CN102608191B - The galvanochemistry on-line cleaning method of heavy metal on-line computing model working electrode - Google Patents
The galvanochemistry on-line cleaning method of heavy metal on-line computing model working electrode Download PDFInfo
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- CN102608191B CN102608191B CN201110403844.7A CN201110403844A CN102608191B CN 102608191 B CN102608191 B CN 102608191B CN 201110403844 A CN201110403844 A CN 201110403844A CN 102608191 B CN102608191 B CN 102608191B
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Abstract
The present invention relates to a kind of galvanochemistry on-line cleaning method of the working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry.Each cleaning frequency comprise the positive potential of working electrode is cleaned, negative potential cleaning and recovery three steps of initial potential, described positive potential cleaning current potential (V1) be on the occasion of, described negative potential cleaning current potential (V2) is negative value, and described initial potential (V3) is between (V1) and (V2).Electrochemical cleaning method of the present invention, can clean working electrode surface comprehensively, ensure that good electrode reappearance, achieve the on-line cleaning of working electrode, the research and development breached based on the heavy metal automatic on-line monitoring instrument of anodic stripping voltammetry limit.
Description
Technical field
The present invention relates to a kind of electrochemical cleaning method, particularly relate to a kind of galvanochemistry on-line cleaning method of the working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry.
Background technology
In recent years, heavy metal pollution event takes place frequently, and since two thousand nine China has recurred more than 30 particularly serious heavy metal pollution event.In the face of heavy metal pollution situation occurred frequently, improvement heavy metal pollution is formally brought into schedule by Chinese Government.Country also will increase input in coherent detection and monitoring instrument.Thus, the heavy metal pollution testing and monitoring instrument of China rapidly increases in recent years.
At present, domestic heavy metal automatic on-line monitoring instrument adopts spectrophotometric method mostly, and this method cost is low, and belong to the chemical analysis method of comparative maturity, be easy to comparatively speaking realize, but this method reagent consumption is large, the impact of colourity and turbidity can not be eliminated, can not realize monitoring multiparameter, and Determination Limit can not meet the demands sometimes simultaneously, if with other concentration and separation technology couplings, can Monitoring lower-cut be reduced, but complex operation.
Adopt anodic stripping voltammetry just can overcome the above problems, this method adopts three-electrode system, device is easy, reagent dosage is few, Determination Limit is low, and colourity and turbidity noiseless, many kinds of parameters can be monitored, so will be more and more welcome based on the heavy metal automatic on-line monitoring instrument of anodic stripping voltammetry simultaneously.But, very poor for the working electrode reappearance of the heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry, seriously govern the development and application of this instrument.At present, working electrode for the heavy metal automatic on-line monitoring instrument based on anodic stripping voltammetry is mainly cleaned by constant potential, a constant potential is added to electrode, make the oxidation of impurities stripping on electrode, although such cleaning way can wash down original impurity major part, new oxidation state interference can be formed at electrode surface.
Summary of the invention
For solving the problem, the invention provides a kind of galvanochemistry on-line cleaning method of the working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry.
Technical scheme of the present invention is: a kind of galvanochemistry on-line cleaning method of the working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry, each cleaning frequency comprise the positive potential of working electrode is cleaned, negative potential cleaning and recovery three steps of initial potential, described positive potential cleaning current potential (V1) be on the occasion of, described negative potential cleaning current potential (V2) is negative value, and described initial potential (V3) is between (V1) and (V2).
Preferably, described positive potential cleaning current potential (V1), negative potential cleaning current potential (V2) and initial potential (V3) are constant potential.
Preferably, described positive potential cleaning current potential (V1) span is 0V ~+3V.
Preferably, described negative potential cleaning current potential (V2) span is-3V ~ 0V.
Preferably, the recovery duration span of the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), initial potential (V3) is for being greater than 0, and being less than or equal to 1000ms, scavenging period is greater than 30s.
Preferably, the duration ratio that described positive potential cleaning current potential (V1) and negative potential clean current potential (V2) is different from the duration ratio that the recovery of initial potential (V3) and negative potential clean current potential (V2).
Preferably, the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration ratio of initial potential are 6: 1: 3 or 14: 1: 5.
Preferably, the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration of initial potential are respectively 60ms, 10ms, 30ms, and scavenging period is 60s.
Preferably, the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration of initial potential are respectively 70ms, 5ms, 25ms, and scavenging period is 100s.
The course of work of the present invention is:
Heavy metal on-line computing model based on anodic stripping voltammetry is set the parameter detecting waste water, waste water sample introduction measures, after mensuration completes, working electrode electrochemical cleaning parameter used is set: it is 0V ~+3V that positive potential cleans current potential V1 used, it is-3V ~ 0V that negative potential cleans current potential V2 used, initial potential V3 is between V1 and V2, the recovery duration span of the duration of positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), initial potential is for being greater than 0, and being less than or equal to 1000ms, scavenging period is greater than 30s; After setting parameter, start cleaning electrode, after having cleaned, with distilled water flushing, complete mensuration.
