CN102645470A - Preparation method of electrochemical sensor for dissolved oxygen detection - Google Patents
Preparation method of electrochemical sensor for dissolved oxygen detection Download PDFInfo
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- CN102645470A CN102645470A CN2012100916729A CN201210091672A CN102645470A CN 102645470 A CN102645470 A CN 102645470A CN 2012100916729 A CN2012100916729 A CN 2012100916729A CN 201210091672 A CN201210091672 A CN 201210091672A CN 102645470 A CN102645470 A CN 102645470A
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Abstract
The invention relates to a preparation method of an electrochemical sensor for dissolved oxygen detection, comprising the following steps of: firstly, preparing a salen ligand; then dissolving 6.4 mol of the salen ligand into 50 ml of an ethanol solution to form a solution C; dissolving 6.4 mol of nickel acetate into 50 mol of the ethanol solution to form a solution D; gradually dripping the solution C into the solution D to form a mixed solution; drying, precipitating and filtering to obtain a nickel-salen ligand; and finally, carrying out electro-polymerization on the nickel-salen ligand on a platinum electrode with the area of 0.071 cmW so as to obtain the electrochemical sensor. The electrochemical sensor for the dissolved oxygen detection prepared by the invention has high flexibility and stability, and has a better application value.
Description
Technical field:
The present invention relates to a kind of preparation method of electrochemical sensor, relate in particular to a kind of electrochemical sensor preparation method that dissolved oxygen DO detects that is used for.
Background technology:
In recent years, oxygen reduction is showing very large importance aspect the theory of a lot of bioprocess and chemosynthesis and the practical application.What wherein attract people's attention most is the research of catalytic process that is applied to the polyelectron oxygen reduction of biological respinse and fuel cell.Because the oxygen reduction process comprises multiple electron transfer; And there is an important activation evergy barrier; Utilize electrocatalysis material; Such as platinum, gold, metal oxide, organism, transition metal ring-type complex compound, biology enzyme etc., carrying out electrochemical reduction oxygen has had a large amount of research, but the conventional efficient that utilizes artificial catalysis to study oxygen reduction at present lowly, is not obtained remarkable success.
Caused researcher extensive interest as the transition metal complex that part constitutes because of its simple preparation method by schiff bases.This complex compound is applied to electrode surface through electro-polymerization usually and comes modified electrode, at last at platinum electrode or the surperficial film that forms conducting polymer of glassy carbon electrode.Compare with the experiment electrochemical techniques, homogeneous is formed and the film modified electrode of thickness shows three kinds of charge transfer speed: fast, slow and moderate.If charge transfer is faster than experimental, so oxidation in the film/reduction site concentration be exactly homogeneous and reach thermodynamic equilibrium with the electrode potential that applies, at this moment VA characteristic curve demonstrates symmetrical shape.
Be not very clear and definite to the detection method of solvent oxygen to the research of the detailed mechanism of catalytic process at present, detection efficiency also has much room for improvement.
Summary of the invention:
The present invention is directed to the deficiency of prior art, a kind of preparation method who is used for the electrochemical sensor that dissolved oxygen DO detects who in the mixed solution of the high oronain of acetonitrile/tetrabutyl, through cyclic voltammetry nickel-salen complex is powered on and forms after causing polymerization at platinum electrode is provided.
A kind of electrochemical sensor preparation method who is used for the dissolved oxygen DO detection, its step is following:
(1) preparation salen part: the salicylide (salicylaldehyde) of 0.284mol is dissolved in the 50ml ethanol forms solution A; The ethylenediamine of 0.142mol is dissolved in the 25ml ethanol forms solution B; And then with solution A and solution B mixing formation mixed solution; The mixed solution that forms obtains the yellow solid sediment at 40 ℃ of following stirring and refluxing 2h; Leach the yellow solid sediment with carrying out recrystallization with methyl alcohol again after the washing with alcohol and to obtain the Salen part, the Salen part is preserved in vacuum;
(2) preparation nickel-salen complex: the Salen part of 6.4mol is dissolved in the ethanolic solution of 50ml and forms solution C; The nickel acetate of 6.4mol is dissolved in the ethanolic solution of 50ml and forms solution D; Again solution C is dropwise dripped and form mixed solution in the solution D; Then mixed solution is obtained the red solid deposition at 40 ℃ of refluxed 2h, the red solid deposition is leached with methyl alcohol carry out obtaining nickel-salen complex behind the recrystallization, with the vacuum preservation at room temperature of nickel-salen complex;
(3) preparation electrochemical sensor: is 0.071cm with nickel-salen complex at area
2Platinum electrode on cause polymerization through electricity, thereby obtain electrochemical sensor.
