CN203385693U - Heavy metal electrochemical sensor - Google Patents
Heavy metal electrochemical sensor Download PDFInfo
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- CN203385693U CN203385693U CN201320499856.9U CN201320499856U CN203385693U CN 203385693 U CN203385693 U CN 203385693U CN 201320499856 U CN201320499856 U CN 201320499856U CN 203385693 U CN203385693 U CN 203385693U
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Abstract
The utility model discloses a heavy metal electrochemical sensor which comprises a plate type conductor layer, a polymer conducting film and an adhesive tape layer, wherein the polymer conducting film is adhered to the plate type conductor layer, and the adhesive tape layer is adhered to the polymer conducting film. The heavy metal electrochemical sensor also comprises a solid-state counter electrode, a solid-state reference electrode, an insulated positioning piece and a paper filter. The polymer conducting film is completely covered by the adhesive tape layer; a round hole with the diameter of 3-5mm is formed in the adhesive tape layer; the solid-state counter electrode and the solid-state reference electrode are fixed on the adhesive tape layer through the insulated positioning piece and positioned at the edge position of the round hole; a bismuth film layer is coated on the surface of a polymer conducting film area at the round hole; the paper filter with the diameter of 5-7mm is adhered to the bismuth film; the diameter of the paper filter is 1-2mm larger than that of the round hole. The heavy metal electrochemical sensor is a disposable electrochemical sensor special for heavy metal detection and can independently or simultaneously detect multiple heavy metal ions, the detection noise is reduced, and the detection sensitivity is improved.
Description
Technical field
The utility model belongs to heavy metal Electrochemical Detection field, particularly relates to a kind of electrochemical sensor detected for heavy metal.
Background technology
Heavy metal refers generally to the metal that proportion is greater than 5, and wherein not human life activity institute is necessary as mercury, lead, cadmium etc. for most of heavy metal.If the content of beary metal in human body exceeds standard, easily cause slow poisoning, cause immune function of human body to reduce, bring out cancer, nervous centralis that even can harm people, cause great bodily injury to health.There is strict limiting the quantity of countries in the world to the content of beary metal in product.At field of Environment Protection, heavy metal is also one of material of greatest concern, and therefore the demand of relevant industries counterweight metal detection is very large at present.Conventional heavy metal detection method has atomic absorption method, inductively coupled plasma atomic emissions method, inductively coupled plasma mass spectrometry, x ray fluorescence spectrometry, By Naa, atomic fluorescence method, ultraviolet colourimetry, electrochemical process and Laser-induced Breakdown Spectroscopy method etc. at present.Yet wherein most of method all needs to use expensive large-scale analytical equipment, be not suitable for the Site Detection of heavy metal.With additive method, compare, electrochemical method in heavy metal detects, have apparatus structure simple, cheap, be easy to integrated and portability, the characteristics such as analysis time is short, sensitivity is high.Yet in the research of heavy metal electrochemical detection system, also there are some still unsolved difficult problems at present, restricting the application of Electrochemical Detection and popularizing.Wherein topmost have 2 points: 1) electrode (electrochemical sensor) needs complicated loaded down with trivial details preprocessing process, and poor reproducibility; 2) traditional electrolytic cell volume is larger, generally at least needs the solution of several ml volumes can carry out Electrochemical Detection, has affected the portability of whole electrochemical detection system.
In earlier stage, we have applied for patent of invention " flat working electrode and preparation method thereof ", application number is 2012104013181, this patented claim provides a kind of flat working electrode and preparation method thereof, has mainly solved that the electrochemical sensor pretreatment process is complicated, the problem of poor reproducibility.But the flat working electrode that above-mentioned patent provides can be used for various Electrochemical Detection, and the opening of application scope is very large, therefore, when detecting for heavy metal, sensitivity is low, and detectable heavy metal scope is little.
The utility model content
The technical problems to be solved in the utility model be to provide a kind of easy and simple to handle, be exclusively used in heavy metal detect, highly sensitive, can detect the heavy metal electrochemical sensor that the heavy metal scope is wide.