The invention has the beneficial effects as follows: electrochemical cleaning method of the present invention, by the alternate sweep of positive negative potential, can by the substance oxidation stripping of enrichment originally on working electrode, oxidation state a small amount of on working electrode can be removed again, can clean working electrode surface comprehensively, make the surface state before each mensuration identical, thus ensure that good electrode reappearance, achieve the on-line cleaning of working electrode, the research and development breached based on the heavy metal automatic on-line monitoring instrument of anodic stripping voltammetry limit.
Accompanying drawing explanation
Fig. 1 and Fig. 2 is the time dependent sweep waveform figure of voltage of the galvanochemistry on-line cleaning method of working electrode of the present invention;
Fig. 3 is that the galvanochemistry on-line cleaning method of working electrode of the present invention is for measuring the volt-ampere curve of lead waste water gained.
Fig. 4 is that the galvanochemistry on-line cleaning method of working electrode of the present invention is for measuring the volt-ampere curve of arsenic-containing waste water gained.
Concrete embodiment
The present invention is mainly applicable to the cleaning of the working electrode of the heavy metal on-line computing model based on anodic stripping voltammetry.A kind of galvanochemistry on-line cleaning method of the working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry, each cleaning frequency comprise the positive potential of working electrode is cleaned, negative potential cleaning and recovery three steps of initial potential, described positive potential cleaning current potential (V1) be on the occasion of, described negative potential cleaning current potential (V2) is negative value, and described initial potential (V3) is between (V1) and (V2).
Positive potential cleaning current potential (V1), negative potential cleaning current potential (V2) and initial potential (V3) are constant potential.
Positive potential cleaning current potential (V1) span is 0V ~+3V.
Negative potential cleaning current potential (V2) span is-3V ~ 0V.
The duration of positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration span of initial potential (V3) are 0 ~ 1000ms, and scavenging period is greater than 30s.
The duration ratio that positive potential cleaning current potential (V1) and negative potential clean current potential (V2) is different from the duration ratio that the recovery of initial potential (V3) and negative potential clean current potential (V2).
The duration of positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration ratio of initial potential are 6: 1: 3 or 14: 1: 5.
The duration of positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration of initial potential are respectively 60ms, 10ms, 30ms, and scavenging period is 60s.
The duration of positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration of initial potential are respectively 70ms, 5ms, 25ms, and scavenging period is 100s.
The course of work of the present invention is:
Heavy metal on-line computing model based on anodic stripping voltammetry is set the parameter detecting waste water, waste water sample introduction measures, after mensuration completes, working electrode electrochemical cleaning parameter used is set: it is 0V ~+3V that positive potential cleans current potential V1 used, it is-3V ~ 0V that negative potential cleans current potential V2 used, initial potential V3 is between V1 and V2, the recovery duration span of the duration of positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), initial potential is for being greater than 0, and being less than or equal to 1000ms, scavenging period is greater than 30s; After setting parameter, start cleaning electrode, after having cleaned, with distilled water flushing, complete mensuration.
Below in conjunction with drawings and the specific embodiments, the specific embodiment of the present invention is described:
Embodiment 1: the repeatedly mensuration of the same water sample of lead waste water in industrial waste water
Choosing certain Electroplate Factory is experimental point, gets 5 parts of same waste water, numbering 1,2,3,4,5# respectively, after suitable pre-service, stand-by.
Get 1# waste water, adopt the heavy metal on-line computing model based on anodic stripping voltammetry, set parameter, sample introduction measures, after mensuration completes, as shown in Figure 1, electrochemical cleaning parameter used is set: positive potential cleans current potential V1=0.3V used, negative potential cleans current potential V2=-0.3V used, initial potential V3=0V, positive potential cleaning duration PT=60ms, negative potential cleaning duration NT=10ms, the recovery duration DT=30ms of initial potential, scavenging period is 60s, and namely loop cycle number of times is 600 times.After setting parameter, start cleaning electrode, after having cleaned, with distilled water flushing, complete mensuration.Get 2# respectively more afterwards, 3#, 4#, 5# water sample, repeat above-mentioned experiment, after completing mensuration, obtain volt-ampere curve as shown in Figure 3.Analysis chart picture, can finding out by adopting the electrochemical cleaning method provided by the present invention working electrode used to the heavy metal on-line computing model based on anodic stripping voltammetry to clean, can meet reproducible requirement.
Embodiment 2: the repeatedly mensuration of the same water sample of arsenic-containing waste water in industrial waste water
Get 5 parts of same arsenic-containing waste waters, numbering 1,2,3,4,5# respectively, after suitable pre-service, stand-by.
