CN103149265B - Based on the method for linear sweep voltammetry and three electrode sensor Fast Measurement copper - Google Patents
Based on the method for linear sweep voltammetry and three electrode sensor Fast Measurement copper Download PDFInfo
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- CN103149265B CN103149265B CN201210595246.9A CN201210595246A CN103149265B CN 103149265 B CN103149265 B CN 103149265B CN 201210595246 A CN201210595246 A CN 201210595246A CN 103149265 B CN103149265 B CN 103149265B
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Abstract
The invention discloses a kind of method based on linear sweep voltammetry and three electrode sensor Fast Measurement copper belonging to environmental monitoring technology field.The concrete steps of the method are: dry cooling after cleaning electrode substrate; Coating electrically conductive silver slurry formation 3 electrode strips on electrode base board, drying also cools; Then coating electrically conductive carbon slurry, forms contrast electrode, working electrode, to electrode and electrode working zone, drying also cools; Then coating insulation slurry becomes dielectric film, can obtain three electrode sensors after dry cooling.Electrochemical workstation is connected after cleaning three electrode sensors, the testing conditions of setting linear sweep voltammetry, measure the scanning peak point current of copper ion titer and liquid to be measured respectively, the linear equation between copper ion concentration and scanning peak point current can be obtained, the concentration value of liquid to be measured can be obtained by linear equation.The invention has the beneficial effects as follows that the cost of manufacture of three electrode sensors is low, during detection, sample requirement is less, quick, sensitive and cheaply effective.
Description
Technical field
The invention belongs to environmental monitoring technology field, be specifically related to a kind of method based on linear sweep voltammetry and three electrode sensor Fast Measurement copper.
Background technology
Along with field cupric massive discharge of pollutants such as industry, agricultural, traffic, copper has become a kind of important environmental contaminants.In recent years, the quick detection of soil, food, underground water, potable water or Cu in waste water was the direction that numerous environmental analysis worker makes great efforts.At present, the analytical approach for measuring copper content has multiple, and wherein the most frequently used instrument analytical method mainly contains flame atomic absorption method, sampling Graphite Furnace Atomic Absorption, ICP atomic emissions etc.Although these detection method preci-sion and accuracies are higher, detecting instrument is expensive, requires high to laboratory and instrumentation degree, and during operating cost, analysis cost is expensive, is unfavorable for promoting the use of, and is difficult to the requirement adapting to great amount of samples and Site Detection.Therefore, find a kind of quick, sensitive and cheap effective detection side's religious services or rituals must go.
And electrochemical sensor analysis and detection technology has the feature that speed is faster, cost is lower by comparison, be considered to the method for the most applicable on-line checkingi trace or ultratrace heavy metal at present.The present invention sets up a kind of method for quick being applicable to copper ion in water body.
