CN104062336A - Golden wire electrochemical microelectrode, manufacturing method and application of golden wire electrochemical microelectrode - Google Patents
Golden wire electrochemical microelectrode, manufacturing method and application of golden wire electrochemical microelectrode Download PDFInfo
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- CN104062336A CN104062336A CN201410215779.9A CN201410215779A CN104062336A CN 104062336 A CN104062336 A CN 104062336A CN 201410215779 A CN201410215779 A CN 201410215779A CN 104062336 A CN104062336 A CN 104062336A
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- Prior art keywords
- microelectrode
- galvanochemistry
- spun gold
- insulating electrode
- herba anoectochili
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- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001514 detection method Methods 0.000 claims abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003822 epoxy resin Substances 0.000 claims abstract description 8
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 5
- FGIWMSAVEQNPPQ-UHFFFAOYSA-N arsenic;hydrate Chemical compound O.[As] FGIWMSAVEQNPPQ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052737 gold Inorganic materials 0.000 claims description 30
- 239000010931 gold Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 17
- 239000004020 conductor Substances 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- 239000000565 sealant Substances 0.000 claims description 8
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 238000000840 electrochemical analysis Methods 0.000 claims description 4
- -1 polypropylene Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims description 2
- 230000037431 insertion Effects 0.000 claims description 2
- 235000013824 polyphenols Nutrition 0.000 claims description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 2
- 238000013138 pruning Methods 0.000 claims 1
- 229910052785 arsenic Inorganic materials 0.000 abstract description 23
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000005538 encapsulation Methods 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000011067 equilibration Methods 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000000835 electrochemical detection Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003673 groundwater Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000000918 plasma mass spectrometry Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005171 square wave anodic stripping voltammetry Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 201000009030 Carcinoma Diseases 0.000 description 1
- 208000017667 Chronic Disease Diseases 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- 208000003351 Melanosis Diseases 0.000 description 1
- 244000141353 Prunus domestica Species 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000119 electrospray ionisation mass spectrum Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
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- 238000004451 qualitative analysis Methods 0.000 description 1
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- 238000010183 spectrum analysis Methods 0.000 description 1
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- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The invention discloses a golden wire electrochemical microelectrode, a manufacturing method and application of the golden wire electrochemical microelectrode in detection on arsenic in underground water. The golden wire electrochemical microelectrode for detecting the arsenic in the underground water is a conventional electrochemical electrode; the conventional electrode manufacturing technology is simplified and is evolved into a manufacturing method which is easy to operate and has mild technical conditions. A gold wire serving as an electrochemical sensitive material is directly connected with a conductive copper wire through conductive silver paste. Furthermore, encapsulation is implemented by common epoxy resin; an insulation electrode sleeve is used as a shell, so that the gold wire microelectrode for detecting the arsenic in the underground water can be obtained, has the advantages of high stability, high detection precision and high interference resistance, and is expected to be a universal underground water arsenic detection device.
Description
Technical field
The present invention relates to a kind of spun gold galvanochemistry microelectrode and make, and detection for arsenic from underwater with it.Specially refer to a kind of design and method for making of simple and easy microelectrode sensor component.
Background technology
Arsenic Contamination in Groundwater problem is the environmental problem that become international, and is detrimental to health, and long-term drinking high-arsenic underground water can cause multiple chronic disease, such as melanose, and skin lesion and various cutaneum carcinoma and lung cancer etc.Therefore, Arsenic Contamination in Groundwater is called " harm of maximum in mankind's history " by the World Health Organization (WHO).Arsenic from underwater analytical approach mainly relies on Atomic absorption or atom fluorescent luminosity method, induced plasma-mass spectrometry, and electro-spray ionization-mass spectrum, gas chromatography-mass spectrography, the methods such as HPLC-MS are carried out qualitative and quantitative analysis.These spectrum or mass spectrometric analysis method have very high sensitivity and accuracy, but also come with some shortcomings part: i) common high precision spectrum or mass spectrometer is larger, are not suitable for real time monitoring application; Ii) to links such as the collection of sample, pre-service and preservations, require stricter.Arsenic morphology is very easily subject to ambient environmental conditions (as Redox Condition, pH, Fe (II/III), organism, microbial activities) change and transforming, thereby the collection of water sample and preservation condition are had to higher requirement, deal with improperly and can cause that analysis result and actual conditions produce deviation; Iii) most of instrumentation process is comparatively complicated, and experimenter's operating experience is had relatively high expectations; Iv) operating cost of instrument is higher.Therefore, need the arsenic from underwater on-the site analysis method that development has the features such as Stability and dependability is high, cost is low, simple to operate badly.
Electrochemical analysis method is to be hopeful most to realize one of method of the on-the site analysis of arsenic from underwater, and it has the features such as highly sensitive, low-cost low, simple to operate.Yet Electrochemical Detection working electrode used is many at present encapsulates with teflon in hot environment, its technique is difficult in the same way, realizes application popular, universality.And conventional electrodes is subject to interference and the pollution of complex environment in the application of complex environment (as underground water) as electrochemical sensing detection means, the deficiencies such as stable difference, thus can not improve reliable, believable detection analysis result.
Summary of the invention
The object of this invention is to provide a kind of easy electrochemical metal microelectrode, by simple and gentle process conditions, realize the encapsulation of microelectrode is made, simplified existing circumscribed technology.This microelectrode can be applicable to the detection of arsenic from underwater, has advantages of that sane, effective, accurate and anti-complex environment disturbs, and the universality that can be electrochemical sensor is effectively promoted.
