CN100585392C - Silk screen printing electrode and producing process, and sensor and detecting method - Google Patents
Silk screen printing electrode and producing process, and sensor and detecting method Download PDFInfo
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- CN100585392C CN100585392C CN200710067411A CN200710067411A CN100585392C CN 100585392 C CN100585392 C CN 100585392C CN 200710067411 A CN200710067411 A CN 200710067411A CN 200710067411 A CN200710067411 A CN 200710067411A CN 100585392 C CN100585392 C CN 100585392C
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Abstract
A screen printing electrode contains a substrate printed electrode, external insulating layer printed on substrate and at least two electrode leading wires. It is characterized in that there are three electrodes printed on substrate, including a gold electrode, a carbon electrode and an Ag/AgCl electrode. Each electrode connects a leading wire correspondingly. Its manufacturing technology is: Firstly, select substrate, clean and drying for heat resisting. Then, print electrode leading wires, drying substrate. Print carbon electrode using carbon slurry and drying, Ag/AgCl electrode using Ag/AgCl slurry and drying in turn. Finally, utilize photofixation insulating slurry to print electrode standard layer and solidify it by ultraviolet light. The invention has simple electrode construction, convenient processing method and low cost. Sensor testing method depending on this electrode has convenient operation and high sensitivity.
Description
Technical field
But what the present invention relates to is the method that the sensor made of the screen printing electrode of content of beary metal in a kind of fast detecting water and preparation technology and screen printing electrode and sensor are used to detect content of heavy metal lead, belongs to technical field of analytical instruments.
Background technology
Plumbous (Pb2+) is a kind of harmful heavy metal ion that occurring in nature exists, and people's nervous system, digestive system, hematopoietic function and male reproductive system etc. are all had harm, especially endangers the children that brain is in the stage of development.For this reason, the Pb2+ content in World Health Organization's regulation water can not surpass 10 μ g/L.The assay method of Pb2+ has dithizone colorimetric method, atomic absorption method, plasma mass and electrochemical method etc.; Wherein sensitive with mass spectroscopy, detectability can reach 1.0 * 10-3 μ g/L, the detection limit of flame atomic absorption method can reach 1.0 μ g/L, the sensitivity of galvanochemistry leaching is between atomic absorption method and mass spectroscopy, and instrument is easy to miniaturization, easy and simple to handle, be applicable to that field condition detects the toxic heavy metal ion, so this method is noticeable day by day.
The high sensitivity of stripping volt-ampere analysis is to come from the inrichment of trace-metal at working electrode surface, adopts suitable scan method, and the stripping volt-ampere analysis not only can provide heavy metal concentration, chemical form that also can analysis heavy metal.In recent years, the stripping volt-ampere analysis is comparatively fast being developed aspect the measurement of heavy metal, and new sensor technology has substituted traditional dropping-mercury electrode, has exempted steps such as deoxygenation, and handheld stripping voltammetric analyzer has also obtained rapid commercialization.Wherein, the mercury film electrode leaching is one of the most effective survey Pb2+ method, but because mercury has environmental toxicity, the researchist has adopted golden film, silverskin, platinum film and carbon film modified electrode to come the replacement for mercury membrane electrode.
In the practical application of electrochemical sensor, because the complicacy of actual sample, sensor exist the phenomenon of " electrode poisoning ", the surface of sensor is damaged easily, therefore, generally study disposable sensor in recent years to eliminate the pollution of testing process for electrode itself.
Summary of the invention
The objective of the invention is to overcome the deficiency that above-mentioned prior art exists, and a kind of simple in structure, easy to operate, cost is low and detection sensitivity is high screen printing electrode and preparation technology and sensor and detection method are provided.It is a kind of electrode, kind electrode adopts the silk-screen printing technique preparation, drink the analysis of differential pulse anodic stripping voltammetry, can the fast detecting underwater trace plumbous Pb, the heavy metal pollution fast monitored that can be used for lake, reservoir, river, Sewage Plant etc. also can be used for the fast detecting of heavy-metal residuals such as vegetables, blood lead.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of screen printing electrode, comprise external insulation and at least two contact conductors of printing on the substrate, substrate of a printed electrode, also be printed with three electrodes on the described substrate, be respectively a gold electrode, a carbon electrode and an Ag/AgCl electrode, each electrode pair should be connected with a contact conductor.
