CN102262112A - Alloy electrode electrochemical sensor for detecting trace heavy metals - Google Patents
Alloy electrode electrochemical sensor for detecting trace heavy metals Download PDFInfo
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Abstract
The invention relates to the field of electrochemical sensors, and particularly relates to an alloy electrode electrochemical sensor for quickly detecting trace heavy metals. The electrochemical sensor specifically comprises an alloy working electrode, a reference electrode and an auxiliary electrode, wherein the working electrode, the reference electrode and the auxiliary electrode are respectively connected to a control potential rectifier by leads; and the working electrode is made of tin-bismuth alloy. The detection method is implemented by inserting the three electrodes into a sample to be detected, then detecting the concentration of heavy metal ions in the sample to be detected through stripping voltammetry. The electrochemical sensor provided by the invention is simple in process, low in cost, high in selectivity and sensitivity and good in stability, and can be widely applied to the quick field detection and daily monitoring of heavy metal ions in fresh water, sea water, food and body fluids.
Description
Technical field
The present invention relates to the electrochemical sensor field, a kind of specifically alloy electrode electrochemical sensor that is used to detect trace heavy metal.
Background technology
Along with the high speed development of modern industry and traffic, environment heavy metal pollution is serious day by day, has become an important social concern that influences human health and public security.Heavy metal element can be accumulated in human body, can cause harm such as anaemia, nervous function imbalance or injury of kidney.Along with people are more and more deep to the understanding of heavy metal harm, each state all adopts various measures and reduces the pollution of heavy metal, and accurately fast and effeciently measuring content of beary metal has become important content in the analytical approach research in recent years.
Measuring the content of beary metal main method at present is atomic absorption spectrography (AAS), atomic fluorescence spectrometry, ICP-AES, neutron activation analysis and galvanochemistry stripping voltammetry.Atomic absorption spectrography (AAS) is to measure a kind of important method of heavy metal concentration, be widely used in environmental monitoring and the Food Inspection as standard, but this method needs large-sized analytic instrument-Atomic Absorption Spectrometer, and determination step is many, and the time is long, and cost is higher.Same atomic fluorescence spectrometry, ICP-AES and neutron activation analysis also exist and need that large-scale instrument and equipment, monitoring velocity are slow, poor continuity, analysis cost is high and can't on-line monitoring etc. defective.The galvanochemistry stripping voltammetry has certain advantage than said method with advantages such as its instrument cost is cheap, easy to operate, standing charges are low, sensitivity height in the METHOD FOR CONTINUOUS DETERMINATION of heavy metal.Yet the preparation of recognition component-sensor is more loaded down with trivial details on the one hand, and the stability of sensor remains further to be improved on the other hand.
Mercury electrode is a kind of galvanochemistry stripping voltammetric sensor of superior performance, but mercury is poisonous, gos deep into it in the use that has been under an embargo of a lot of countries along with the reinforcement of environmental consciousness and research.Therefore the electrode material of replacement for mercury receives increasing concern.Bismuth can generate binary or multicomponent alloy with various heavy as a kind of environmentally friendly metallic element, and analytical performance and mercury are suitable, and background current is subjected to the influence of dissolved oxygen DO hardly, is generally believed it is a kind of environmental type electrode material of replacement for mercury.But aspects such as bismuth bar electrode of making based on bismuth metal and bismuth film electrode sensor production process complexity, testing process are easily oxidized, electrode stability and reappearance are demanded urgently improving, and detect at the scene and the application of instrumentation aspect so limited it.
Summary of the invention
The objective of the invention is to provides a kind of alloy electrode electrochemical sensor that is used for the trace heavy metal fast detecting simple, favorable reproducibility of making at above-mentioned weak point.
For achieving the above object, technical scheme provided by the invention is:
A kind of alloy electrode electrochemical sensor that is used to detect trace heavy metal comprises working electrode, contrast electrode and auxiliary electrode, the electrode of described alloy working electrode for being made by sn-bi alloy.
Described electrochemical sensor is the alloy working electrode; Working electrode, contrast electrode and auxiliary electrode one end insert and have in the detection cell of stirrer, and the other end is connected in the CONTROLLED POTENTIAL instrument by lead respectively; Described alloy working electrode is made by sn-bi alloy.
Described alloy working electrode can be sn-bi alloy disk electrode, sn-bi alloy post electrode or sn-bi alloy and prints electrode.