Summary of the invention
The object of this invention is to provide a kind of method based on linear sweep voltammetry and three electrode sensor Fast Measurement copper.Its concrete steps are as follows:
(1) select length to be 40mm, width is 15mm, the electrode base board 1 of thickness to be 2mm material be polyethylene terephthalate, by washed with de-ionized water three times, with washes of absolute alcohol three times, in 50 DEG C of drying boxes dry 3 hours, be then cooled to 20 DEG C;
(2) form contrast electrode bar 2, working electrode bar 3 and to electrode strip 4 to coating electrically conductive silver slurry on the electrode base board 1 in step (1), the length of these three electrode strips is 25mm, and width is 2mm; When coating electrically conductive silver slurry from the bottom of electrode base board 1, first apply middle working electrode bar 3, the position of working electrode bar 3 is in the centre of electrode base board 1, its center line overlaps with the center line of electrode base board 1, then contrast electrode bar 2 is applied at interval, the left side 3mm of working electrode bar 3, apply electrode strip 4 at interval, the right side 3mm of working electrode bar 3, apply and to be completely placed in 130 DEG C of drying boxes dry 35 minutes, be then cooled to 20 DEG C;
(3) to coating electrically conductive carbon slurry on the electrode base board 1 in step (2), first start to apply contrast electrode 5, working electrode 6 and to electrode 7 in the bottom of electrode base board 1, the length of these three electrodes is 10mm, width is 2mm, wherein contrast electrode 5 is identical with the position of contrast electrode bar 2, working electrode 6 is identical with the position of working electrode bar 3, identical with to the position of electrode strip 4 to electrode 7; Then applying external radius on the top of electrode base board 1 is 6.83mm, inside radius is the annulus 8 of 4.52mm, and the center of circle is positioned at substrate center's line, and is 12.9mm with the distance at electrode base board 1 top, annulus angle is 208 °, through the center of circle in top parallel from left side to right rotation 208 °; Then apply electrode connecting line 9, being 4mm to the bottom of electrode connecting line 9 and the distance of annulus 8 exterior bottom, is 5.16mm with the distance of annulus 8 inside bottom, its width 2mm, and its position overlaps with to electrode strip 4; Then coated electrode workspace 10, it is the filled circles of radius 1.5mm, and the center of circle overlaps with the center of circle of annulus 8; Then application job electrode connecting line 11, the bottom of working electrode connecting line 11 and the distance of center circle of electrode working zone 10 are from being 7.26mm, and its width is 2mm, and its position overlaps with working electrode bar 3; Apply and to be completely placed in 130 DEG C of drying boxes dry 35 minutes, be then cooled to 20 DEG C;
(4) on the electrode base board 1 in step (3), coating insulation slurry becomes dielectric film 12, and in dielectric film 12, the length of each grid is 1.5mm, and width is 0.05mm; When coating coating insulating film 12 from the top of electrode base board 1, and the distance bottom dielectric film 12 and between electrode base board 1 top is 35mm, and the width of dielectric film 12 is identical with the width of electrode base board 1; When coating coating insulating film 12, do not apply to insulate in the region overlapped with annulus on the right side of annulus 8 vertically center line and starch, do not apply to insulate in the left field symmetrical with this region yet and starch; Simultaneously also not starching with applying to insulate in all identical filled circles of electrode working zone 10 size and position; Apply complete after within 35 minutes, to be placed in 120 DEG C of drying boxes dry 30 minutes through Ultraviolet radiation, be then cooled to 20 DEG C, three electrode sensors can be obtained;
(5) repeat step (1) to (4), prepare 50 three electrode sensors, be placed in 4 DEG C of refrigerator kept dry for subsequent use;
(6) with high purity water, cupric chloride is mixed with the storing solution that concentration is 200mg/L, then storing solution is diluted with high purity water, be mixed with the use liquid that concentration is 5mg/L, liquid is used again with high purity water dilution, be mixed with concentration and be respectively 0.02mg/L, the titer of 0.05mg/L, 0.1mg/L, 0.3mg/L and 0.5mg/L;
(7) to take from three electrode sensors that step (5) saves backup three electrode sensors, dry after this three electrode sensor being cleaned 5 minutes in ultrasonic cleaner with deionized water, by the contrast electrode 5 bottom three electrode sensors, working electrode 6 with electrode 7 is connected respectively to the contrast electrode of electrochemical workstation, working electrode and to electrode, then the accumulating potential setting linear sweep voltammetry is-1.2V, and enrichment time is 270s;
(8) ammonium chloride of the dissolved liquid of citric acid and 100 μ l0.55mol/L that drip 100 μ lpH=5.5 in the electrode working zone 10 of step (7) three electrode sensor as supporting electrolyte, and stirs;
(9) in the electrode working zone 10 of step (8) three electrode sensor, add the copper ion titer that 100 μ l concentration are 0.02mg/L, then measure its scanning peak point current;
(10) step (7) is repeated to (8), adding 100 μ l concentration in electrode working zone 10 respectively to step (8) three electrode sensor is 0.02mg/L, 0.05mg/L, 0.1mg/L, the copper ion titer of 0.3mg/L and 0.5mg/L, then measures its scanning peak point current respectively;
(11) according to each various criterion liquid concentration and the scanning peak point current that corresponds, the linear equation between copper ion concentration and scanning peak point current can be obtained;
(12) step (7) is repeated to (8), 100 μ l liquid to be measured is added in the electrode working zone 10 of step (8) three electrode sensor, measure its scanning peak point current, according to linear equation obtain surveys and scans concentration value corresponding to peak point current.