Also be printed with an electrode standard layer on the described substrate, this layer is between electrode and insulation course.
A kind of preparation technology of screen printing electrode as mentioned above is: at first choose substrate cleaning and dry heat-resisting; Printed electrode goes between then; Then dry substrate, successively with the carbon paste slurry print carbon electrode and oven dry, the Ag/AgCl paste is printed Ag/AgCl electrode and oven dry and gold paste material and is printed gold electrode and oven dry; Then adopt light to insulate admittedly again and starch printed electrode standard layer and use ultraviolet light polymerization; Adopt light to insulate admittedly at last and starch the printed electrode insulation course and use ultraviolet light polymerization.
In the described gold electrode printing process, bake out temperature is the 60-80 degree, and time 15-30 minute, in carbon electrode and the Ag/AgCl electrode printing process, bake out temperature was the 100-150 degree, time 8-15 minute.
Described gold electrode is printed process, and bake out temperature is 70 degree, and 20 minutes time, in carbon electrode and the Ag/AgCl electrode printing process, bake out temperature is 120 degree, 10 minutes time.
A kind of employing is the sensor made of screen printing electrode as mentioned above, which comprises at least a screen printing electrode and an external structure, and screen printing electrode is fixedlyed connected with external structure, print electrode and external structure between be provided with a T type and detect cavity.
Described external structure is to be fixed on the stiffening plate of screen printing electrode one side and the loam cake and the bracing frame of opposite side, and described T type cavity is arranged on the bracing frame.
A kind of utilization sensor as mentioned above is used to detect the method for content of heavy metal lead, adopts the square wave volt-ampere analysis, at first, described sensor is linked to each other with electrochemical analytical instrument; Secondly, will originally in the 5mL test tube, mix formation for test sample and detect solution with 0.1M HCl; At last, solution is immersed in the sensor electrode lower end and begin the square wave volt-ampere analysis.
The blending ratio of described detection solution is: 0.8-1ml for test sample this, the deionized water of 3-5ml and the HCL solution of 5ml0.1M; Described square wave voltammetry analytical parameters is: burning voltage+0.5V 30 is wonderful, and accumulating potential-0.5V 120 is wonderful, and equilibration time 30 is wonderful, square wave amplitude 28mV, current potential step value 3mV, frequency 15Hz, operating potential window :-0.5-+0.2V.
The present invention compared with prior art, it is simple in structure to have a screen printing electrode, simple and convenient processing method, cost are low, characteristics such as, detection sensitivity height easy to operate with the sensor detecting method that this screen printing electrode is made.
Description of drawings
Fig. 1 is a screen printing electrode structural representation of the present invention
Fig. 2 is the structural representation of the sensor made of screen printing electrode of the present invention
Embodiment
The present invention will be described in detail below in conjunction with accompanying drawing: as shown in Figure 1, screen printing electrode of the present invention, comprise external insulation 2 and at least 2 contact conductors 1 of printing on the substrate 7, substrate of a printed electrode, also be printed with 3 electrodes on the described substrate, be respectively: gold electrode 4, a carbon electrode 5 and an Ag/AgCl electrode 6, each electrode pair should be connected with a contact conductor, also be printed with an electrode standard layer 3 on the described substrate, this layer is between electrode and insulation course.
