CN102262112B - 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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- CN102262112B CN102262112B CN201110093150.8A CN201110093150A CN102262112B CN 102262112 B CN102262112 B CN 102262112B CN 201110093150 A CN201110093150 A CN 201110093150A CN 102262112 B CN102262112 B CN 102262112B
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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 electrochemical sensor field, specifically a kind of alloy electrode electrochemical sensor for detection of trace heavy metal.
Background technology
Along with the high speed development of modern industry and traffic, Heavy-Metal-Contaminated Environments is day by day serious, has become an important social concern that affects human health and public security.Heavy metal element can, at people's body accumulation, can cause the 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 Pollution, 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 the important content in analytical approach research in recent years.
Measuring content of beary metal main method is at present atomic absorption spectrography (AAS), atomic fluorescence spectrometry, ICP-AES, neutron activation analysis and Electrochemical 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 Food Inspection, but the method needs large-sized analytic instrument-Atomic Absorption Spectrometer as standard, 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 needs that large-scale instrument and equipment, monitoring velocity are slow, poor continuity, analysis cost is high and cannot on-line monitoring etc. defect.Electrochemical Stripping voltammetry, with advantages such as its instrument cost are cheap, easy to operate, standing charges are low, sensitivity is high, has certain advantage than said method 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, the stability of sensor needs further to be improved on the other hand.
Mercury electrode is a kind of Electrochemical Stripping voltammetric sensor of superior performance, but mercury is poisonous, going deep into it and be prohibited from using in 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, as a kind of environmentally friendly metallic element, can generate binary or multicomponent alloy with various heavy, and analytical performance and mercury are suitable, and background current is subject to the impact of dissolved oxygen DO hardly, is generally considered a kind of environmental type electrode material of replacement for mercury.But the bismuth bar electrode of making based on bismuth metal and bismuth film electrode sensor production process are complicated, testing process is easily urgently improved the aspect such as oxidized, electrode stability and reappearance, so limited it, detect at the scene and the application of instrumentation aspect.
Summary of the invention
The object of the invention is to provides a kind of alloy electrode electrochemical sensor for trace heavy metal fast detecting simple, favorable reproducibility of making for above-mentioned weak point.
For achieving the above object, technical scheme provided by the invention is:
An alloy electrode electrochemical sensor for detection of 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 alloy working electrode; Insert in the detection cell with stirrer working electrode, contrast electrode and auxiliary electrode one end, and the other end is connected in control potentiometer by wire 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 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 sn-bi alloy silk outside surface sealed inert insulated enclosure material structure, and one 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 prints electrode as usining Polyvinylchloride as electrode basement, is printed with conductive silver glue-line in electrode basement, is printed with sn-bi alloy layer on conductive silver glue-line, on sn-bi alloy layer, is printed with insulation course; On described insulation course, have preformed hole, the useful area that the sn-bi alloy layer being exposed by this preformed hole is working electrode; On described conductive silver glue-line, be connected with contact conductor.
The trace heavy metal of described mensuration is cadmium, zinc, chromium, cobalt, nickel, gallium or thallium.The present invention has advantages of: 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 without any modification step, makes simply, with low cost, and reliable and stable; It has good chemical property 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 subject to the impact of dissolved oxygen DO hardly, and detected solution, without letting nitrogen in and deoxidizing, has been avoided the loaded down with trivial details step in some actual measurements, is more conducive to the demand of field quick detection.
Sn-bi alloy electrode Stripping Voltammetry sensor of the present invention can be measured at least 56 times continuously in solution, and gained testing result relative standard deviation is controlled in 5% scope; Surface is easily upgraded simultaneously, favorable reproducibility.The present invention makes simply, with low cost, highly sensitive, good stability, and favorable reproducibility, can be widely used in field quick detection and the daily monitoring of heavy metal ion in fresh water, seawater, food and body fluid.
Accompanying drawing explanation
The schematic diagram of the sensor that Fig. 1 provides for the embodiment of the present invention (wherein 1 is working electrode, and 2 be auxiliary electrode, and 3 be contrast electrode, and 4 is control potentiometer, and 5 is detection cell, and 6 is stirrer).
The schematic diagram of the sensor sn-bi alloy disk working electrode that Fig. 2 provides for the embodiment of the present invention (wherein 7 is sn-bi alloy silk, and 8 is contact conductor, and 9 is polytetrafluoroethylmaterial material).
The schematic diagram of the sensor sn-bi alloy post electrode that Fig. 3 provides for the embodiment of the present invention (wherein 7 is 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 present invention (wherein 10 is Polyvinylchloride substrate, and 11 is silver conductive layer, and 12 is sn-bi alloy layer, and 13 is insulation course, and 14 is contact conductor).
The reappearance detection figure of the sensor that Fig. 5 provides for the embodiment of the present invention to heavy metal cadmium sample detection.