For solving the problems of the technologies described above, the utility model adopts following technical scheme:
One heavy metal species electrochemical sensor, comprise flat conductor layer, the conducting polymer film, adhesive tape layer, the conducting polymer film sticks on flat conductor layer, adhesive tape layer sticks on the conducting polymer film, also comprise solid-state to electrode, solid state reference electrode, the insulation keeper, filter paper, the complete overlie polymer conducting film of adhesive tape layer, have the circular hole that diameter is 3～5mm on adhesive tape layer, solid-state electrode and solid state reference electrode are fixed on adhesive tape layer by the insulation keeper, solid-state to electrode and solid state reference electrode the marginal position in circular hole, the conducting polymer diaphragm area surface at circular hole place is coated with one deck bismuth film, paste the filter paper that diameter is 5～7mm on the bismuth film, the diameter of filter paper is than the large 1～2mm of the diameter of circular hole.
The utility model heavy metal electrochemical sensor, wherein said conducting polymer film covers the area of flat conductor layer 1/3～1/2.
The utility model heavy metal electrochemical sensor, wherein said insulation keeper is selected plastic clip.
The utility model heavy metal electrochemical sensor, wherein said solid-state to electrode adopt Pt to electrode or Au to electrode, solid state reference electrode adopts the Ag/AgCl contrast electrode.
The utility model heavy metal electrochemical sensor, wherein said flat conductor layer 1 adopts ito glass, conductive metal sheet or graphite flake to make, and its width is 0.5cm～1cm, and length is 1.5cm～2.5cm.
The utility model heavy metal electrochemical sensor, for the disposable electrochemical sensor that is exclusively used in the heavy metal detection, its manufacturing process is simple, quick, can in common lab, complete, with low cost, can be detected individually or simultaneously contents of many kinds of heavy metal ion, only need the solution of micro updating to be detected, good portability, measurement result is accurately and reliably, the electrode perform region is circular, diameter is 3～5mm, has reduced effective electrode area, electrode perform region form symmetry, reduce detection noise, improved detection sensitivity.
Below in conjunction with accompanying drawing, heavy metal electrochemical sensor of the present utility model is described further.
The accompanying drawing explanation
The structural representation that Fig. 1 is the utility model heavy metal electrochemical sensor;
Fig. 2 be the utility model heavy metal electrochemical sensor omit contrast electrode, to the sectional view of electrode and plastic clip;
Fig. 3 is the electrochemical response collection of illustrative plates of variable concentrations standard solution on electrochemical sensor in embodiment 4;
The canonical plotting that Fig. 4 is Pb in embodiment 4;
Fig. 5 is the corresponding collection of illustrative plates of the galvanochemistry of variable concentrations standard solution on electrochemical sensor in embodiment 5;
The canonical plotting that Fig. 6 is Zn in embodiment 5;
The canonical plotting that Fig. 7 is Cd in embodiment 5;
The canonical plotting that Fig. 8 is Pb in embodiment 5;
Fig. 9 is the utility model heavy metal electrochemical sensor and previous " flat working electrode " the detection sensitivity curve comparison figure applied in embodiment 6.
Embodiment
As shown in Figure 1, 2, the utility model heavy metal electrochemical sensor comprises flat conductor layer 1, conducting polymer film 2, adhesive tape layer 3, solid-state to electrode 4, solid state reference electrode 5, insulation keeper 6, filter paper 7, conducting polymer film 2 sticks on flat conductor layer 1, conducting polymer film 2 covers the area of flat conductor layer 1/3～1/2, adhesive tape layer 3 sticks on conducting polymer film 2, the complete overlie polymer conducting film 2 of adhesive tape layer 3, have the circular hole that diameter is 3～5mm on adhesive tape layer 3, the conducting film zone that expose at the circular hole place is the electrode perform region.Solid-state electrode 4 and solid state reference electrode 5 are fixed on adhesive tape layer 3 by insulation keeper 6, solid-state to electrode 4 and solid state reference electrode 5 marginal position in circular hole.The conducting polymer diaphragm area surface at circular hole place is coated with one deck bismuth film 8, pastes the filter paper 7 that diameter is 5～7mm on bismuth film 8, and the diameter of filter paper 7 is than the large 1～2mm of the diameter of circular hole.
