CN1645127A - COD electrochemical analyzers - Google Patents

COD electrochemical analyzers Download PDF

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Publication number
CN1645127A
CN1645127A CN 200510023445 CN200510023445A CN1645127A CN 1645127 A CN1645127 A CN 1645127A CN 200510023445 CN200510023445 CN 200510023445 CN 200510023445 A CN200510023445 A CN 200510023445A CN 1645127 A CN1645127 A CN 1645127A
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China
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electrode
upper cover
cover plate
cod
lower cover
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CN 200510023445
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Chinese (zh)
Inventor
金利通
李嘉庆
李洛平
郑蕾
张文
鲜跃仲
吴荣坤
庄荣华
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East China Normal University
Donghua University
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East China Normal University
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Priority to CN 200510023445 priority Critical patent/CN1645127A/en
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Abstract

An electrochemical analyser of chemical oxygen demand is composed of sample feeding system of flowing injection mode analysing and detecting device, as well as data processing system. The analysing and detecting device applies three electrodes electrochemical system including operation electrode, reference electrode, inlet and outlet tube, top cover, bottom cover, and teflon film setting between two covers and having a notch at middle to form detection cell.

Description

COD electrochemical analyzers
Technical field
The present invention relates to a kind of analytical instrument of fast detecting chemical oxygen demand of water body, especially a kind of pick-up unit that adopts galvanochemistry Amperometric Detection Coupled technology fast measuring chemical oxygen demand of water body belongs to analytical chemistry and sensor technical field.
Background technology
Chemical oxygen demand (COD) (to call COD in the following text) is to measure in the water body to be subject to strong oxidizer, as Cr 2O 7 2-, MnO 4 -Equivalent Deng the organism of oxidation required oxygen when the oxidation.COD detection method commonly used has permanganate index method and potassium dichromate oxidation, and the apparatus of therefore measuring COD mostly is the conventional used instrument of titrimetry.Adopt above-mentioned instrument detecting COD will consume a large amount of concentrated sulphuric acids and expensive silver sulfate except analytic process, and in order to eliminate the interference of chlorion, outside the mercuric sulfate of need adding severe toxicity is sheltered, also need heating even high temperature to clear up, therefore return time is long, and operating process is loaded down with trivial details, and minute reaches 2-4 hour, the measurement result poor accuracy is easy to generate secondary pollution.
Along with COD detects the concern that is subjected to the environmental analysis field day by day, the new method of many detection COD has appearred in recent years, as: spectrophotometric method, coulometric titration etc.These methods are just improved traditional method on detection means, and it is long still to exist digestion time, and the measurement result accuracy is relatively poor, is easy to generate secondary pollution problems.
Summary of the invention
The object of the present invention is to provide a kind of device that can fast, accurately detect chemical oxygen demand of water body, specifically be meant and directly detect, preserve testing result, calculate the COD value that records, assay determination result's electrochemical analyser.
To achieve these goals, galvanochemistry oxygen demand electrochemical analyser provided by the invention is made up of three parts: flow injection sampling system, analysis and detection device and data handling system.Wherein the flow injection sampling system comprises constant current peristaltic pump and microsyringe, and constant current peristaltic pump model is a D100B/C type digital display constant current peristaltic pump, purchases the instrument plant in Shanghai City Hu Xi, can control current-carrying flow velocity 2-6000mL/h; The microsyringe model is 7520 type microsyringes, purchases the Rheodyne company limited in the U.S., accurate sample introduction 15 μ L at every turn, utilize this sampling system can realize the current-carrying system of constant flow rate and continuously, accurate sample introduction.
Analysis and detection device adopts the three-electrode electro Chemical system, comprise working electrode, auxiliary electrode, contrast electrode, induction pipe, outlet, upper cover plate, lower cover and poly tetrafluoroethylene, wherein induction pipe and outlet place the both sides of upper cover plate respectively, contrast electrode places within the outlet, poly tetrafluoroethylene places the centre of upper cover plate and lower cover, and the middle part has a breach to form detection cell, working electrode is in the central authorities of lower cover, auxiliary electrode is in the central authorities of upper cover plate, working electrode is the nano-oxide modified electrode, contrast electrode is saturated calomel electrode or Ag/AgCl electrode, with upper cover plate, poly tetrafluoroethylene and lower cover are fixed, and they are fused.The analysis and detection device of COD electrochemical analyzers of the present invention, its auxiliary electrode is the noncorroding metal electrode, the present invention is preferably gold electrode; Its upper cover plate and lower cover are the corrosion resistance material, preferably polytetrafluoroethylene plate of the present invention; Need closely to be associated in together between its upper cover plate, poly tetrafluoroethylene and the lower cover three, the present invention preferably fixes by screw or rivet.