Described sn-bi alloy disk electrode is a sn-bi alloy silk outside surface sealed inert insulated enclosure material structure, and wherein the sn-bi alloy silk other end is drawn by lead-in wire; Described inertia insulated enclosure material can be teflon, Ke1-F, AB glue or glass bushing.
Described sn-bi alloy post electrode is a sn-bi alloy silk outside surface sealed inert insulated enclosure material structure, and an end of sn-bi alloy silk is passed by an end face of inertia insulated enclosure material, and the other end is drawn by lead-in wire.
Described sn-bi alloy print electrode into Polyvinylchloride as electrode basement, on electrode basement, be printed with the conductive silver glue-line, on the conductive silver glue-line, be printed with the sn-bi alloy layer, be printed with insulation course on the sn-bi alloy layer; Have preformed hole on the described insulation course, the sn-bi alloy layer that is exposed by this preformed hole is the useful area of working electrode; Be connected with contact conductor on the described conductive silver glue-line.
The trace heavy metal of described mensuration is cadmium, zinc, chromium, cobalt, nickel, gallium or thallium.The advantage that the present invention had: make simple, with low cost, good stability, favorable reproducibility, can use in applications such as environmental monitoring, food security and clinical detection.
The present invention adopts sn-bi alloy to be made into working electrode, and stable in properties can directly be measured, and need not any modification step, makes simply, and is with low cost, and reliable and stable; It has good electrochemical to heavy metal ion simultaneously, can form binary or multicomponent alloy with tested metallic ion, and analytical performance and mercury are suitable; Background current is subjected to the influence of dissolved oxygen DO hardly, and detected solution need not letting nitrogen in and deoxidizing, has avoided the loaded down with trivial details step in some actual measurements, more helps the demand of field quick detection.
Sn-bi alloy electrode stripping voltammetric sensor of the present invention can be measured 56 times in solution continuously at least, and gained testing result relative standard deviation is controlled in 5% scope; The surface is upgraded easily simultaneously, favorable reproducibility.The present invention makes simply, and is with low cost, highly sensitive, good stability, and favorable reproducibility can be widely used in the field quick detection and the daily monitoring of heavy metal ion in fresh water, seawater, food and the body fluid.
Description of drawings
The synoptic diagram of the sensor that Fig. 1 provides for the embodiment of the invention (wherein 1 is working electrode, and 2 is auxiliary electrode, and 3 is contrast electrode, and 4 is the CONTROLLED POTENTIAL instrument, and 5 is detection cell, and 6 is stirrer).
The synoptic diagram of the sensor sn-bi alloy disk working electrode that Fig. 2 provides for the embodiment of the invention (wherein 7 are the sn-bi alloy silk, and 8 is contact conductor, and 9 is polytetrafluoroethylmaterial material).
The synoptic diagram of the sensor sn-bi alloy post electrode that Fig. 3 provides for the embodiment of the invention (wherein 7 are the sn-bi alloy silk, and 8 is contact conductor, and 9 is polytetrafluoroethylmaterial material).
The schematic top plan view of the sensor sn-bi alloy printing work electrode that Fig. 4 provides for the embodiment of the invention (wherein 10 are the Polyvinylchloride substrate, and 11 is silver conductive layer, and 12 is the sn-bi alloy layer, and 13 is insulation course, and 14 is contact conductor).
The sensor that Fig. 5 provides for the embodiment of the invention is to the reappearance detection figure of heavy metal cadmium sample detection.
The sensor that Fig. 6 provides for the embodiment of the invention is to cobalt ions high sensitivity response diagram.
The sensor that Fig. 7 provides for the embodiment of the invention is to the stripping voltammogram and the corresponding working curve diagram of variable concentrations heavy metal zinc sample.
The sensor that Fig. 8 provides for the embodiment of the invention is to actual wine sample detection of zinc ions figure.
Embodiment
Adopting the sn-bi alloy disk electrode is the sensor of working electrode:
Sensor as illustrated in fig. 1 and 2: working electrode 1, contrast electrode 2 and auxiliary electrode 3 are connected in CONTROLLED POTENTIAL instrument 4 by the lead traction respectively; Working electrode 1, contrast electrode 2 and auxiliary electrode 3 insert and fill in the detection cell 5 that detects liquid, are provided with the magnetic stirrer 6 with beating action in the detection cell 5, and supporting at the bottom of the detection cell have magnetic stirring apparatus to rotate magnetic stir bar.The platinized platinum electrode is as auxiliary electrode, and saturated calomel electrode is a contrast electrode, and the CONTROLLED POTENTIAL instrument is measured the current-responsive value.