The method for making of the utility model heavy metal electrochemical sensor comprises the following steps:
(1) ito glass, conductive metal sheet or graphite flake being cut into to width is 0.5cm～1cm, and the rectangle lamella that length is 1.5cm～2.5cm, form flat conductor layer,
(2) the conducting polymer film is attached to an end of flat conductor layer, covers the area of flat conductor layer 1/3～1/2,
(3) with the card punch of external diameter 3～5mm, on adhesive tape, punch, then by tape sticker on the conducting polymer film, form adhesive tape layer, adhesive tape layer covers the conducting film zone fully, the conducting film zone that expose at the circular hole place is the electrode perform region,
(4) use the insulation keeper as plastic clip, by solid-state, electrode and solid state reference electrode be fixed on adhesive tape layer, make solid-state to electrode and solid state reference electrode the marginal position in circular hole,
(5) bismuth nitrate that is 20～100mM by 30～80 μ L concentration, containing 0.15mol/L trisodium citrate and 1.5moL/LHCl, pH1, drop in the circular hole place,-1.2V～-deposit 120s under the 1.0V condition, after deposition is good, with redistilled water, rinse, then dry up, on circular hole place plated surface one deck bismuth film
(6) the circular filter paper sheet that is 5～7mm by diameter is pasted on the bismuth film, and the diameter of filter paper is than the large 1～2mm of the diameter of circular hole.
The utility model heavy metal electrochemical sensor, be the disposable electrochemical sensor that heavy metal detects that is exclusively used in, can be to Pb,, the contents of many kinds of heavy metal ion such as Cd, Zn are detected.
(1) ito glass being cut into to width is 0.5cm, and the rectangle lamella that length is 1.5cm, form flat conductor layer,
(2) end at flat conductor layer by the carbonaceous conductive sticker, cover the area of flat conductor layer 1/3,
(3) punch on adhesive tape with the card punch of external diameter 3mm, then adhesive tape is attached on carbonaceous conductive glue, form adhesive tape layer, the complete coated carbon conducting resinl of adhesive tape layer, the carbonaceous conductive glue zone that expose at the circular hole place is the electrode perform region,
(4) use plastic clip, Pt be fixed on adhesive tape layer electrode and Ag/AgCl contrast electrode, make Pt to electrode and Ag/AgCl contrast electrode the marginal position in circular hole,
(5) bismuth nitrate that is 20mM by 30 μ L concentration, containing 0.15mol/L trisodium citrate and 1.5moL/L HCl, pH1, drop in the circular hole place, under-1.2V condition, deposit 120s, rinse with redistilled water after deposition is good, then dry up, on circular hole place plated surface one deck bismuth film
(6) the circular filter paper sheet that is 5mm by diameter is pasted on the bismuth film, makes heavy metal electrochemical sensor of the present utility model.Embodiment 2
(1) conductive metal sheet being cut into to width is 0.8cm, and the rectangle lamella that length is 2cm, form flat conductor layer,
(2) the polymkeric substance silver conductive film is attached to an end of flat conductor layer, covers the area of flat conductor layer 1/2,
(3) punch on adhesive tape with the card punch of external diameter 4mm, then adhesive tape is attached on the polymkeric substance silver conductive film, form adhesive tape layer, adhesive tape layer covers the conducting film zone fully, and the conducting film zone that expose at the circular hole place is the electrode perform region,
(4) use plastic clip, Au be fixed on adhesive tape layer electrode and Ag/AgCl contrast electrode, make Au to electrode and Ag/AgCl contrast electrode the marginal position in circular hole,
(5) bismuth nitrate that is 60mM by 70 μ L concentration, containing 0.15mol/L trisodium citrate and 1.5moL/L HCl, pH1, drop in the circular hole place, under-1.0V condition, deposit 120s, rinse with redistilled water after deposition is good, then dry up, on circular hole place plated surface one deck bismuth film