In method of the present invention, the electrochemical workstation used is CHI440D electrochemical workstation.
The invention has the beneficial effects as follows that three obtained electrode sensor volumes are smaller and more exquisite, easy to carry, cost of manufacture is low, needs sample size less when detecting the copper in sample, quick, sensitive and cheaply effective.
Accompanying drawing explanation
Accompanying drawing 1 is the schematic diagram after coating electrically conductive silver slurry.In accompanying drawing 1,1 is electrode base board, 2 be contrast electrode bar, 3 for working electrode bar, 4 is to electrode strip.
Accompanying drawing 2 is the schematic diagram after coating electrically conductive carbon slurry.In accompanying drawing 2,5 is contrast electrode, and 6 is working electrode, and 7 is to electrode, and 8 is annulus, and 9 is working electrode connecting line, and 10 is electrode working zone, and 11 is to electrode connecting line.
Accompanying drawing 3 is the schematic diagram after coating insulation slurry.In accompanying drawing 3,12 is dielectric film.
Accompanying drawing 4 is schematic diagram of three electrode sensors after completing.
Accompanying drawing 5 is detailed dimensions figure of three electrode sensors.In accompanying drawing 5, A is the schematic diagram after coating electrically conductive silver slurry, and B is the schematic diagram after coating electrically conductive carbon slurry, and C is the schematic diagram after coating insulation slurry, and D is the schematic diagram of three electrode sensors after completing.
Embodiment
The present invention is further illustrated below in conjunction with example.
Material and instrument:
(1) material is the electrode base board of polyethylene terephthalate.
(2) silver slurry, insulation slurry, carbon slurry.
(3) ammonium chloride (99.999%, AlfaAesar company), cupric chloride (G.R, Tianjin recovery fine chemistry industry research institute).
(4) concentration is the cupric chloride storing solution of 200mg/L, and concentration is that the cupric chloride of 5mg/L uses liquid, and concentration is respectively 0.02mg/L, the cupric chloride titer of 0.05mg/L, 0.1mg/L, 0.3mg/L and 0.5mg/L.
(5) liquid to be measured: by 5mL concentration be 5mg/L cupric chloride use liquid join in 150mL tap water the liquid to be measured being mixed with containing copper chloride.
(6) citric acid solution of pH=5.5.
(7) concentration is the ammonium chloride solution of 0.55mol/L.
(8) CHI440D electrochemical workstation.
Embodiment
Selecting long is 40mm, wide 15mm, the electrode base board of thickness to be 2mm material be polyethylene terephthalate, by washed with de-ionized water three times, with washes of absolute alcohol three times, and then in 50 DEG C of drying boxes dry 3 hours.On electrode base board, coating electrically conductive silver slurry formation 3 length are 25mm, and width is the contrast electrode bar of 2mm, working electrode bar and to electrode strip, apply completely to be placed in 130 DEG C of drying boxes dry 35 minutes, are cooled to 20 DEG C.Then coating electrically conductive carbon slurry, from bottom, first apply contrast electrode, working electrode and to electrode, then applying external radius on top is 6.83mm, inside radius is the annulus of 4.52mm, then apply electrode connecting line, electrode working zone and working electrode connecting line, apply and to be completely placed in 130 DEG C of drying boxes dry 35 minutes, be cooled to 20 DEG C.Then coating insulation slurry becomes dielectric film, apply complete after within 35 minutes, to be placed in 120 DEG C of drying boxes dry 30 minutes through Ultraviolet radiation, be cooled to 20 DEG C, three electrode sensors can be obtained.Said process makes 50 three electrode sensors respectively on time, then these three electrode sensors is positioned over kept dry in 4 DEG C of refrigerators for subsequent use.
