and valve is controlled, also accept the detection information of data acquisition processing circuit, controller also can be provided with the PORT COM that connects with host computer simultaneously, make the online testing of COD in central control room, send the detection control signal by host computer, and reception testing result, carry out data and gather, print, or make the functions such as examining report book of electronics shelves.
The present invention adopts the COD in the BDD determination of electrode water, measure in the process of COD at the BDD membrane electrode, indirect oxidation reaction by the hydroxyl radical free radical mediation is the committed step that COD measures process, the hydroxyl radical free radical that produces has very high oxidizing potential (about 2.8V), almost non-selectivity ground, various organism of oxidation apace, make the organism permineralization, generate CO
2And H
2O, reaction principle suc as formula 1 with formula 2.And with PbO
2Be metal oxide electrode " activity " electrode normally of representative, organic oxidation is closely related with the electrode composition, organic oxidation is had selectivity, so the BDD membrane electrode helps the detection of COD more.
M+H
2O→M(·OH)+H++e- (1)
M(·OH)+R→M+CO
2+H
2O+H++e- (2)
M representative " electrode surface attachment " in the formula, R represents " organism "
Utilize electrochemical analyser (electrochemical analysis unit) that constant potential is provided and marking current is gathered, in three electrode electrochemical cell (electrolytic cell), carry out, being working electrode with the BDD membrane electrode respectively, is to electrode with platinized platinum, is contrast electrode with the Ag/AgCl electrode.
Generally prepared BDD membrane electrode electrochemical potential window is all greater than 3.2V, in present technique when as long as its anode potential is higher than 2.2V, can think that electrode quality is good.This wide electromotive force window has guaranteed that it can measure accurately to COD in the water.
Apparatus of the present invention are controlled each operating process by controller (as adopting PLC or utilizing the nonshared control unit of microcontroller exploitation such as single-chip microcomputer), elder generation's inspection apparatus operate as normal whether during measurement, and wash each pipeline and detection cell (being electrolytic cell) with corresponding liquid, rinse detection cell then, last sample introduction is measured, whole process stirs always, and adopts the Na of 0.1mol/L
2SO
4Solution is as supporting electrolyte, 2.2-3.5V under suitable constant potential, and the anodic oxidation organism detects the current signal that is generated simultaneously, and as measurement standard, organic concentration is high more, and the current value of response is big more.Measure voltage that finishes after-applied 3.0V and the Na that uses 0.5mol/L
2SO
4The solution regeneration electrode.In testing process, used supporting electrolyte, also can come the concentration of dilute sample (sample liquid) by the adding deionized water, reduce the concentration of COD, thereby make the scope of the concentration of testing sample (sample liquid) at typical curve, so sample liquid that when detecting, is written into, supporting electrolyte, the ratio of deionized water is passed through sample liquid by controller, supporting electrolyte, the flow of the valve of deionized water or pump (valve or pump with analog quantity control function) draws, in carrying out the data acquisition process process, in this ratio reduction, calculate the COD value of sample liquid by the COD value of mixing material in the electrolytic cell.It below is the case study on implementation of three detections.
Example 1:
Measure pollutant common in certain wastewater from chemical industry and the pharmacy waste water, as phenol, p-nitrophenol, salicylic acid and cysteamine.Employing Ag/AgCl is a contrast electrode, apply voltage 3.2V, add standard model (0mg/l, 500mg/l, 1000mg/l) respectively, automatically calibrate, draw calibration curve, automatically measure then, gather live signal by data acquisition processing circuit, the COD value that can directly read this reagent water sample is 1652.1mg/L.
Example 2:
Measure certain sanitary sewage.Employing Ag/AgCl is a contrast electrode, apply voltage 2.5V, add standard model (0mg/l, 500mg/l, 1000mg/l) respectively, automatically calibrate, draw calibration curve, automatically measure then, gather live signal by data acquisition processing circuit, the COD value that can directly read this reagent water sample is 39.8mg/L.
Example 3:
Measure certain food additives waste water, the main containing alcohol-based cyclopentanone of this waste water, organism such as acetic acid and diacetyl, employing Ag/AgCl is a contrast electrode, applies voltage 2.4V, add standard model (0mg/l, 500mg/l, 1000mg/l) respectively, automatically calibrate, draw calibration curve, measure automatically then, gather live signal by data acquisition processing circuit, the COD value that can directly read this reagent water sample is 2498.6mg/L.