(6) the circular filter paper sheet that is 6mm by diameter is pasted on the bismuth film, makes heavy metal electrochemical sensor of the present utility model.Embodiment 3
(1) graphite flake being cut into to width is 1cm, and the rectangle lamella that length is 2.5cm, form flat conductor layer,
(2) end at flat conductor layer by the carbonaceous conductive sticker, cover the area of flat conductor layer 1/3,
(3) punch on adhesive tape with the card punch of external diameter 5mm, then adhesive tape is attached on carbonaceous conductive glue, form adhesive tape layer, the complete coated carbon conducting resinl of adhesive tape layer zone, the carbonaceous conductive glue zone that expose at the circular hole place is the electrode perform region,
(4) use plastic clip, Au be fixed on adhesive tape layer electrode and Ag/AgCl contrast electrode, make Au to electrode and Ag/AgCl contrast electrode the marginal position in circular hole,
(5) bismuth nitrate that is 100mM by 80 μ L concentration, containing 0.15mol/L trisodium citrate and 1.5moL/L HCl, pH1, drop in the circular hole place, under-1.1V condition, deposit 120s, rinse with redistilled water after deposition is good, then dry up, on circular hole place plated surface one deck bismuth film
(6) the circular filter paper sheet that is 7mm by diameter is pasted on the bismuth film, makes heavy metal electrochemical sensor of the present utility model.
The mensuration of trace lead ion in embodiment 4 solution
Specific implementation process is as follows:
(1) accurately prepare plumbum ion concentration and be respectively 20 μ g/L, 50 μ g/L, 100 μ g/L, 200 μ g/L, 300 μ g/L, 400 μ g/L, the standard solution of 500 μ g/L;
(2) electrochemical sensor embodiment 1 made and Electrochemical Detection main frame are (as electrochemical workstation, potentiostat, voltammetric analyzer etc.) connect, then drip above-mentioned 7 standard solution of 20 μ L on surface, electrode perform region, utilize stripping voltammetry to be detected the lead in solution, can obtain as the electrochemical signals curve in Fig. 3, the peak height of the electrochemical signals of its lead ion is relevant with plumbum ion concentration, exist two linear relationships between peak height and concentration, as shown in Figure 4: in 0 to 80 μ g/L concentration range, linear slope is 1.26nA/ (μ g/L), linear equation is Y=1.26X, related coefficient is 0.98, at 80 μ g/L, in 500 μ g/L concentration ranges, the linear gradient obtained is 3.16nA/ (μ g/L), and linear equation is Y=3.16X+45.2, and related coefficient is 0.98,
(3) drip 20 μ L testing sample solutions on surface, electrode perform region, utilize stripping voltammetry to be detected the lead ion in sample, the peak current that obtains electrochemical signals is 380nA, and it is 106 μ g/L that its substitution linear equation is obtained to concentration plumbous in this sample solution.
Reappearance as a result between different sensors: prepared respectively 20 heavy metal electrochemical sensors, according to the step of above-mentioned (1)～(3), the lead in sample has been measured, the detection error between different sensors is less than 10%.
In the time of trace lead in embodiment 5 solution, cadmium and zinc ion, measure
The electrochemical sensor that the utility model provides can be for measure the concentration of solution trace lead (Pb), cadmium (Cd) and zinc (Zn) ion simultaneously, and specific implementation process is as follows:
(1) accurately preparation lead, cadmium and zinc ion concentration are respectively 20 μ g/L, 50 μ g/L, 100 μ g/L, the standard solution of 200 μ g/L and 500 μ g/L;
(2) electrochemical sensor of embodiment 2 is connected with Electrochemical Detection main frame (as electrochemical workstation, potentiostat, voltammetric analyzer etc.), then drip above-mentioned 5 standard solution of 20 μ L on surface, electrode perform region, utilize stripping voltammetry to be detected the lead in solution, can obtain as the electrochemical signals curve in Fig. 5, the peak height of the electrochemical signals of each heavy metal ion is relevant with concentration of heavy metal ion.