It is to be with 100mVs in the mixed solution of acetonitrile, the high oronain of the tetrabutyl of 0.1mol/L in concentration that described electricity causes polymerization
-1Speed in the voltage range of 0～1.4V (contrast saturated calomel electrode), carry out polyreaction four times with cyclic voltammetry.
The present invention can solve following technical matters:
(1) the present invention is through preparation nickel-salen complex; Make nickelous-salen complex at first be reduced to monovalence nickel-salen complex; Monovalence nickel-salen complex is oxidized to nickelous-salen complex again by oxygen then; Nickelous-salen the complex that generates can be monovalence nickel-salen complex by electrochemical reduction again, thereby makes cathode current strengthen, so plated with nickel-salen coordination compound film can promote the reduction of oxygen on platinum electrode.
The electricity of the electron transfer catalysis dissolved oxygen DO that (2) platinum electrode of the present invention through nickel-salen complex decorating can be through contact bed causes reduction process; Compare with pure platinum electrode; Polarizing voltage has reduced 0.15eV in containing the solution of oxygen; The platinum electrode of prepared nickel-salen complex decorating all is very useful to quality control in commercial sample and the Environmental Water and conventional analysis, and is very consistent with the testing result of commercial oxygen sensor to the result who detects oxygen.
Embodiment:
In order to deepen, the present invention is made further detailed description below in conjunction with implementing to understanding of the present invention.
A kind of electrochemical sensor preparation method who is used for the dissolved oxygen DO detection, its step is following:
(1) preparation salen part: the salicylide (salicylaldehyde) of 0.284mol is dissolved in the 50ml ethanol forms solution A; The ethylenediamine of 0.142mol is dissolved in the 25ml ethanol forms solution B; And then with solution A and solution B mixing formation mixed solution; The mixed solution that forms obtains the yellow solid sediment at 40 ℃ of following stirring and refluxing 2h; Leach the yellow solid sediment with carrying out recrystallization with methyl alcohol again after the washing with alcohol and to obtain the Salen part, the Salen part is preserved in vacuum;
(2) preparation nickel-salen complex: the Salen part of 6.4mol is dissolved in the ethanolic solution of 50ml and forms solution C; The nickel acetate of 6.4mol is dissolved in the ethanolic solution of 50ml and forms solution D; Again solution C is dropwise dripped and form mixed solution in the solution D; Then mixed solution is obtained the red solid deposition at 40 ℃ of refluxed 2h, the red solid deposition is leached with methyl alcohol carry out obtaining nickel-salen complex behind the recrystallization, with the vacuum preservation at room temperature of nickel-salen complex;
(3) preparation electrochemical sensor: is 0.071cm with nickel-salen complex at area
2Platinum electrode on cause polymerization through electricity, thereby obtain electrochemical sensor.
It is to be with 100mVs in the mixed solution of acetonitrile, the high oronain of the tetrabutyl of 0.1mol/L in concentration that described electricity causes polymerization
-1Speed in the voltage range of 0～1.4V (contrast saturated calomel electrode), carry out polyreaction four times with cyclic voltammetry.
The prepared sensor of the present invention has high sensitivity and stability, and low-work voltage is easy and cost is low, has using value preferably at the detection range of dissolved oxygen DO.