In sum, the present invention compared with prior art has the following advantages: 1. apparatus of the present invention operation is simple and easy, weak point consuming time, and signal response is rapid; 2. do not have the noxious material discharging in the test process and after finishing, do not produce the secondary pollution problem; 3.BDD the hydroxyl radical free radical that electrode surface produces is the strong oxidizer of a kind of high redox potential (2.8V), its oxidation-reduction potential is considerably beyond ozone (2.1V) and dichromate ion (1.4V), can complete oxidation water in organic contaminant; 4.BDD membrane electrode is substrate with the titanium sheet, the physical strength height, and antipollution, anticorrosive, environment-friendly material; 5. realized that COD measures automatically, operation continuously, promoted environmental protection, original position better, in the development of line style COD test macro.The beneficial effect of apparatus of the present invention with promoting people's green environment monitoring theory, can further promote the understanding of people to environmental protection, promotes the development of environmental protection cause.
The above only further specifies technology contents of the present invention with embodiment, so that the reader is more readily understood, but does not represent embodiments of the present invention to only limit to this, anyly extends or recreation according to the technology that the present invention did, and all is subjected to protection of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (7)
1. based on the COD fast measuring device of BDD electrode, it comprises the electrochemical analysis unit, it is characterized in that described electrochemical analysis unit comprises to be provided with working electrode, contrast electrode and to the electrolytic cell of electrode, described working electrode is the BDD electrode.
2. the COD fast measuring device based on the BDD electrode according to claim 1, it is characterized in that described electrochemical analysis unit also comprises fixing pole and the supporting plate that connects with fixing pole, described electrolytic cell is located on the supporting plate, and electrolytic cell upper end is provided with the electrolytic cell that connects with fixing pole and covers; Described supporting plate is provided with magnetic stirring apparatus, and described electrolytic cell bottom is provided with magnetic bar; The lower sides of electrolytic cell is provided with the carrier fluid mouth, and another sidewall of bottom is provided with drain; Described electrolytic cell covers and is equipped with aforesaid working electrode, contrast electrode and to electrode.
3. the COD fast measuring device based on the BDD electrode according to claim 2 is characterized in that also comprising data acquisition unit and control module, and the carrier fluid mouth of described electrochemical analysis unit is connected with sampling pipe and purge pipe; Described sampling pipe is provided with sampling pump, and described purge pipe is provided with scavenging pump; Described data acquisition unit comprises data acquisition processing circuit, and described control module comprises controller, and described data acquisition processing circuit is provided with working electrode, contrast electrode with to the test side that electrode connects, and is provided with the communication terminal that connects with controller; Described controller is provided with the control end that connects with sampling pump, scavenging pump.
4. the COD fast measuring device based on the BDD electrode according to claim 3 is characterized in that described sampling pipe comprises sample liquid pipe and supporting electrolyte pipe; Described sample liquid pipe is provided with the sample liquid valve, and described supporting electrolyte pipe is provided with the supporting electrolyte valve, and described sample liquid valve, supporting electrolyte valve all connect with the control end of controller.
5. the COD fast measuring device based on the BDD electrode according to claim 4, the described purge pipe of its feature comprises cleaning fluid pipe and supporting electrolyte pipe; Described scavenging pump comprises cleaning liquid pump and supporting electrolyte pump.
6. the COD fast measuring device based on the BDD electrode according to claim 5, the described carrier fluid mouth of its feature outside also is provided with the heater block that connects with controller, and described purge pipe, sampling pipe pass heater block and connect with the carrier fluid mouth.
7. the COD fast measuring device based on the BDD electrode according to claim 6 is characterized in that described electrolytic cell upper portion side wall is provided with overflow vent; Described electrolytic cell is the vertebral body shape; Described working electrode, contrast electrode and electrode is arranged in is fixed in the rubber band that electrolytic cell covers; Described electrolytic cell covers and also is provided with pore; Described BDD electrode is to be the membrane electrode of substrate with the titanium sheet.