Get 1# waste water, adopt the heavy metal on-line computing model based on anodic stripping voltammetry, set parameter, sample introduction measures, after mensuration completes, as shown in Figure 2, electrochemical cleaning parameter used is set: positive potential cleans current potential V1=1.0V used, negative potential cleans current potential V2=-0.5V used, initial potential V3=0V, positive potential cleaning duration PT=70ms, negative potential cleaning duration NT=5ms, the recovery duration DT=25ms of initial potential, scavenging period is 100s, and namely loop cycle number of times is 1000 times.After setting parameter, start cleaning electrode, after having cleaned, with distilled water flushing, complete mensuration.Get 2# respectively more afterwards, 3#, 4#, 5# water sample, repeat above-mentioned experiment, after completing mensuration, obtain volt-ampere curve as shown in Figure 4.Analysis chart picture, can finding out by adopting the electrochemical cleaning method provided by the present invention working electrode used to the heavy metal on-line computing model based on anodic stripping voltammetry to clean, can meet reproducible requirement.
Claims (6)
1. the galvanochemistry on-line cleaning method for the working electrode of the heavy metal on-line computing model based on anodic stripping voltammetry, comprise in each cleaning frequency and the positive potential of working electrode is cleaned, recovery three steps of negative potential cleaning and initial potential, described positive potential cleaning current potential (V1) be on the occasion of, described negative potential cleaning current potential (V2) is negative value, described initial potential (V3) is between positive potential cleaning current potential (V1) and negative potential cleaning current potential (V2), the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration span of initial potential (V3) is for being greater than 0, and be less than or equal to 1000ms, scavenging period is greater than 30s.
2. the galvanochemistry on-line cleaning method of a kind of working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry as claimed in claim 1, the duration ratio that described positive potential cleaning current potential (V1) and negative potential clean current potential (V2) is different from the duration ratio that the recovery of initial potential (V3) and negative potential clean current potential (V2).
3. the galvanochemistry on-line cleaning method of a kind of working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry as claimed in claim 2, the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration ratio of initial potential are 6:1:3 or 14:1:5.
4. the galvanochemistry on-line cleaning method of a kind of working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry as claimed in claim 2 or claim 3, the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration of initial potential are respectively 60ms, 10ms, 30ms, and scavenging period is 60s.
5. the galvanochemistry on-line cleaning method of a kind of working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry as claimed in claim 2 or claim 3, the duration of described positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration of initial potential are respectively 70ms, 5ms, 25ms, and scavenging period is 100s.
6. the galvanochemistry on-line cleaning method of a kind of working electrode for the heavy metal on-line computing model based on anodic stripping voltammetry as claimed in claim 1, its course of work is:
Heavy metal on-line computing model based on anodic stripping voltammetry is set the parameter detecting waste water, waste water sample introduction measures, after mensuration completes, working electrode electrochemical cleaning parameter used is set: it is 0V ~+3V that positive potential cleans current potential used (V1), it is-3V ~ 0V that negative potential cleans current potential used (V2), initial potential (V3) is between positive potential cleaning current potential (V1) and negative potential cleaning current potential (V2), the duration of positive potential cleaning current potential (V1), the duration of negative potential cleaning current potential (V2), the recovery duration span of initial potential is for being greater than 0, and be less than or equal to 1000ms, , scavenging period is greater than 30s, after setting parameter, start cleaning electrode, after having cleaned, use distilled water flushing.
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| CN104359965B (en) * | 2014-11-12 | 2017-01-11 | 福州大学 | Trace metal ion detection device based on multi-auxiliary-electrode stripping voltammetry and use method |
| CN104914152B (en) * | 2015-05-22 | 2017-09-22 | 中国科学院长春应用化学研究所 | The cleaning method of the microelectrode of water body toxicity detection means |
| CN107305194B (en) * | 2016-04-21 | 2019-06-25 | 北京华科天宇环保科技有限公司 | A kind of heavy metal detector and its electrolytic cell |
| 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 |
| CN111537590B (en) * | 2020-04-15 | 2022-06-14 | 力合科技（湖南）股份有限公司 | Automatic on-line repairing method for mercury membrane modified electrode |
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| WO2011005764A1 (en) * | 2009-07-06 | 2011-01-13 | Ada Technologies, Inc. | Electrochemical device and method for long-term measurement of hypohalites |
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| CN1224838A (en) * | 1999-01-12 | 1999-08-04 | 核工业北京化工冶金研究院 | Surface scale preventing method for metal electrode |
| CN101271080A (en) * | 2008-05-12 | 2008-09-24 | 杭州电子科技大学 | On-line automatic cleaning device for electro-chemistry glass electrode |
| CN101504385A (en) * | 2009-03-17 | 2009-08-12 | 武汉大学 | Method for improving sensibility, selectivity and anti-poisoning ability of carbon electrode |
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