The sensor that Fig. 6 provides for the embodiment of the present invention is to cobalt ions high sensitivity response diagram.
The sensor that Fig. 7 provides for the embodiment of the present invention is to the Stripping Voltammetry figure of variable concentrations heavy metal zinc sample and corresponding working curve diagram.
The detection figure of the sensor that Fig. 8 provides for the embodiment of the present invention to actual wine sample zinc ion.
Embodiment
Adopt the sensor that sn-bi alloy disk electrode is working electrode:
Sensor as illustrated in fig. 1 and 2: working electrode 1, contrast electrode 2 and auxiliary electrode 3 are connected in and are controlled potentiometer 4 by wire 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 magnetic stirring 6 with beating action in detection cell 5, and supporting at the bottom of detection cell have magnetic stirring apparatus to rotate magnetic stir bar.Platinum plate electrode is as auxiliary electrode, and saturated calomel electrode is contrast electrode, controls potentiometer and measures current-responsive value.
Described sn-bi alloy disk electrode is sn-bi alloy silk 7 outside surface sealed inert insulated enclosure material 9 structures, and wherein sn-bi alloy silk 7 other ends 8 are drawn by going between.
Difference from Example 1 is that working electrode is:
Sn-bi alloy post electrode is sn-bi alloy silk 7 outside surface 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 is connected (referring to Fig. 3) with the lead-in wire 8 in inserting sealed inert insulated enclosure material.
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 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 usings 6mm * 5cm pvc material as electrode basement 10, after being cleaned and being dried, utilize 3mm * 4cm conductive silver glue-line 11 and contact conductor 14 on screen printer print, be placed in infrared lamp and dry for lower 24 hours; Then with sn-bi alloy paste printing 4mm * 4cm sn-bi alloy electrode layer 12 oven dry; Finally adopt light admittedly to insulate and starch printed electrode insulation course 13, reserve 4mm * 4mm as effective working area (referring to Fig. 4) of working electrode, finally use ultraviolet light polymerization.
Described contrast electrode is printed silver/silver chloride electrode, and auxiliary electrode is printed silver electrode.
Application examples 1
Sensor described in employing embodiment 1 detects cadmium:
Sensor described in employing embodiment 1, the α-Al by above-mentioned working electrode by 0.05 μ m granularity
2o
3on polishing cloth by polishing electrode to minute surface, with redistilled water, rinse, then use respectively the salpeter solution of 1: 1 (volume ratio) and ethanol to clean 1-2min, centre is rinsed with redistilled water respectively.Then in containing 0.1M HAc-NaAc (pH5.0) damping fluid, by controlling potentiometer, at-1.4V, within the scope of-0.7V, carry out cyclic voltammetric linear sweep, until cyclic voltammetry curve overlaps better.Reach the object of activated electrode, can be used for the detection of cadmium.
With above-mentioned electrode, under magnetic agitation condition, to filling in the detection cell of 20mL 0.1M HAc-NaAc (pH5.0) damping fluid, add 10 μ L 10
-2the cadmium standard solution of M, energising, stirs enrichment 1min, and stripping obtains the electrochemical oxidation current signal of cadmium; . by applying constant potential, electrode surface is cleaned, measure for the second time after in 5min, find continuous coverage 56 times, relative standard deviation≤5% of peak current size.If Fig. 5 is ten stacking diagrams wherein.As figure shows, adopt the present invention to detect heavy metal ion and there is good reappearance.
Application examples 2
Sensor described in employing embodiment 1 uses adsorptive stripping voltammetry to detect cobalt or nickel:
Electrode, after polishing cleaning treatment, dries disc surfaces, with microsyringe, gets 6 * 10
-3the dimethylglyoxime solution 5 μ L of M, drip at working electrode surface, under room temperature, place 2min.After electrode surface natural air drying, with above-mentioned electrode under magnetic agitation condition, to filling 20mL 0.1M NH
3h
2o-NH
4in Cl (pH9.0) damping fluid, add 10 μ L 10
-2the Co of M
2+or Ni
2+standard solution.Sensor is inserted in measuring cell, and energising, stirs enrichment 1min, and stripping obtains the electrochemical reduction current signal of cobalt or nickel; In buffer solution, add nitrite ion, the reduction current signal of cobalt obviously strengthens (referring to Fig. 6).The size of the Stripping Voltammetry peak to peak current by cobalt or nickel is known, adopts novel sensor of the present invention to have good response to the detection of cobalt or nickel.
Application examples 3
Sensor described in employing embodiment 2 uses adsorptive stripping voltammetry to detect chromium:
Adopt sensor described in embodiment 2, under 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), add wherein 10 μ L 10
-2the Cr of M
6+standard solution.Sensor is inserted in measuring cell, and energising, stirs enrichment 1min, and stripping obtains chromic electrochemical reduction current signal.Adopt novel sensor of the present invention to be expected to be applied to the detection analysis to hexavalent chromium in seawater sample.