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| CN102298067A (en) * | 2011-07-21 | 2011-12-28 | 杭州电子科技大学 | Full-automatic on-line monitoring system of COD (chemical oxygen demand) and monitoring method thereof |
| CN102680542A (en) * | 2012-05-17 | 2012-09-19 | 大连理工大学 | Fully-automatic portable flow injection chemical oxygen demand monitor based on BDD (Boron-Doped Diamond) membrane electrode |
| CN104614486A (en) * | 2013-11-05 | 2015-05-13 | 东亚Dkk株式会社 | Automatic apparatus for measuring chemical oxygen demand (cod) |
| CN105866365A (en) * | 2016-04-04 | 2016-08-17 | 方艳玲 | Split type synchronous water quality testing device for drinking water |
| CN105954337A (en) * | 2016-04-28 | 2016-09-21 | 中国人民武装警察部队学院 | Method for on-line cleaning and activation of boron-doped diamond thin-film electrode |
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| CN107449882A (en) * | 2017-07-24 | 2017-12-08 | 东华工程科技股份有限公司 | A kind of high-concentration sewage COD on-line monitoring systems |
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| CN110133071A (en) * | 2019-04-22 | 2019-08-16 | 湖北工业大学 | A kind of method that COD electrochemistry is quickly monitored on-line |
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| CN102298067A (en) * | 2011-07-21 | 2011-12-28 | 杭州电子科技大学 | Full-automatic on-line monitoring system of COD (chemical oxygen demand) and monitoring method thereof |
| CN102680542A (en) * | 2012-05-17 | 2012-09-19 | 大连理工大学 | Fully-automatic portable flow injection chemical oxygen demand monitor based on BDD (Boron-Doped Diamond) membrane electrode |
| CN102680542B (en) * | 2012-05-17 | 2014-05-21 | 大连理工大学 | Fully-automatic portable flow injection chemical oxygen demand monitor based on BDD (Boron-Doped Diamond) membrane electrode |
| CN104614486A (en) * | 2013-11-05 | 2015-05-13 | 东亚Dkk株式会社 | Automatic apparatus for measuring chemical oxygen demand (cod) |
| TWI651534B (en) * | 2013-11-05 | 2019-02-21 | 東亞Ｄｋｋ股份有限公司 | Chemical oxygen demand (COD) automatic measuring device |
| CN105866365A (en) * | 2016-04-04 | 2016-08-17 | 方艳玲 | Split type synchronous water quality testing device for drinking water |
| CN105954337A (en) * | 2016-04-28 | 2016-09-21 | 中国人民武装警察部队学院 | Method for on-line cleaning and activation of boron-doped diamond thin-film electrode |
| CN105954337B (en) * | 2016-04-28 | 2018-04-06 | 中国人民武装警察部队学院 | The method that on-line cleaning activates boron-doped diamond thin-film electrode |
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| CN107449882A (en) * | 2017-07-24 | 2017-12-08 | 东华工程科技股份有限公司 | A kind of high-concentration sewage COD on-line monitoring systems |
| CN110389164A (en) * | 2018-04-20 | 2019-10-29 | 北京先驱威锋技术开发公司 | Automatic flushing device for the measurement of solution electric signal |
| CN110389164B (en) * | 2018-04-20 | 2022-01-07 | 北京先驱威锋技术开发公司 | Automatic cleaning device for solution electric signal measurement |
| CN109900765A (en) * | 2019-04-10 | 2019-06-18 | 黑龙江大学 | A kind of electrochemical testing device that electrode surface mass transfer is controllable and method |
| CN109900765B (en) * | 2019-04-10 | 2021-07-20 | 黑龙江大学 | Electrochemical testing device and method with controllable mass transfer on electrode surface |
| CN110133071B (en) * | 2019-04-22 | 2021-09-17 | 湖北工业大学 | COD electrochemical rapid on-line monitoring method |
| CN110133071A (en) * | 2019-04-22 | 2019-08-16 | 湖北工业大学 | A kind of method that COD electrochemistry is quickly monitored on-line |
| CN111504863A (en) * | 2020-05-08 | 2020-08-07 | 农业农村部南京农业机械化研究所 | Droplet deposition amount measuring device and method based on metal ion concentration detection |
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| CN113252748A (en) * | 2021-05-31 | 2021-08-13 | 清池水环境治理科技发展(天津)有限公司 | Adopt integration electrode unit's portable COD rapid survey appearance |
| CN113358721A (en) * | 2021-05-31 | 2021-09-07 | 清池水环境治理科技发展(天津)有限公司 | Portable COD rapid determination appearance is with disposable integrated electrode unit |
| CN113358721B (en) * | 2021-05-31 | 2024-05-07 | 清池水环境治理科技发展(天津)有限公司 | Disposable integrated electrode unit for portable COD rapid determination instrument |
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