Data handling system is made of CHI electrochemical workstation and computing machine, and the CHI electrochemical workstation is purchased in Shanghai occasion China instrument company.The electric signal that produces on nano COD sensor is gathered, is amplified by the CHI electrochemical workstation, is input to computing machine, finally by computing machine data is handled, analyzed directly to obtain chemical oxygen demand of water body (COD) value.
The analysis and detection device of COD electrochemical analyzers provided by the invention has carried out breakthrough improvement to traditional COD detection method, sample passes through the flow injection sampling system by quantitative injection analyzing and testing system, organism in the sample is degraded by the degree of depth on the nano COD sensor surface that applies certain potentials, on nano COD sensor, produce simultaneously electric signal, so just, realized the synchronization of digestion process and analyte detection process, shorten minute, improved the sensitivity of measuring.
The present invention has following advantage:
1, the present invention adopts flowing injecting analysis technology, therefore can realize fast, accurately detect chemical oxygen demand of water body (COD), finishes only to need 30 seconds consuming time to measuring from the beginning sample introduction;
2, the present invention has adopted high-level oxidation technology, and the hydroxyl radical free radical with strong oxidizing property that utilizes nano COD sensor to produce under certain current potential carries out degree of depth degraded to the organism in the water body;
3, the present invention has adopted thin layer Amperometric Detection Coupled device, has not only reduced sample size, has shortened digestion time, improved the sensitivity of analyzing, and sample need not loaded down with trivial details pre-service;
4, the present invention utilizes anodised method that the organic contaminant in the water body is cleared up, and only needs in the reaction body to add an amount of electrolyte, does not need to add other poisonous, hazardous agents.Therefore, utilize the present invention to measure chemical oxygen demand of water body and can not cause secondary pollution;
5, the present invention had both made things convenient for storage, the inquiry of determination data with detecting device and computing machine coupling, also was convenient to processing, the analysis of data;
6, compact conformation of the present invention, reasonable in design, easy to make.
Description of drawings
Fig. 1 is the analysis and detection device figure of COD electrochemical analyzers
Wherein, each member is respectively: working electrode 1, auxiliary electrode 2, contrast electrode 3, induction pipe 4, outlet 5, upper cover plate 6, lower cover 7 and poly tetrafluoroethylene 8.
Specific embodiment
Describe the structure and the course of work thereof of COD electrochemical analyzers provided by the invention in detail below in conjunction with Figure of description:
COD electrochemical analyzers provided by the invention comprises flow injection sampling system, analyzing and testing system and data handling system.The flow injection sampling system is made up of constant current peristaltic pump and microsyringe; Data handling system is made up of CHI electrochemical workstation and computing machine, be characterized in: the CHI electrochemical workstation can be reliably produces aqueous sample stream during pick-up unit by analysis at working electrode surface electric signal is gathered, is amplified, by computing machine to analyzing this signal Processing, analyzing final chemical oxygen demand (COD) (COD) value that obtains water sample.The analyzing and testing system comprises working electrode 1, auxiliary electrode 2, contrast electrode 3, induction pipe 4, outlet 5, upper cover plate 6, lower cover 7 and poly tetrafluoroethylene 8, wherein induction pipe 4 and outlet 5 place the both sides of upper cover plate 6 respectively, contrast electrode 3 places within the outlet 5, poly tetrafluoroethylene 8 places the centre of upper cover plate 6 and lower cover 7, and the middle part has a breach to form detection cell, working electrode 1 is in the central authorities of lower cover 7, auxiliary electrode 2 is in the central authorities of upper cover plate 6, working electrode 1 is the nano-oxide modified electrode, contrast electrode 3 is saturated calomel electrode or Ag/AgCl electrode, with upper cover plate 6, poly tetrafluoroethylene 8 and lower cover 7 are fixed, and they are fused.
When utilization COD electrochemical analyzers of the present invention detects the COD value of water sample, at first connect the constant current peristaltic pump, the interface of microsyringe and detecting device is also guaranteed that whole pipeline is unimpeded and is not had the phenomenon of leakage, open the constant current peristaltic pump then and be pre-charged with pipeline with current-carrying, after the populated pipeline of current-carrying, with working electrode 1, auxiliary electrode 2 and contrast electrode 3 are connected respectively to the CHI electrochemical workstation and apply certain operating potential on working electrode 1 surface, sample introduction is realized by microsyringe, water sample enters microsyringe afterwards by quantitative filling line and along with current-carrying flows into poly tetrafluoroethylenes 8 central thin layer detection cells from current-carrying induction pipe 4, water sample is flowed through with current-carrying and is flowed into current-carrying outlet 5 behind the thin layer detection cell, flows out pipelines from current-carrying outlet 5 at last.When the organic substance in the water sample is diffused into working electrode 1 surface, can be by catalytic oxidation, on working electrode 1, produce corresponding electric signal simultaneously, this electric signal is transferred to the CHI electrochemical workstation, obtain digital signal by amplification, analog to digital conversion, this digital signal is transferred to computing machine finally calculates water sample by data processing COD value again.