Application examples 4
Sensor described in employing embodiment 3 detects cadmium:
With above-mentioned electrode, under magnetic agitation condition, to filling in the detection cell of 20mL 0.1M HAc-NaAc (pH5.0) damping fluid, add 10 μ L 10
-2the cadmium standard solution of M, energising, stirs enrichment 1min, and stripping obtains the electrochemical oxidation current signal of cadmium.This electrode structure is simple, and simple and convenient processing method, cost are low, easy to operate with this sensor detecting method of making of printing electrode, detection sensitivity is high.
Application examples 5
Adopting embodiment 1 sensor to measure zinc ion concentration in drinks and honey actual sample is example:
Working electrode adopts sn-bi alloy disk electrode, and contrast electrode is saturated calomel electrode, and auxiliary electrode is platinum plate electrode.Respectively the Zinc standard solution of variable concentrations is measured.The size of the Stripping Voltammetry peak to peak current by variable concentrations zinc is drawn the working curve (referring to Fig. 7) of zinc response.Known, adopt sensor of the present invention to have good response to zinc ion, detection sensitivity is high, for disturbing little actual sample can adopt working curve method to record the content of zinc in actual sample.Wherein: the concentration of Zinc standard solution is followed successively by 1,3,5,10,15,20, and, 25 μ M from bottom to top.
For drinks and the honey sample through pre-treatment, due to the existence of disturbing, adopt standard addition method to detect.Concrete steps are as follows: first the sample after clearing up is diluted to certain proportion with HAc-NaAc damping fluid, then pipettes 20ml to measuring cell.Sensor is inserted in measuring cell, and enrichment 1min is stirred in energising under magnetic agitation condition, and stripping obtains disturbing under existence condition the electrochemical oxidation current signal of zinc in sample.Separately get the liquid to be measured of amount same as described above simultaneously, the Zinc standard solution that adds a series of variable concentrations (being respectively 3,6,9,12 μ M) in liquid to be measured, detects the zinc peak current signal that obtains corresponding a series of Zinc standard solutions by above-mentioned same assay method.With zinc concentration, current signal is mapped, extrapolated curve obtains containing in actual detection liquid the concentration (referring to Fig. 8) of zinc ion.
Adopt the zinc ion concentration known (referring to table 1) of the actual drinks of this sensor and Atomic Absorption Spectrometry and honey sample, the zinc ion concentration of the present invention in can Accurate Determining actual food product sample simultaneously.
Table 1
The sensor that each application examples adopts above can be replaced by embodiment 1-3 any sensor, sensor of the present invention, can to contents of many kinds of heavy metal ion, detect analysis according to diverse ways, can be widely used in field quick detection and the daily monitoring of heavy metal ion in fresh water, seawater, food and body fluid.
Claims (6)
1. for detection of an alloy electrode electrochemical sensor for trace heavy metal, comprise 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; Described alloy working electrode (1) is that sn-bi alloy disk electrode, sn-bi alloy post electrode or sn-bi alloy print electrode.
2. by the alloy electrode electrochemical sensor for detection of trace heavy metal claimed in claim 1, it is characterized in that: described electrochemical sensor is alloy working electrode; Insert in the detection cell (5) with stirrer (6) working electrode (1), contrast electrode (2) and auxiliary electrode (3) one end, and the other end is connected in and is controlled potentiometer (4) by wire respectively; Described alloy working electrode (1) is made by sn-bi alloy.
3. by the alloy electrode electrochemical sensor for detection of trace heavy metal claimed in claim 1, it is characterized in that: described sn-bi alloy disk electrode is sn-bi alloy silk (7) outside surface sealed inert insulated enclosure material (9) structure, and wherein sn-bi alloy silk (7) other end is drawn by go between (8); Described inertia insulated enclosure material (9) is teflon, Ke1-F, AB glue or glass bushing.
4. by the alloy electrode electrochemical sensor for detection of trace heavy metal claimed in claim 1, it is characterized in that: described sn-bi alloy post electrode is sn-bi alloy silk (7) outside surface sealed inert insulated enclosure material (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 go between (8).
5. by the alloy electrode electrochemical sensor for detection of trace heavy metal claimed in claim 1, it is characterized in that: described sn-bi alloy prints electrode as usining Polyvinylchloride as electrode basement (10), in electrode basement (10), be printed with conductive silver glue-line (1), on conductive silver glue-line (11), be printed with sn-bi alloy layer (12), on sn-bi alloy layer (12), be printed with insulation course (13); Described insulation course has preformed hole on (13), and the sn-bi alloy layer (12) being exposed by this preformed hole is the useful area of working electrode; On described conductive silver glue-line (11), be connected with contact conductor (14).
6. by the alloy electrode electrochemical sensor for detection of trace heavy metal claimed in claim 1, it is characterized in that: the trace heavy metal of described mensuration is cadmium, zinc, chromium, brill, nickel, gallium or thallium.
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