CN103604852A - Method for preparing Ag/AgCl work electrode for monitoring chloride ion concentration - Google Patents
Method for preparing Ag/AgCl work electrode for monitoring chloride ion concentration Download PDFInfo
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- CN103604852A CN103604852A CN201310624990.1A CN201310624990A CN103604852A CN 103604852 A CN103604852 A CN 103604852A CN 201310624990 A CN201310624990 A CN 201310624990A CN 103604852 A CN103604852 A CN 103604852A
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Abstract
The invention relates to corrosion on-line safety monitoring on sea port engineering and especially relates to a method for preparing an Ag/AgCl work electrode for monitoring a chloride ion concentration. The method comprises the following steps that Ag powder and AgCl powder are uniformly mixed according to a mass ratio of 9-10: 1; the mixture is put into a mortar and is fully grinded and polyethylene glycol 1000 is added into the mortar in grinding; the grinded powder is cleaned orderly by n-heptane and distilled water; and the cleaned powder is dried and pressed to form the Ag/AgCl work electrode. Through powder homogenization treatment before tabletting, electrode stability is guaranteed; and in tabletting, silver threads are embedded in the powder and then are directly pressed into the Ag/AgCl work electrode so that use is convenient, and welded lead loosening or drilling time and labor consumption is avoided. The Ag/AgCl work electrode can guarantee Ag/AgCl electrode stability and has a utilization rate close to 100%.
Description
Technical field
The present invention relates to the corrosion on-line monitoring of ocean port engineering, be specifically related to a kind of method of the Ag/Agcl working electrode for the preparation of monitoring chloride ions concentration of concrete.
Background technology
Ag/Agcl electrode is because its current potential is stable, reappearance is good, easily the advantage such as preparation is widely used in every field.Ag/Agcl is applied to surveying laboratory reinforcing steel to Atkins CP etc. and concrete extrudes chlorine ion concentration in hole solution, and result shows that measured chlorine ion concentration and the value calculating according to activity coefficient theory are identical good.The Ag/Agcl electrode of the preparations such as M.A Climent-Llorca is imbedded in mortar specimen prepared by the sodium chloride solution of different chlorine ion concentrations and is tested its performance, finds that electrode shows good linear response in certain chlorine ion concentration.Montemo.M.F etc. imbed Ag/Agcl electrode the different depth of mortar and concrete sample, monitoring is invaded chlorion under bubble to the diffusion process in mortar and concrete at chloride solution, and result shows that Ag/Agcl electrode has good stability at whole duration of test.The application of the visible Ag/Agcl electrode type chlorion sensor based on electrochemical principle in concrete works has huge potentiality, and as the stability of the Ag/Agcl electrode of working sensor electrode, will directly affect the accuracy of Monitoring Data and permanance judgement, so the stability of Ag/Agcl electrode has very important effect to the accuracy of sensor.
The manufacture craft of Ag/Agcl electrode probably has three kinds at present: electrolytic process, screen printing technique and pressed disc method.Electrolytic process: take purity as 99.99% fine silver silk be anode, the platinum filament that the purity of take is 99.95% is negative electrode, anode electrolysis chlorination has under these conditions prepared Ag/Agcl electrode.Ag/Agcl electrode prepared by the method is that physical strength is not high at Ag surface electrolysis last layer Agcl layer.The words of careless grazing in assembling or experimentation, Agcl layer may will be rubbed off, affect electrode stability, and the electrolytic process technique of preparing Ag/Agcl electrode can be subject to the impact of Anodic polarization current and electrolysis time, cause the compactness of Ag/Agcl electrolyte layers different, thus the stability of having influence on.Screen printing technique: this technology is to adopt a semi-automatic printer is first printed one deck Ag China ink in polyimide substrate, then on Ag China ink, prints one deck Agcl layer, and Ag and Agcl layer are dried to 20min at 120 ℃.Finally, at electrolysis last layer protective layer China ink, at 120 ℃, dry 30min equally.Just prepared thus Ag/Agcl electrode.This technology is newer, at Japanese magazine, has been, and technology more complicated, the domestic exploitation of not meeting this type of technology, is not easy to prepare this electrode by the method, and application aspect is also not universal.Pressed disc method: the method is that Ag and Agcl are mixed according to a certain percentage, puts into stirring machine high speed and stirs 120s, then weighs the powder of getting certain mass in the balance and puts into mould, adopts sheeter compressing, preparation Ag/Agcl electrode.The method is relatively simple, within one day, can press more than 40 electrode, but poor aspect stability, and compressing tablet only has 1/3-1/2 electrode to use at every turn, and utilization factor is lower.Follow-up welding lead or the drilling and tapping of also needing of electrode suppressing connects wire, wastes time and energy.The limitation and the deficiency that for said method, exist, need to provide the stabilized electrodes that utilization factor is high.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing the Ag/Agcl working electrode that is applicable to monitor chlorine ion concentration.