Described sn-bi alloy disk electrode is sn-bi alloy silk 7 outside surface sealed inert insulated enclosure materials 9 structures, and wherein sn-bi alloy silk 7 other ends are drawn by lead-in wire 8.
Difference from Example 1 is that working electrode is:
Sn-bi alloy post electrode is sn-bi alloy silk 7 outside surfaces sealing teflon sleeve 9 structures, one end of sn-bi alloy silk 7 is passed by an end face of teflon sleeve 9, and the other end lead-in wire 8 interior with inserting sealed inert insulated enclosure material is connected (referring to Fig. 3).
Teflon sleeve can be replaced by Ke1-F, AB gum cover pipe or glass bushing.Contrast electrode is silver/silver chloride electrode, and auxiliary electrode is a glass-carbon electrode.
Difference from Example 1 is that working electrode is:
Working electrode 1 prints electrode for sn-bi alloy, its method for making is specially with 6mm * 5cm pvc material as electrode basement 10, to utilize 3mm on the screen printer print * 4cm conductive silver glue-line 11 and contact conductor 14 after its cleaning and the drying, place infrared lamp oven dry in following 24 hours; Then with sn-bi alloy paste printing 4mm * 4cm sn-bi alloy electrode layer 12 and oven dry; Adopt light to insulate admittedly at last and starch printed electrode insulation course 13, reserve the effective working area (referring to Fig. 4) of 4mm * 4mm, use ultraviolet light polymerization at last as working electrode.
Described contrast electrode is printed silver/silver chloride electrode, and auxiliary electrode is the printed silver electrode.
Application examples 1
Adopt embodiment 1 described sensor cadmium:
Adopt embodiment 1 described sensor, with the α-Al of above-mentioned working electrode with 0.05 μ m granularity
2O
3On polishing cloth with polishing electrode to minute surface, with redistilled water flushing, use the salpeter solution of 1: 1 (volume ratio) and ethanol to clean 1-2min more respectively, the centre is washed with redistilled water respectively.Then in containing 0.1M HAc-NaAc (pH5.0) damping fluid, in-0.7V scope, carry out cyclic voltammetric linear sweep at-1.4V by the CONTROLLED POTENTIAL instrument, overlap better until cyclic voltammetry curve.Promptly reach the purpose of activated electrode, can be used for the detection of cadmium.
Under the magnetic agitation condition, in the detection cell that fills 20mL 0.1M HAc-NaAc (pH5.0) damping fluid, add 10 μ L 10 with above-mentioned electrode
-2The cadmium standard solution of M, enrichment 1min is stirred in energising, and stripping obtains the electrochemical oxidation current signal of cadmium; . by applying constant potential electrode surface is cleaned, carry out the second time after in 5min and measure, find continuous coverage 56 times, the relative standard deviation of peak current size≤5%.Be ten stacking diagrams wherein as Fig. 5.As figure shows, adopt the present invention to detect heavy metal ion and have good reappearance.
Application examples 2
Adopt embodiment 1 described sensor utilization adsorptive stripping voltammetry to detect cobalt or nickel:
Electrode dries disc surfaces after the polishing cleaning treatment, get 6 * 10 with microsyringe
-3The dimethylglyoxime solution 5 μ L of M drip at working electrode surface, place 2min under the room temperature.After treating the electrode surface natural air drying, with above-mentioned electrode under the magnetic agitation condition, to filling 20mL 0.1M NH
3H
2O-NH
4Add 10 μ L 10 in Cl (pH9.0) damping fluid
-2The Co of M
2+Or Ni
2+Standard solution.Sensor is inserted in the measuring cell, and enrichment 1min is stirred in energising, and stripping obtains the electrochemical reduction current signal of cobalt or nickel; Add nitrite ion in buffer solution, the reduction current signal of cobalt obviously strengthens (referring to Fig. 6).The size of the stripping volt-ampere peak to peak current by cobalt or nickel adopts novel sensor of the present invention that the detection of cobalt or nickel is had good response as can be known.
Application examples 3
Adopt embodiment 2 described sensor utilization adsorptive stripping voltammetries to detect chromium:
Adopt embodiment 2 described sensors, under the magnetic agitation condition, that gets back-ground electolyte and be 19mL contains 0.25M KNO
30.1M HAc-NaAc (pH6.0) damping fluid and 1mL 0.1M diethylene triamine pentacetic acid (DTPA) solution (DTPA), to wherein adding 10 μ L 10
-2The Cr of M
6+Standard solution.Sensor is inserted in the measuring cell, and enrichment 1min is stirred in energising, and stripping obtains chromic electrochemical reduction current signal.Adopt novel sensor of the present invention to be expected to be applied to check and analysis to hexavalent chromium in the seawater sample.