Claims (4)

1, a kind of COD electrochemical analyzers, by the flow injection sampling system, analysis and detection device and data handling system are formed, it is characterized in that: analysis and detection device adopts the three-electrode electro Chemical system, comprise working electrode (1), auxiliary electrode (2), contrast electrode (3), induction pipe (4), outlet (5), upper cover plate (6), lower cover (7) and poly tetrafluoroethylene (8), wherein induction pipe (4) and outlet (5) place the both sides of upper cover plate (6) respectively, contrast electrode (3) places within the outlet (5), poly tetrafluoroethylene (8) places the centre of upper cover plate (6) and lower cover (7), and the middle part has a breach to form detection cell, working electrode (1) is in the central authorities of lower cover (7), auxiliary electrode (2) is in the central authorities of upper cover plate (6), working electrode (1) is the nano-oxide modified electrode, auxiliary electrode (2) is the noncorroding metal electrode, contrast electrode (3) is saturated calomel electrode or Ag/AgCl electrode, upper cover plate (6) and lower cover (7) are resistant material, with upper cover plate (6), poly tetrafluoroethylene (8) and lower cover (7) are fixed, and they are fused.
2, COD electrochemical analyzers as claimed in claim 1 is characterized in that auxiliary electrode (2) is a gold electrode.
3, COD electrochemical analyzers as claimed in claim 1 is characterized in that upper cover plate (6) and lower cover (7) are polyfluortetraethylene plate.
4, COD electrochemical analyzers as claimed in claim 1 is characterized in that fixing by screw or rivet between upper cover plate (6), poly tetrafluoroethylene (8) and lower cover (7) three.
CN 200510023445 2005-01-19 2005-01-19 COD electrochemical analyzers Pending CN1645127A (en)

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CN 200510023445 CN1645127A (en) 2005-01-19 2005-01-19 COD electrochemical analyzers

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CN 200510023445 CN1645127A (en) 2005-01-19 2005-01-19 COD electrochemical analyzers

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1975400B (en) * 2006-09-29 2010-05-12 华东师范大学 Apparatus for measuring chemical oxyger requirement by photoelectric concerted catalysis
CN102866186A (en) * 2012-09-12 2013-01-09 合肥工业大学 Circulating-type water chemical oxygen demand detection photoelectrochemical sensor
CN103207225A (en) * 2013-03-14 2013-07-17 华中科技大学 Electrochemical transducer probe for detecting chemical oxygen demand and manufacturing method of electrochemical transducer probe
CN103376219A (en) * 2012-04-27 2013-10-30 中国科学院电子学研究所 Integrated resolved-chip system and water sample resolving method
CN104597094A (en) * 2015-01-22 2015-05-06 北京农业智能装备技术研究中心 Device for detecting dynamic ion flow of vegetable living body
CN105092676A (en) * 2015-09-10 2015-11-25 鞠文军 Electrochemical detection cell
CN110044810A (en) * 2019-03-28 2019-07-23 中国船舶重工集团公司第七二五研究所 A kind of artificial gap device studied for crevice corrosion under simulated deep-sea environment

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1975400B (en) * 2006-09-29 2010-05-12 华东师范大学 Apparatus for measuring chemical oxyger requirement by photoelectric concerted catalysis
CN103376219A (en) * 2012-04-27 2013-10-30 中国科学院电子学研究所 Integrated resolved-chip system and water sample resolving method
CN102866186A (en) * 2012-09-12 2013-01-09 合肥工业大学 Circulating-type water chemical oxygen demand detection photoelectrochemical sensor
CN103207225A (en) * 2013-03-14 2013-07-17 华中科技大学 Electrochemical transducer probe for detecting chemical oxygen demand and manufacturing method of electrochemical transducer probe
CN104597094A (en) * 2015-01-22 2015-05-06 北京农业智能装备技术研究中心 Device for detecting dynamic ion flow of vegetable living body
CN104597094B (en) * 2015-01-22 2017-02-22 北京农业智能装备技术研究中心 Device for detecting dynamic ion flow of vegetable living body
CN105092676A (en) * 2015-09-10 2015-11-25 鞠文军 Electrochemical detection cell
CN110044810A (en) * 2019-03-28 2019-07-23 中国船舶重工集团公司第七二五研究所 A kind of artificial gap device studied for crevice corrosion under simulated deep-sea environment
CN110044810B (en) * 2019-03-28 2021-12-31 中国船舶重工集团公司第七二五研究所 Artificial gap device for simulating gap corrosion research under deep sea environment

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