CN102507710B - Electrochemical method for rapidly detecting trace polychlorinated biphenyl - Google Patents
Electrochemical method for rapidly detecting trace polychlorinated biphenyl Download PDFInfo
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Abstract
The invention discloses an electrochemical method for rapidly detecting trace polychlorinated biphenyl, which mainly comprises preparing a seed crystal layer, performing electrochemical deposition and performing cyclic voltammetry scan. The method has easy operation, simple apparatus and low cost, and only needs to connect a silver nanoelectrode with an electrochemical workstation to form a loop in an electrolyte containing polychlorinated biphenyl, which realizes rapid, accurate and high-performance detection of trace persistent organic pollutants in environment.
Description
Technical field
A kind of pervasive electrochemical redox method of the present invention is specifically related to the electrochemical method of a kind of trace, fast detecting polychlorinated biphenyl.
Background technology
Defectives such as environmental problem more and more causes people's extensive concern, and methods such as liquid chromatography, fluoroscopic examination are adopted in the testing of the persistence organic pollutant in the environment all the time, but all has the cost costliness, and detection time is long.Cyclic voltammetry curve scanning in the electrochemical detection method is simple fast, has aspect chemical detection very widely always and uses.For a long time, people are devoted to update its accuracy of detection, accuracy and improve the work that mechanism is annotated that detects.Working electrode has very important Research Significance as the carrier of electrochemical reaction for improving precision, accuracy and further understanding reaction mechanism.People successively probe into various metal electrodes as the detection performance of working electrode, but the effect of these metals is subjected to the restriction of bulk factor.Along with the rise of nanometer technology, the preparation of nano material is very ripe, the excellent properties that utilizes nano material for probe into fast, accurately, efficient detection method is significant.Simultaneously, adopt the electrochemical detection method of nano material for widening the nanometer technology application and promoting the development of pollutant detection technique that new opportunity is provided.
The present invention is intended to develop a kind of simple, with low cost, method that can realize pollutant in the environment is carried out trace detection fast of operating, and has also widened the range of application of nano material simultaneously.Based on electrochemical workstation, utilize silver nanoparticle electrode that prepared by electrodeposition forms as working electrode, form the loop in electrolytic solution, room temperature following a few minutes can be finished repeatedly the cyclic voltammetry curve sweep test of pcb molecule, thus the peak signal of meeting with a response.By voltage range, the sweep velocity of change detection, and the direction of scanning, can obtain to react the relevant information of how to carry out, judge its reaction mechanism effectively.
Summary of the invention
In order to solve the deficiencies in the prior art, the object of the present invention is to provide the electrochemical method of a kind of trace, fast detecting polychlorinated biphenyl, realized fast, accurately, organic micro-pollutant in the efficient detection environment.
The present invention adopts following technical scheme to achieve these goals:
The electrochemical method of trace, fast detecting polychlorinated biphenyl is characterized in that may further comprise the steps:
(1) preparation of inculating crystal layer: with 0.5 ml, 55-65 mM silver nitrate and 1 ml, 30-40 mM sodium citrate injects 95-105 ml deionized water, stirs rapidly 2-3 minute, again with 0.5 ml, 0.015-0.025 the M sodium borohydride injects above solution, stirred 8-12 minute, and at room temperature aging 15-25 hour, utilized the spin coating instrument, be that the seed crystal colloidal solution of 10 μ L is spin-coated on the clean ITO substrate with volume, the area of spin coating is 1 cm
2About, put into baking oven, 35-45 ℃ of evaporation down, only seed crystal is stayed on the ITO substrate;
(2) electrochemical deposition growth: 0.04-0.06 g silver nitrate and 0.23-0.28 g polyvinylpyrrolidone are dissolved in the 45-55 ml deionized water, stirring is up to dissolving fully, with this solution as electrolytic solution, in electrochemical deposition process, to scribble the ITO substrate of seed crystal as negative electrode, graphite flake adopts the pattern of continuous current to carry out electrochemical deposition as anode, and current density is 5 μ A/cm
2, the time of deposition is 9-11 hour, sample takes out from electrolytic solution, rinses well with deionized water, dries up with nitrogen;
(3) cyclic voltammetry curve sweep test:
A: electrolytic solution is formed: solvent is dimethyl formamide, and supporting electrolyte is 0.1 M tetrabutylammonium perchlorate,, active substance is 5 * 10
4M 3, and 3 ', 4,4 '-tetrachloro biphenyl;
B: circuit connects: the silver nanoparticle electrode is as working electrode, and saturated silver/silver chloride electrode is as contrast electrode, and the platinized platinum electrode is as to electrode, immerses respectively in the electrolytic solution and with electrochemical workstation to link to each other;
C: direction of scanning: in the solution of trace, measure to voltage max again to the voltage minimum from voltage max; Sweep velocity: 100 mV/s.