As shown in Figure 6, in 0 to 500 μ g/L concentration range, linear equation is the μ A of Y(unit to the linear relationship of Zn)=the μ g/L of 0.192+0.0035X(unit), related coefficient is 0.98.
As shown in Figure 7, in 0 to 500 μ g/L concentration range, linear equation is Y=0.402+0.007X to the linear relationship of Cd, and related coefficient is 0.99.
As shown in Figure 8, in 0 to 500 μ g/L concentration range, linear equation is Y=0.227+0.0032X to the linear relationship of Pb, and related coefficient is 0.99.
(3) drip 20 μ L testing sample solutions on surface, electrode perform region, utilize stripping voltammetry to be detected the heavy metal ion in sample, the peak current that obtains Zn is 0.39 μ A, and the concentration that the linear equation of its substitution Zn is obtained to Zn in this sample solution is 56.6 μ g/L; The peak current that obtains Cd is 0.74 μ A, and the concentration that the linear equation of its substitution Cd is obtained to Cd in this sample solution is 48.3 μ g/L; The peak current that obtains Pb is 0.87 μ A, and the concentration that the linear equation of its substitution Pb is obtained to Pb in this sample solution is 200.9 μ g/L.
Reappearance as a result between different sensors: prepared respectively 20 heavy metal electrochemical sensors, according to the step of above-mentioned (1)～(3), the Pb in sample, Zn, Cd ion have been measured, the detection error between different sensors is less than 10%.Embodiment 6 the utility model heavy metal electrochemical sensors and previous " flat working electrode " detection sensitivity Comparative Examples of applying for
Adopt the heavy metal electrochemical sensor of above-described embodiment 3, having prepared the electrode zone area according to the method for " the flat working electrode " of application before is 25mm
2electrode, respectively lead, cadmium, the Zinc standard solution that concentration is all 100ug/L carried out to control experiment, its result as shown in Figure 9.
The testing result of the heavy metal electrochemical sensor that in Fig. 9, curve 1 provides for this patent, the testing result of " flat working electrode " that curve 2 is previous application.Can significantly find out, in curve 1, the signal peak of each heavy metal element is more sharp-pointed, and the electric current background value is lower, and curve is more level and smooth.Through calculating, the detection signal-to-noise ratio that obtains each heavy metal element in curve 1 is respectively 22,43 and 20, and in curve 2, the detection signal-to-noise ratio of each heavy metal element is respectively 3.5,5.2 and 4.7.Therefore can find out, the sensitivity of the heavy metal electrochemical sensor detection that adopts the utility model to provide is significantly increased.
The utility model heavy metal electrochemical sensor, compare with the flat working electrode of previous application, has the following advantages:
(1) for the disposable electrochemical sensor that is exclusively used in the heavy metal detection, can be detected individually or simultaneously contents of many kinds of heavy metal ion, can be detected the heavy metal scope wide;
(2) plating bismuth better effects if, improved the reappearance as a result between different sensors, and measurement result is more reliable;
(3) the electrode perform region is circular, and diameter is 3～5mm, has reduced effective electrode area, and electrode perform region form symmetry, reduced detection noise, improved detection sensitivity.
Above-described embodiment is described preferred implementation of the present utility model; not scope of the present utility model is limited; under the prerequisite that does not break away from the utility model design spirit; various distortion and improvement that those of ordinary skills make the technical solution of the utility model, all should fall in the definite protection domain of the utility model claims.