Application examples 4
Adopt embodiment 3 described sensor cadmiums:
Under the magnetic agitation condition, in the detection cell that fills 20mL 0.1M HAc-NaAc (pH5.0) damping fluid, add 10 μ L 10 with above-mentioned electrode
-2The cadmium standard solution of M, enrichment 1min is stirred in energising, and stripping obtains the electrochemical oxidation current signal of cadmium.This electrode structure is simple, and simple and convenient processing method, cost are low, and is easy to operate with this sensor detecting method of making of printing electrode, detection sensitivity is high.
Application examples 5
Zinc ion concentration is an example in employing embodiment 1 sensor determination drinks and the honey actual sample:
Working electrode adopts the sn-bi alloy disk electrode, and contrast electrode is a saturated calomel electrode, and auxiliary electrode is the platinized platinum electrode.Respectively the zinc standard solution of variable concentrations is measured.The size of the stripping volt-ampere peak to peak current by variable concentrations zinc is drawn the working curve (referring to Fig. 7) of zinc response.As can be known, adopt sensor of the present invention that zinc ion is had good response, the detection sensitivity height is for disturbing little actual sample can adopt working curve method to record the content of zinc in the actual sample.Wherein: the concentration of zinc standard solution is followed successively by 1,3,5,10,15,20 from bottom to top, and 25 μ M.
For drinks and honey sample, because the existence of disturbing adopts standard addition method to detect through pre-treatment.Concrete steps are as follows: the sample after at first will clearing up is diluted to certain proportion with the HAc-NaAc damping fluid, pipettes 20ml again to measuring cell.Sensor is inserted in the measuring cell, and enrichment 1min is stirred in energising under the magnetic agitation condition, and stripping obtains disturbing under the existence condition electrochemical oxidation current signal of zinc in the sample.Simultaneously get the liquid to be measured of amount same as described above in addition, in liquid to be measured, add the zinc standard solution of a series of variable concentrations (being respectively 3,6,9,12 μ M), detect the zinc peak current signal that obtains corresponding a series of zinc standard solution by above-mentioned same assay method.With zinc concentration current signal is mapped, extrapolated curve promptly obtains containing in the actual detected liquid concentration (referring to Fig. 8) of zinc ion.
The zinc ion concentration that adopts actual drinks of this sensor and Atomic Absorption Spectrometry and honey sample simultaneously is (referring to table 1) as can be known, and the present invention can accurately measure the zinc ion concentration in the actual food product sample.
Table 1
More than sensor that each application examples adopted can replace by embodiment 1-3 any sensor, sensor of the present invention, can carry out check and analysis to contents of many kinds of heavy metal ion according to diverse ways, can be widely used in the field quick detection and the daily monitoring of heavy metal ion in fresh water, seawater, food and the body fluid.
Claims (7)
1. an alloy electrode electrochemical sensor that is used to detect trace heavy metal comprises working electrode, contrast electrode and auxiliary electrode, it is characterized in that: the electrode of described alloy working electrode for being made by sn-bi alloy.
2. by the described alloy electrode electrochemical sensor that is used to detect trace heavy metal of claim 1, it is characterized in that: described electrochemical sensor is the alloy working electrode; Working electrode (1), contrast electrode (2) and auxiliary electrode (3) one ends insert and have in the detection cell (5) of stirrer (6), and the other end is connected in CONTROLLED POTENTIAL instrument (4) by lead respectively; Described alloy working electrode (1) is made by sn-bi alloy.
3. by claim 1 or the 2 described alloy electrode electrochemical sensors that are used to detect trace heavy metal, it is characterized in that: described alloy working electrode (1) can be sn-bi alloy disk electrode, sn-bi alloy post electrode or sn-bi alloy and prints electrode.
4. by the described alloy electrode electrochemical sensor that is used to detect trace heavy metal of claim 3, it is characterized in that: described sn-bi alloy disk electrode is sn-bi alloy silk (7) outside surface sealed inert insulated enclosure material (a 9) structure, and wherein sn-bi alloy silk (7) other end is drawn by lead-in wire (8); Described inertia insulated enclosure material (9) can be teflon, Ke1-F, AB glue or glass bushing.