The present invention is with the polychlorinated biphenyl of silver nanoparticle electrode for detection of trace in the liquid, and based on nano material good adsorption performance, the enrichment electrode surface participates in the pcb molecule of electrooxidation reduction greatly, thereby reaches the purpose that detects the low concentration bioactive molecule.
Beneficial effect of the present invention:
Preparation method of the present invention is easy to operate, equipment is simple, with low cost, only need the silver nanoparticle electrode to link to each other with electrochemical workstation, to form the loop in containing the electrolytic solution of polychlorinated biphenyl can detect, this detection method realized fast, accurately, the persistence organic pollutant of trace in the efficient detection environment.
Description of drawings
The synoptic diagram of Fig. 1 proving installation of the present invention.
Fig. 2 the present invention is by a kind of silver nanoparticle electrode of pervasive electrochemical deposition method preparation.
Fig. 3 silver nanoparticle electrode carries out the collection of illustrative plates of cyclic voltammetry scan test as the electrolytic solution of solvent to dimethyl formamide as working electrode.
Fig. 4 contains 0.1M supporting electrolyte and 500 ppm 3,3 ', 4, the electrolytic solution of 4 '-tetrachloro biphenyl (PCB77), the cyclic voltammetry scan test collection of illustrative plates that the silver nanoparticle electrode is tested.
Fig. 5 contains 0.1 M supporting electrolyte and 5 ppm 3,3 ', 4, the electrolytic solution of 4 '-tetrachloro biphenyl (PCB77), the cyclic voltammetry scan test collection of illustrative plates that the silver nanoparticle electrode is tested.
Embodiment
Embodiment 1:As shown in Figure 1, the silver nanoparticle electrode is as working electrode, the conduct of platinized platinum electrode is to electrode, saturated silver/silver chloride electrode is as contrast electrode, three electrodes all part immerse in the electrolytic solution, and wherein working electrode is with relative and put to electrode, and contrast electrode places the centre, while three electrodes link to each other with electrochemical workstation respectively and form the loop, can test.Electrochemical workstation is linked to each other with computing machine, and relevant test data can show on computers.The colloidal solution that Fig. 2 at first prepares silver nano-grain is spin-coated on the ITO substrate with the spin coating instrument, after 40 ℃ are heated down, will stay silver-colored particle seed crystal at substrate, and then in the electrolytic solution that contains silver ion of configuration, carry out electro-deposition, ITO substrate top surface as negative electrode has been assembled silver ion under electric field action, progressively form the flake nano structure, formed the silver nanoparticle electrode.The direction of scanning of Fig. 3: voltage max → voltage minimum → voltage max; Sweep velocity: 100 mV/s.The blank comparative solution that only contains 0.1 M supporting electrolyte (tetrabutylammonium perchlorate) in the above-mentioned solvent, the silver nanoparticle electrode test collection of illustrative plates in this solution does not demonstrate any redox peak.Fig. 4 is for containing 0.1M supporting electrolyte and 500 ppm 3,3 ', 4, the electrolytic solution of 4 '-tetrachloro biphenyl (PCB77), the cyclic voltammetry scan test collection of illustrative plates that the silver nanoparticle electrode is tested demonstrates a plurality of reduction peak, by containing 0.1 M supporting electrolyte and 5 ppm 3 with Fig. 5,3 ', 4, the electrolytic solution of 4 '-tetrachloro biphenyl (PCB77), the contrast of two collection of illustrative plates of cyclic voltammetry scan that the silver nanoparticle electrode is tested test collection of illustrative plates can well detect PCB77 molecule in the solution with the method.