Three electrode sensors of making and CHI440D electrochemical workstation is used to measure the scanning peak point current of copper ion titer below, its detailed process measured is as follows: three electrode sensors of taking, dry after three electrode sensors being cleaned 5 minutes in ultrasonic cleaner with deionized water, by the contrast electrode bottom three electrode sensors, working electrode and contrast electrode electrode being connected respectively to CHI440D electrochemical workstation, working electrode and to electrode, then the testing conditions of linear sweep voltammetry is set, wherein accumulating potential is-1.2V, enrichment time is 270s.The ammonium chloride of the citric acid solution from 100 μ lpH=5.5 to electrode working zone and 100 μ l0.55mol/L that drip as supporting electrolyte, and stirs; Then add the copper ion titer that 100 μ l concentration are 0.02mg/L to electrode working zone, measure scanning peak point current.
Repeat said determination process, measuring concentration is respectively the copper ion titer of 0.05mg/L, 0.1mg/L, 0.3mg/L and 0.5mg/L and the scanning peak point current of liquid to be measured.According to each various criterion liquid concentration and the scanning peak point current that corresponds, the linear equation between copper ion concentration and scanning peak point current can be obtained, i=0.0977c+0.9634, coefficient R
2=0.9991.Can obtain concentration value corresponding to the scanning peak point current of liquid to be measured by linear equation, result shows that the concentration of liquid to be measured is 0.16mg/L.
Claims (1)
1., based on a method for linear sweep voltammetry and three electrode sensor Fast Measurement copper, it is characterized in that, the concrete steps of the method are as follows:
(1) select length to be 40mm, width is 15mm, the electrode base board 1 of thickness to be 2mm material be polyethylene terephthalate, by washed with de-ionized water three times, with washes of absolute alcohol three times, in 50 DEG C of drying boxes dry 3 hours, be then cooled to 20 DEG C;
(2) form contrast electrode bar 2, working electrode bar 3 and to electrode strip 4 to coating electrically conductive silver slurry on the electrode base board 1 in step (1), the length of these three electrode strips is 25mm, and width is 2mm; When coating electrically conductive silver slurry from the bottom of electrode base board 1, first apply middle working electrode bar 3, the position of working electrode bar 3 is in the centre of electrode base board 1, its center line overlaps with the center line of electrode base board 1, then contrast electrode bar 2 is applied at interval, the left side 3mm of working electrode bar 3, apply electrode strip 4 at interval, the right side 3mm of working electrode bar 3, apply and to be completely placed in 130 DEG C of drying boxes dry 35 minutes, be then cooled to 20 DEG C;
(3) to coating electrically conductive carbon slurry on the electrode base board 1 in step (2), first start to apply contrast electrode 5, working electrode 6 and to electrode 7 in the bottom of electrode base board 1, the length of these three electrodes is 10mm, width is 2mm, wherein contrast electrode 5 is identical with the position of contrast electrode bar 2, working electrode 6 is identical with the position of working electrode bar 3, identical with to the position of electrode strip 4 to electrode 7; Then applying external radius on the top of electrode base board 1 is 6.83mm, inside radius is the annulus 8 of 4.52mm, and the center of circle is positioned at substrate center's line, and is 12.9mm with the distance at electrode base board 1 top, annulus angle is 208 °, through the center of circle in top parallel from left side to right rotation 208 °; Then apply electrode connecting line 9, being 4mm to the bottom of electrode connecting line 9 and the distance of annulus 8 exterior bottom, is 5.16mm with the distance of annulus 8 inside bottom, its width 2mm, and its position overlaps with to electrode strip 4; Then coated electrode workspace 10, it is the filled circles of radius 1.5mm, and the center of circle overlaps with the center of circle of annulus 8; Then application job electrode connecting line 11, the bottom of working electrode connecting line 11 and the distance of center circle of electrode working zone 10 are from being 7.26mm, and its width is 2mm, and its position overlaps with working electrode bar 3; Apply and to be completely placed in 130 DEG C of drying boxes dry 35 minutes, be then cooled to 20 DEG C;