For achieving the above object, the technical solution used in the present invention is:
A kind of method of preparing the Ag/Agcl working electrode that is applicable to monitor chlorine ion concentration, the Ag powder that is 9-10:1 by mass ratio and Agcl powder mix, mix to be placed in mortar and fully grind, during grinding, add cetomacrogol 1000, powder after fully grinding, with rinsing through normal heptane and distilled water successively, is then dried compacting and is Ag/Agcl electrode.
Described when compacting Ag/Agcl electrode, directly by silver-colored line pressure in electrode the inside.Specifically powder is put into after mould, first filamentary silver line is penetrated in the ommatidium of depression bar bottom (ommatidium diameter 0.5mm), filamentary silver line will grow the about 2mm of ommatidium left and right, then depression bar is put into mould compacting obtains the Ag/Agcl electrode with filamentary silver line.
After described mixing, powder is placed in agate mortar and grinds 10-15min, then adds cetomacrogol 1000 that Ag powder and Agcl powder in mixed-powder are uniformly dispersed.
After described grinding, powder, with rinsing through normal heptane and distilled water successively, is then dried compacting and is Ag/Agcl electrode under 27 ℃ of-45 ℃ of low temperature.
Preferably, powder after grinding, with rinsing through normal heptane and distilled water successively, is then dried under 27-32 ℃ of low temperature, after oven dry, in mortar, grind again, under dark, stand-by after grinding.
Described normal heptane concentration is 0.1mol/L.
The present invention has advantages of: the present invention had carried out uniform treatment to powder before compressing tablet, to guarantee electrode stability, and in compressing tablet process, filamentary silver line is imbedded in powder, be directly pressed in electrode the inside, very easy to use, avoided becoming flexible of welding lead or wasting time and energy of jewel hole.The working electrode that the present invention makes can guarantee the stability of Ag/Agcl electrode, and utilization factor approaches 100%.
Accompanying drawing explanation
Ag/Agcl electrode open circuit potential (OCP) figure that Fig. 1 provides for the embodiment of the present invention.
The Ag/Agcl electrode 30d potential value variation diagram that Fig. 2 provides for the embodiment of the present invention.
Embodiment
The preparation of electrode:
By Ag powder and Agcl powder, be that 9:1 is even in stirrer for mixing in mass ratio, after mixing, putting into agate mortar grinds 15min and fully grinds, grinding limit, limit adds cetomacrogol 1000, Ag powder and Agcl powder in mixed-powder are uniformly dispersed, after to be ground completing, powder is poured in beaker, the normal heptane and the distilled water that by concentration, are 0.1mol/L successively rinse, then dry, be put in dark place standby.
With the spoon above-mentioned powder that takes a morsel, put into the pan paper on balance, taking quality is 2g, load weighted powder is slowly poured in the duct of mould, filamentary silver line is penetrated to (diameter is about 0.5mm) in the ommatidium in depression bar and expose 2mm left and right length.Depression bar is put into mould duct, with hand, firmly push depression bar, and rotation prevents powder demoulding difficulty after compacting in depression bar and space, duct.Mould is put on sheeter platform, manual turn screw rod, makes mould and sheeter press together (mould is placed on platform central authorities, prevent eccentric force from mould is damaged by pressure) again.Tighten fuel outlet valve, manually press depression bar pressurization, stop, in 1min, then, continuing to be pressurized to 20Mpa, to unclamp fuel outlet valve when being pressurized to 10Mpa, mold removal, takes mould apart, takes out electrode.If depression bar be cannot take out, be placed on sheeter, slowly pressurization carry out the demoulding (all experiments are all to operate in darkroom, spoon, beaker etc. all through absolute ethyl alcohol and distilled water flushing and dried).Then prepare again in the manner described above 12 groups of electrodes.