The processing technology of described screen printing electrode is: at first choose substrate 7 cleanings and dry heat-resisting, substrate is the PET substrate; The printed electrode lead-in wire 1 then; Then dry substrate 7, print carbon electrode 5 and oven dry with the carbon paste slurry successively, bake out temperature is the 100-150 degree, time 8-15 minute, the 6 also oven dry of Ag/AgCl paste printing Ag/AgCl electrode, bake out temperature is the 100-150 degree, and time 8-15 minute, the gold paste material was printed gold electrode 4 and oven dry, bake out temperature is the 60-80 degree, time 15-30 minute; Then adopt light to insulate admittedly again and starch printed electrode standard layer 3 and use ultraviolet light polymerization; Adopt light to insulate admittedly at last and starch printed electrode insulation course 2 and use ultraviolet light polymerization.
In order to reach best drying effect, described gold electrode 4 printing processes, bake out temperature is 70 degree, 20 minutes time, carbon electrode (5) and Ag/AgCl electrode 6 printing processes, bake out temperature is 120 degree, 10 minutes time.
As shown in Figure 2, the sensor made from screen printing electrode, which comprises at least a screen printing electrode 10 and an external structure, screen printing electrode 10 adopts adhesive to be connected with external structure, print electrode 10 and external structure between a T type be set detect cavity 12, described external structure is to be fixed on the stiffening plate 11 of screen printing electrode one side and the loam cake 8 and the bracing frame 9 of opposite side, and described T type cavity 12 is arranged on the bracing frame 9.
Sensor of the present invention is used to detect the method for content of heavy metal lead, adopts the square wave volt-ampere analysis, at first, described sensor is linked to each other with electrochemical analytical instrument; Secondly, will be for test sample this in the 5mL test tube, mix to form with 0.1M HCl and detect solution, the blending ratio of solution is: 0.8-1ml for test sample originally, the deionized water of 3-5ml and the HCL solution of 5ml0.1M; At last, solution is immersed in the sensor electrode lower end begin the square wave volt-ampere analysis, the voltammetry analytical parameters is: burning voltage+0.5V 30 is wonderful, accumulating potential-0.5V 120 is wonderful, equilibration time 30 is wonderful, square wave amplitude 28mV, current potential step value 3mV, frequency 15Hz, operating potential window :-0.5-+0.2V.
Embodiment: detect the Pb in the mark-on sample in the tap water
Adopt CHI660A electrochemical analyser (CHI company), wherein the carbon electrode slurry is Japanese Jujo, and gold paste material, AgCl and insulation paste are Acheson, and the PET substrate is from Lekai, Baoding photographic film plant.Get Jiaxing Area water sample from the beginning, a series of mark-on solution of preparation 0～30 * 10-6g/LPb ion.According to the method for the invention, detect test, can obtain as the square wave volt-ampere curve in figure below, the Pb ion concentration is demarcated, and reads-peak current during the 0.24V current potential, and the Pb ion concentration adopts formula: C=A * I, and wherein I is an electric current 10
-6A, C are plumbum ion concentrations, unit 10
-6G/L.A is a calibration factor,
Representative value is 0.01.
The result shows, is 0～50 * 10 between this method linear zone
-6G/L, sensitivity 0.08A/g L-1, accuracy of detection 0.5 * 10
-6G/L.To 10 * 10
-6G/L carries out revision test 10 times, shows that error is less than 10%.
Claims (6)
1, a kind of screen printing electrode, comprise external insulation and at least two contact conductors of printing on the substrate, substrate of a printed electrode, it is characterized in that also being printed with on the described substrate (7) three electrodes, be respectively a gold electrode (4), a carbon electrode (5) and an Ag/AgCl electrode (6), each electrode pair should be connected with a contact conductor; Also be printed with an electrode standard layer (3) on the described substrate (7), this layer is between electrode and insulation course.
2, a kind of preparation technology of screen printing electrode as claimed in claim 1 is characterized in that: at first choose substrate (7) cleaning and dry heat-resisting; Printed electrode lead-in wire (1) then; Then dry substrate (7), print carbon electrode (5) and oven dry, Ag/AgCl paste with the carbon paste slurry successively and print Ag/AgCl electrode (6) and oven dry and gold paste material and print gold electrode (4) and dry; Then adopt light to insulate admittedly again and starch printed electrode standard layer (3) and use ultraviolet light polymerization; Adopt light to insulate admittedly at last and starch printed electrode insulation course (2) and use ultraviolet light polymerization.