(4) on the electrode base board 1 in step (3), coating insulation slurry becomes dielectric film 12, and in dielectric film 12, the length of each grid is 1.5mm, and width is 0.05mm; When coating coating insulating film 12 from the top of electrode base board 1, and the distance bottom dielectric film 12 and between electrode base board 1 top is 35mm, and the width of dielectric film 12 is identical with the width of electrode base board 1; When coating coating insulating film 12, do not apply to insulate in the region overlapped with annulus on the right side of annulus 8 vertically center line and starch, do not apply to insulate in the left field symmetrical with this region yet and starch; Simultaneously also not starching with applying to insulate in all identical filled circles of electrode working zone 10 size and position; Apply complete after within 35 minutes, to be placed in 120 DEG C of drying boxes dry 30 minutes through Ultraviolet radiation, be then cooled to 20 DEG C, three electrode sensors can be obtained;
(5) repeat step (1) to (4), prepare 50 three electrode sensors, be placed in 4 DEG C of refrigerator kept dry for subsequent use;
(6) with high purity water, cupric chloride is mixed with the storing solution that concentration is 200mg/L, then storing solution is diluted with high purity water, be mixed with the use liquid that concentration is 5mg/L, liquid is used again with high purity water dilution, be mixed with concentration and be respectively 0.02mg/L, the titer of 0.05mg/L, 0.1mg/L, 0.3mg/L and 0.5mg/L;
(7) to take from three electrode sensors that step (5) saves backup three electrode sensors, dry after this three electrode sensor being cleaned 5 minutes in ultrasonic cleaner with deionized water, by the contrast electrode 5 bottom three electrode sensors, working electrode 6 with electrode 7 is connected respectively to the contrast electrode of electrochemical workstation, working electrode and to electrode, then the accumulating potential setting linear sweep voltammetry is-1.2V, and enrichment time is 270s;
(8) ammonium chloride of the dissolved liquid of citric acid and 100 μ l0.55mol/L that drip 100 μ lpH=5.5 in the electrode working zone 10 of step (7) three electrode sensor as supporting electrolyte, and stirs;
(9) in the electrode working zone 10 of step (8) three electrode sensor, add the copper ion titer that 100 μ l concentration are 0.02mg/L, then measure its scanning peak point current;
(10) step (7) is repeated to (8), adding 100 μ l concentration in electrode working zone 10 respectively to step (8) three electrode sensor is 0.02mg/L, 0.05mg/L, 0.1mg/L, the copper ion titer of 0.3mg/L and 0.5mg/L, then measures its scanning peak point current respectively;
(11) according to each various criterion liquid concentration and the scanning peak point current that corresponds, the linear equation between copper ion concentration and scanning peak point current can be obtained;
(12) step (7) is repeated to (8), 100 μ l liquid to be measured is added in the electrode working zone 10 of step (8) three electrode sensor, measure its scanning peak point current, according to linear equation obtain surveys and scans concentration value corresponding to peak point current.
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| CN105388201A (en) * | 2015-10-21 | 2016-03-09 | 浙江大学 | Three-electrode integrated electrochemical sensor based on microelectrode array |
| CN113109408A (en) * | 2021-04-08 | 2021-07-13 | 海南师范大学 | Portable palm electrochemical sensor for detecting enzyme concentration based on chip electrode and preparation method and detection method thereof |
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| CN202066830U (en) * | 2011-01-25 | 2011-12-07 | 北京师范大学 | Screen printing electrode enzyme sensor capable of quickly detecting organic phosphorous pesticides |
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