Application examples
13 groups of Ag/Agcl electrodes prepared by above-described embodiment carry out open circuit potential (OCP) and detect, and specifically, adopt three-electrode system, and working electrode is Ag/Agcl electrode, and contrast electrode is saturated calomel electrode, and auxiliary electrode is platinized platinum (referring to Fig. 1).
In addition, above-mentioned 13 groups of electrodes are carried out to electrode 30d potential value change detection, result is referring to Fig. 2.
13 groups of Ag/Agcl electrodes OCP in 10min as seen from Figure 1, all electrodes after left and right remains on radix point always in front 300s 6, continue to have observed 10min, and after radix point 5 always of open circuit potentials, have good stability.
By 2 visible above-mentioned Ag/Agcl electrodes, be immersed in 0.1mol/L Nacl solution a month potential value variation diagram of test constantly.Ag/Agcl electrode shows long-term stability, has changed one time Nacl solution when 23d, and potential value fluctuation is larger, but potential value, always in steady state (SS), illustrates that electrode has good reappearance and stability in the lasting observation of 10d subsequently.Potential value in this electrode solution under the same conditions floats and is starting to be to the maximum for several days 2mv, much smaller than the 10mv limiting in standard, continuous two always remain on-43mv of electrode potential value of 6d after soaking 10d, change between always remain on-51mv of solution afterpotential value, show good reappearance, same electrode maximum float is 0.5mv, and Different electrodes maximum potential value in same one-shot measurement is floated as 0.1mv.
Research is found by experiment, and the present invention makes simple and convenient, and electrode stability and reappearance are good, and utilization ratio is high.
Claims (6)
1. a method of preparing the Ag/Agcl working electrode that is applicable to monitor chlorine ion concentration, it is characterized in that: the Ag powder that is 9-10:1 by mass ratio and Agcl powder mix, mix to be placed in mortar and fully grind, during grinding, add cetomacrogol 1000, powder after fully grinding, with rinsing through normal heptane and distilled water successively, is then dried compacting and is Ag/Agcl electrode.
2. by preparation claimed in claim 1, be applicable to monitor the method for the Ag/Agcl working electrode of chlorine ion concentration, it is characterized in that: described when compacting Ag/Agcl electrode, directly by silver-colored line pressure in electrode the inside.
3. by preparation claimed in claim 1, be applicable to monitor the method for the Ag/Agcl working electrode of chlorine ion concentration, it is characterized in that: powder after mixing is placed in to agate mortar and grinds 10-15min, then add cetomacrogol 1000 that Ag powder and Agcl powder in mixed-powder are uniformly dispersed.
4. by preparation claimed in claim 1, be applicable to monitor the method for the Ag/Agcl working electrode of chlorine ion concentration, it is characterized in that: powder after grinding, with rinsing through normal heptane and distilled water successively, is then dried to compacting and is Ag/Agcl electrode under 27 ℃ of-45 ℃ of low temperature.
5. by preparation claimed in claim 4, be applicable to monitor the method for the Ag/Agcl working electrode of chlorine ion concentration, it is characterized in that: by powder after grinding with rinsing through normal heptane and distilled water successively, then under 27-32 ℃ of low temperature, dry, after oven dry, in mortar, grind again, under dark, stand-by after grinding.
6. by the preparation described in claim 1,3 or 4, be applicable to monitor the method for the Ag/Agcl working electrode of chlorine ion concentration, it is characterized in that: described normal heptane concentration is 0.1mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969306A (en) * | 2014-04-18 | 2014-08-06 | 中国科学院海洋研究所 | Silver/silver chloride electrode applicable to deep sea and preparation method thereof |
| CN107271799A (en) * | 2017-06-02 | 2017-10-20 | 中国地质大学（武汉） | A kind of preparation method of the small solid electrode of extreme difference drift |
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Cited By (3)
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|---|---|---|---|---|
| CN103969306A (en) * | 2014-04-18 | 2014-08-06 | 中国科学院海洋研究所 | Silver/silver chloride electrode applicable to deep sea and preparation method thereof |
| CN103969306B (en) * | 2014-04-18 | 2016-08-24 | 中国科学院海洋研究所 | A kind of silver/silver chloride electrode being applicable to deep-sea and preparation method thereof |
| CN107271799A (en) * | 2017-06-02 | 2017-10-20 | 中国地质大学（武汉） | A kind of preparation method of the small solid electrode of extreme difference drift |
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