Claims (2)
1. one kind is used for the electrochemical sensor preparation method that dissolved oxygen DO detects, and it is characterized in that: step is following:
(1) preparation salen part: the salicylide (salicylaldehyde) of 0.284mol is dissolved in the 50ml ethanol forms solution A; The ethylenediamine of 0.142mol is dissolved in the 25ml ethanol forms solution B; And then with solution A and solution B mixing formation mixed solution; The mixed solution that forms obtains the yellow solid sediment at 40 ℃ of following stirring and refluxing 2h; Leach the yellow solid sediment with carrying out recrystallization with methyl alcohol again after the washing with alcohol and to obtain the Salen part, the Salen part is preserved in vacuum;
(2) preparation nickel-salen complex: the Salen part of 6.4mol is dissolved in the ethanolic solution of 50ml and forms solution C; The nickel acetate of 6.4mol is dissolved in the ethanolic solution of 50ml and forms solution D; Again solution C is dropwise dripped and form mixed solution in the solution D; Then mixed solution is obtained the red solid deposition at 40 ℃ of refluxed 2h, the red solid deposition is leached with methyl alcohol carry out obtaining nickel-salen complex behind the recrystallization, with the vacuum preservation at room temperature of nickel-salen complex;
(3) preparation electrochemical sensor: is 0.071cm with nickel-salen complex at area
2Platinum electrode on cause polymerization through electricity, thereby obtain electrochemical sensor.
2. according to the said a kind of electrochemical sensor preparation method that dissolved oxygen DO detects that is used for of claim 1, it is characterized in that: it is to be with 100mVs in the mixed solution of acetonitrile, the high oronain of the tetrabutyl of 0.1mol/L in concentration that described electricity causes polymerization
-1Speed in the voltage range of 0～1.4V, carry out polyreaction four times with cyclic voltammetry.
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| CN2012100916729A CN102645470A (en) | 2012-03-31 | 2012-03-31 | Preparation method of electrochemical sensor for dissolved oxygen detection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106660785A (en) * | 2013-11-01 | 2017-05-10 | 田纳西大学研究基金会 | Reversible bifunctional air electrode catalyst |
| CN108103523A (en) * | 2017-12-07 | 2018-06-01 | 湖北文理学院 | The preparation method of Ni-Salen complexs and Ni-Salen complexs |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101042365A (en) * | 2007-04-11 | 2007-09-26 | 浙江大学 | Dissolved oxygen electrochemical sensor |
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2012
- 2012-03-31 CN CN2012100916729A patent/CN102645470A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101042365A (en) * | 2007-04-11 | 2007-09-26 | 浙江大学 | Dissolved oxygen electrochemical sensor |
Non-Patent Citations (1)
| Title |
|---|
| CIBELY S. MARTIN等: ""Development of an electrochemical sensor for determination of dissolved oxygen by nickel–salen polymeric film modified electrode"", 《SENSORS AND ACTUATORS B: CHEMICAL》, 16 January 2012 (2012-01-16) * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106660785A (en) * | 2013-11-01 | 2017-05-10 | 田纳西大学研究基金会 | Reversible bifunctional air electrode catalyst |
| CN106660785B (en) * | 2013-11-01 | 2019-06-14 | 田纳西大学研究基金会 | It is a kind of for bielectron, the catalyst of reversible redox reactions |
| US10522842B2 (en) | 2013-11-01 | 2019-12-31 | University Of Tennessee Research Foundation | Reversible bifunctional air electrode catalyst for rechargeable metal air battery and regenerative fuel cell |
| US11031606B2 (en) | 2013-11-01 | 2021-06-08 | University Of Tennessee Research Foundation | Reversible bifunctional air electrode catalyst for rechargeable metal air battery and regenerative fuel cell |
| CN108103523A (en) * | 2017-12-07 | 2018-06-01 | 湖北文理学院 | The preparation method of Ni-Salen complexs and Ni-Salen complexs |
| CN108103523B (en) * | 2017-12-07 | 2019-06-25 | 湖北文理学院 | The preparation method and Ni-Salen complex of Ni-Salen complex |
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Application publication date: 20120822 |