5. by the described alloy electrode electrochemical sensor that is used to detect trace heavy metal of claim 3, it is characterized in that: described sn-bi alloy post electrode is sn-bi alloy silk (7) outside surface sealed inert insulated enclosure material (a 9) structure, one end of sn-bi alloy silk (7) is passed by an end face of inertia insulated enclosure material (9), and the other end is drawn by lead-in wire (8).
6. by the described alloy electrode electrochemical sensor that is used to detect trace heavy metal of claim 3, it is characterized in that: described sn-bi alloy print electrode into Polyvinylchloride as electrode basement (10), on electrode basement (10), be printed with conductive silver glue-line (11), on conductive silver glue-line (11), be printed with sn-bi alloy layer (12), be printed with insulation course (13) on the sn-bi alloy layer (12); Described insulation course has preformed hole on (13), and the sn-bi alloy layer (12) that is exposed by this preformed hole is the useful area of working electrode; Be connected with contact conductor (14) on the described conductive silver glue-line (11).
7. by the described alloy electrode electrochemical sensor that is used to detect trace heavy metal of claim 2, it is characterized in that: the trace heavy metal of described mensuration is cadmium, zinc, chromium, cobalt, nickel, gallium or thallium.
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| CN104267086A (en) * | 2014-10-14 | 2015-01-07 | 深圳大学 | Chemically modified carbon paste electrode as well as preparation method and application thereof |
| CN105675679A (en) * | 2016-03-04 | 2016-06-15 | 济南大学 | Preparation and application of ZnO-NCQDs (Nitrogen-doped Carbon Quantum Dots) DNA photoelectric sensor |
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| CN107576716A (en) * | 2017-09-18 | 2018-01-12 | 中国科学院烟台海岸带研究所 | A kind of acupuncture needle base working electrode electrochemical sensor for detecting trace heavy metal |
| CN107589169A (en) * | 2017-08-31 | 2018-01-16 | 山东理工大学 | The apparatus and method of cadmium ion in a kind of detection water |
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| CN107843633B (en) * | 2017-11-03 | 2020-05-19 | 大连大学 | Flexible electrode for copper ion determination and determination method thereof |
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| CN103344692A (en) * | 2013-06-27 | 2013-10-09 | 安徽大地熊新材料股份有限公司 | Method for detecting heavy metal ions in sewage |
| CN104267086B (en) * | 2014-10-14 | 2017-01-11 | 深圳大学 | Chemically modified carbon paste electrode as well as preparation method and application thereof |
| CN104267086A (en) * | 2014-10-14 | 2015-01-07 | 深圳大学 | Chemically modified carbon paste electrode as well as preparation method and application thereof |
| CN105675679A (en) * | 2016-03-04 | 2016-06-15 | 济南大学 | Preparation and application of ZnO-NCQDs (Nitrogen-doped Carbon Quantum Dots) DNA photoelectric sensor |
| CN105891294B (en) * | 2016-06-23 | 2019-07-23 | 中国科学院长春应用化学研究所 | A kind of method of Applied Electrochemistry analytic approach detection heavy metal ion |
| CN105891294A (en) * | 2016-06-23 | 2016-08-24 | 中国科学院长春应用化学研究所 | Method for detecting heavy metal ions by electrochemical analysis |
| CN107589169A (en) * | 2017-08-31 | 2018-01-16 | 山东理工大学 | The apparatus and method of cadmium ion in a kind of detection water |
| CN107589169B (en) * | 2017-08-31 | 2020-06-16 | 山东理工大学 | Manufacturing method of working electrode applied to molecular lead/tin film modified sensor |
| CN107576716A (en) * | 2017-09-18 | 2018-01-12 | 中国科学院烟台海岸带研究所 | A kind of acupuncture needle base working electrode electrochemical sensor for detecting trace heavy metal |
| CN107643328A (en) * | 2017-10-31 | 2018-01-30 | 中国农业科学院农业信息研究所 | A kind of SMD gas sensor device for food container formaldehyde examination and its preparation method and application |
| CN107843633B (en) * | 2017-11-03 | 2020-05-19 | 大连大学 | Flexible electrode for copper ion determination and determination method thereof |
| CN109406612A (en) * | 2018-11-21 | 2019-03-01 | 上海仪电科学仪器股份有限公司 | Use the electrolyte solution and its Cr VI detection method of mercury film electrode detection Cr VI |
| CN112730555A (en) * | 2020-12-16 | 2021-04-30 | 湖南华耀百奥医疗科技有限公司 | Zinc-based alloy working electrode and preparation method thereof |
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