3, the preparation technology of screen printing electrode according to claim 2, it is characterized in that described gold electrode (4) printing process, bake out temperature is the 60-80 degree, time 15-30 minute, carbon electrode (5) and Ag/AgCl electrode (6) printing process, bake out temperature is the 100-150 degree, time 8-15 minute.
4, the preparation technology of screen printing electrode according to claim 3 is characterized in that described gold electrode (4) printing process, and bake out temperature is 70 degree, 20 minutes time, carbon electrode (5) and Ag/AgCl electrode (6) printing process, bake out temperature are 120 degree, 10 minutes time.
5, a kind of sensor made from the described screen printing electrode of claim 1 is used to detect the method for content of heavy metal lead, described sensor comprises a screen printing electrode (10) and an external structure at least, screen printing electrode (10) is fixedlyed connected with external structure, and the T type that is provided with between (10) and the external structure detects cavity (12) printing electrode; Described external structure is the stiffening plate (11) that is fixed on screen printing electrode one side and the loam cake (8) and the bracing frame (9) of opposite side, and described T type cavity (12) is arranged on the bracing frame (9); It is characterized in that described method is: it adopts the square wave volt-ampere analysis, at first, described sensor is linked to each other with electrochemical analytical instrument; Secondly, sample to be tested is mixed formation with 0.1M HCl in the 5mL test tube and detect solution; At last, solution is immersed in the sensor electrode lower end and begin the square wave volt-ampere analysis.
6, the sensor made from screen printing electrode according to claim 5 is used to detect the method for content of heavy metal lead, it is characterized in that the blending ratio of described detection solution is: the HCl solution of the sample to be tested of 0.8-1ml, the deionized water of 3-5ml and 5ml0.1M; Described square wave voltammetry analytical parameters is: burning voltage+0.5V 30 seconds, accumulating potential-0.5V 120 seconds, equilibration time 30 seconds, square wave amplitude 28mV, current potential step value 3mV, frequency 15Hz, operating potential window :-0.5-+0.2V.
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| CN200710067411A CN100585392C (en) | 2007-03-01 | 2007-03-01 | Silk screen printing electrode and producing process, and sensor and detecting method |
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Cited By (1)
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| CN103402327A (en) * | 2013-08-07 | 2013-11-20 | 苏州扬清芯片科技有限公司 | Manufacturing method of printing electrode for portable heavy metal detection |
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| US8411413B2 (en) * | 2008-08-28 | 2013-04-02 | Ioxus, Inc. | High voltage EDLC cell and method for the manufacture thereof |
| CN101344501B (en) * | 2008-08-22 | 2011-10-05 | 中南大学 | Silk screen printing electrode, manufacturing technique and use thereof |
| CN101666772B (en) * | 2008-09-04 | 2013-06-05 | 北京金达清创环境科技有限公司 | Preparation method for screen printing cobalt sensor for detecting phosphate |
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| CN103207223B (en) * | 2012-11-23 | 2015-04-01 | 上海仪电科学仪器股份有限公司 | Manufacturing method of portable heavy metal meter printing electrode |
| CN103932676A (en) * | 2013-01-23 | 2014-07-23 | 四川锦江电子科技有限公司 | Flexible circuit electrode |
| CN103149255A (en) * | 2013-02-25 | 2013-06-12 | 长沙理工大学 | Method for quickly determining lead content in blood |
| CN115406946B (en) * | 2022-08-16 | 2023-06-30 | 山东卓越生物技术股份有限公司 | PO (potential of Hydrogen) of disposable instant detection card and sensor chip 2 Electrode preparation method |
| CN118067819A (en) * | 2024-04-17 | 2024-05-24 | 武汉千星铄金科技有限公司 | Method for simultaneously and rapidly detecting cadmium and lead in milk and dairy products |
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