Claims (5)
1. a heavy metal species electrochemical sensor, comprise flat conductor layer, the conducting polymer film, adhesive tape layer, the conducting polymer film sticks on flat conductor layer, adhesive tape layer sticks on the conducting polymer film, it is characterized in that: also comprise solid-state to electrode, solid state reference electrode, the insulation keeper, filter paper, the complete overlie polymer conducting film of adhesive tape layer, have the circular hole that diameter is 3～5mm on adhesive tape layer, solid-state electrode and solid state reference electrode are fixed on adhesive tape layer by the insulation keeper, solid-state to electrode and solid state reference electrode the marginal position in circular hole, the conducting polymer diaphragm area surface at circular hole place is coated with one deck bismuth film, paste the filter paper that diameter is 5～7mm on the bismuth film, the diameter of filter paper is than the large 1～2mm of the diameter of circular hole.
2. heavy metal electrochemical sensor according to claim 1, it is characterized in that: described conducting polymer film covers the area of flat conductor layer 1/3～1/2.
3. heavy metal electrochemical sensor according to claim 2, it is characterized in that: described insulation keeper is selected plastic clip.
4. heavy metal electrochemical sensor according to claim 3 is characterized in that: described solid-state to electrode adopt Pt to electrode or Au to electrode, solid state reference electrode adopts the Ag/AgCl contrast electrode.
5. heavy metal electrochemical sensor according to claim 4 is characterized in that: described flat conductor layer (1) adopts ito glass, conductive metal sheet or graphite flake to make, and its width is 0.5cm～1cm, and length is 1.5cm～2.5cm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103399067A (en) * | 2013-05-07 | 2013-11-20 | 中国检验检疫科学研究院 | Heavy-metal electrochemical sensor and manufacturing method thereof |
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| CN104713928A (en) * | 2015-04-03 | 2015-06-17 | 中国检验检疫科学研究院 | Hexavalent chromium electrochemical sensor as well as manufacturing method and application thereof |
| CN105466991B (en) * | 2015-12-30 | 2019-01-04 | 中国检验检疫科学研究院 | Bisphenol-A disposable paper base sensor and its preparation method and application |
| CN110887710A (en) * | 2019-11-08 | 2020-03-17 | 华中科技大学 | Sample preparation method for analyzing elements in water body based on laser-induced breakdown spectroscopy technology |
| CN112304859A (en) * | 2020-11-27 | 2021-02-02 | 四川福方医疗器械有限公司 | Electrochemical sensor for pollution detection and detection system |
| CN113862735B (en) * | 2021-09-24 | 2023-08-08 | 鲍宁 | Coating liquid, coating electrode, and preparation method and application of coating liquid |
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| CN101055262A (en) * | 2006-04-11 | 2007-10-17 | 禅谱科技股份有限公司 | Discard type electrochemical sensing test piece and its making process |
| US8128794B2 (en) * | 2007-05-16 | 2012-03-06 | Korea Atomic Energy Research Institute | Water pollution sensor for detecting heavy metal and method of manufacturing the same |
| CN101363812A (en) * | 2007-08-07 | 2009-02-11 | 华东师范大学 | Bismuth film electrode modified by Nafion and use thereof |
| CN101852761B (en) * | 2010-05-18 | 2013-04-17 | 浙江大学 | All-solid sodium ion selective electrode and preparation method thereof |
| CN102928487A (en) * | 2012-10-19 | 2013-02-13 | 中国检验检疫科学研究院 | Plate-type working electrode and method for manufacturing same |
| CN103399067B (en) * | 2013-05-07 | 2015-05-13 | 中国检验检疫科学研究院 | Heavy-metal electrochemical sensor and manufacturing method thereof |
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| CN103399067A (en) * | 2013-05-07 | 2013-11-20 | 中国检验检疫科学研究院 | Heavy-metal electrochemical sensor and manufacturing method thereof |
| CN103399067B (en) * | 2013-05-07 | 2015-05-13 | 中国检验检疫科学研究院 | Heavy-metal electrochemical sensor and manufacturing method thereof |
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