Embodiment 2:The electrochemical method of trace, fast detecting polychlorinated biphenyl may further comprise the steps:
(1) preparation of inculating crystal layer: with 0.5 ml, 59 mM silver nitrates and 1 ml, 34 mM sodium citrates inject 98 ml deionized waters, stir rapidly 2 minutes, again with 0.5 ml, 0.02 the M sodium borohydride injects above solution, stirred 10 minutes, and at room temperature aging 20 hours, utilized the spin coating instrument, be that the seed crystal colloidal solution of 10 μ L is spin-coated on the clean ITO substrate with volume, the area of spin coating is 1 cm
2, put into baking oven, 40 ℃ of evaporations down, only seed crystal is stayed on the ITO substrate;
(2) electrochemical deposition growth: 0.05 g silver nitrate and 0.25 g polyvinylpyrrolidone are dissolved in the 50ml deionized water, stirring is up to dissolving fully, with this solution as electrolytic solution, in electrochemical deposition process, to scribble the ITO substrate of seed crystal as negative electrode, graphite flake adopts the pattern of continuous current to carry out electrochemical deposition as anode, and current density is 5 μ A/cm
2, the time of deposition is 10 hours, sample takes out from electrolytic solution, rinses well with deionized water, dries up with nitrogen;
(3) cyclic voltammetry curve sweep test:
A: electrolytic solution is formed: solvent is dimethyl formamide, and supporting electrolyte is 0.1 M tetrabutylammonium perchlorate,, active substance is 5 * 10
4M 3, and 3 ', 4,4 '-tetrachloro biphenyl;
B: circuit connects: the silver nanoparticle electrode is as working electrode, and saturated silver/silver chloride electrode is as contrast electrode, and the platinized platinum electrode is as to electrode, immerses respectively in the electrolytic solution and with electrochemical workstation to link to each other;
C: direction of scanning: in the solution of trace, measure to voltage max again to the voltage minimum from voltage max; Sweep velocity: 100 mV/s.
Claims (1)
1. fast detection of trace 3,3 ', 4, the electrochemical method of 4 '-tetrachloro biphenyl is characterized in that may further comprise the steps:
(1) preparation of inculating crystal layer: with 0.5 ml, 55-65 mM silver nitrate and 1 ml, 30-40 mM sodium citrate injects 95-105 ml deionized water, stirs rapidly 2-3 minute, again with 0.5 ml, 0.015-0.025 the M sodium borohydride injects above solution, stirred 8-12 minute, and at room temperature aging 15-25 hour, utilized the spin coating instrument, be that the seed crystal colloidal solution of 10 μ L is spin-coated on the clean ITO substrate with volume, the area of spin coating is 1 cm
2About, put into baking oven, 35-45 ℃ of evaporation down, only seed crystal is stayed on the ITO substrate;
(2) electrochemical deposition growth: 0.04-0.06 g silver nitrate and 0.23-0.28 g polyvinylpyrrolidone are dissolved in the 45-55 ml deionized water, stirring is up to dissolving fully, with this solution as electrolytic solution, in electrochemical deposition process, to scribble the ITO substrate of seed crystal as negative electrode, graphite flake adopts the pattern of continuous current to carry out electrochemical deposition as anode, and current density is 5 μ A/cm
2, the time of deposition is 9-11 hour, sample takes out from electrolytic solution, rinses well with deionized water, dries up with nitrogen, obtains the silver nanoparticle electrode with flake nano silver structure;
(3) cyclic voltammetry curve sweep test:
A: electrolytic solution is formed: solvent is dimethyl formamide, and supporting electrolyte is 0.1 M tetrabutylammonium perchlorate, and active substance is 5 * 10
4M 3, and 3 ', 4,4 '-tetrachloro biphenyl;
B: circuit connects: the silver nanoparticle electrode is as working electrode, and saturated silver/silver chloride electrode is as contrast electrode, and the platinized platinum electrode is as to electrode, immerses respectively in the electrolytic solution and with electrochemical workstation to link to each other;
C: direction of scanning: containing trace 3,3 ', 4, in the electrolytic solution of 4 '-tetrachloro biphenyl, measure to the mode of voltage max again to the voltage minimum from voltage max; Sweep velocity: 100 mV/s.
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