A kind of spun gold galvanochemistry microelectrode of the present invention, comprises an insulating electrode cover, and one end of described insulating electrode cover is connected with copper conductor, and the other end is connected with Herba Anoectochili roxburghii, and described copper conductor is connected by being placed in the electrocondution slurry of insulating electrode cover with Herba Anoectochili roxburghii.
Described insulating electrode cover can be for taper be as taper shape, square taper etc., and its cone tip part inserts Herba Anoectochili roxburghii.
The cone tip of described taper insulating electrode rod scribbles fluid sealant; Described fluid sealant is as being epoxy resin, phenolics, organic siliconresin or unsaturated polyester resin etc.
The described Herba Anoectochili roxburghii length that leans out cone tip seal glue is no more than 5 millimeters and is advisable.
Described insulating electrode cover is the hollow cone structure of acid and alkali-resistance material, and its material can be the insulating material such as polypropylene based polymers, glass or teflon.
Described electrocondution slurry can be conductive silver paste etc.
The method for making of spun gold galvanochemistry microelectrode of the present invention, first one end of Herba Anoectochili roxburghii is inserted to the cone tip part of taper insulating electrode cover, the tip seal of with fluid sealant, taper insulating electrode being overlapped again, normal temperature cure fluid sealant, then injecting conductive silver paste makes one end of overlapping the copper conductor of other end insertion from insulating electrode pass through the adhesion of electrocondution slurry phase with the Herba Anoectochili roxburghii termination that is inserted into taper insulating electrode cover, curing conductive slurry, prunes Herba Anoectochili roxburghii and makes the Herba Anoectochili roxburghii length that leans out taper insulating electrode cover tip seal glue be no more than 5 millimeters.
Finally, can be placed in fixed cover (as pp pipeline) by making complete spun gold galvanochemistry microelectrode, in order to Electrochemical Detection, use.
Described Herba Anoectochili roxburghii diameter 5-20 micron is advisable.
Spun gold galvanochemistry microelectrode of the present invention can be used as working electrode in electrochemical analysis method for the detection of water arsenic.The present invention can encapsulate by common epoxy resin, can pp pipeline as shell, thereby obtain can be used for detecting the spun gold microelectrode of arsenic from underwater, and there is good stability, accuracy of detection is high, antijamming capability is strong.
Beneficial effect of the present invention is:
The detecting element of the spun gold galvanochemistry microelectrode of one, this detection underground water is different from traditional conventional electrodes, adopt spun gold as sensitive material, to improve the anti-interference of electrode itself, can realize the efficient of arsenic in complex environment and accurately detect, significantly improve it and detected effect.
Two, unique easy technique is made and can under gentle condition, be realized the encapsulation to microelectrode, greatly improves its range of application.
Three, designed spun gold microelectrode device volume is less and manufacture craft is simple to operation, thereby can make galvanochemistry effectively be promoted in actual environment analyzing and testing, and is expected to obtain generalization, popular application.
Accompanying drawing explanation
Fig. 1 is spun gold microelectrode structural representation;
Fig. 2 be take the test result of the arsenic that spun gold microelectrode is 10-100ppb to concentration;
Fig. 3 is for adopting the concentration determination result of spun gold galvanochemistry microelectrode test arsenic from underwater.
In figure, 1, copper conductor, 2, taper insulating electrode cover, 3, conductive silver paste, 4, epoxide-resin glue, 5, Herba Anoectochili roxburghii.
Embodiment
Following embodiment is usingd as the explaination to the technology of the present invention content for further illustrating of content of the present invention; but flesh and blood of the present invention is not limited in described in following embodiment, those of ordinary skill in the art can and should know any simple change or replacement based on connotation of the present invention all should belong to protection domain of the presently claimed invention.
As shown in Figure 1, a kind of spun gold galvanochemistry microelectrode of the present invention, comprise a taper insulating electrode cover 2, the cone tip part of taper insulating electrode cover 2 is connected with copper conductor 1, its other end is connected with Herba Anoectochili roxburghii 5, and copper conductor 1 is mutually bonding by the electrocondution slurry 3 being placed in taper insulating electrode cover 2 with Herba Anoectochili roxburghii 5; The cone tip of taper insulating electrode cover 2 scribbles epoxide-resin glue 4.
Make spun gold galvanochemistry microelectrode, and it is as follows to adopt the electrode of making to carry out the detection example of arsenic in water:
embodiment 1
The making of spun gold galvanochemistry microelectrode of the present invention.First by 1.5 centimetres of length, the Herba Anoectochili roxburghii 5 that diameter is 12.7 microns inserts taper hollow polypropylene pipe 2, approximately 0.5 centimetre of exposed partial-length outside the mouth of pipe; With epoxide-resin glue, by taper hollow polypropylene pipe tip seal, make at normal temperatures its natural drying solidifying; Utilize conductive silver paste 3 by copper conductor 1 and Herba Anoectochili roxburghii 5 adhesions, then dry, so that electrocondution slurry solidifies, stablize; Cut off that part is exposed overlaps most advanced and sophisticated spun gold at taper insulating electrode, retain lean out epoxide-resin glue spun gold length between 1 millimeter to 2 millimeters.Finally by making complete spun gold galvanochemistry microelectrode, be placed in fixed cover, in order to using.
The electrochemical analysis condition of this example: adopt galvanochemistry square wave anodic stripping voltammetry to analyze arsenic, end liquid: N
2h
42HCl(2g/L), accumulating potential :-0.35V, enrichment time: 90s, equilibration time: 20s.In liquid at the bottom of 10mL, drip successively trivalent arsenic standard solution, solution concentration increases progressively from 10ppb to 100ppb, and result shows that the present invention has good linear response to arsenic, and sensitivity is 0.472 nA/ppb (R
2=0.998), detect and be limited to 5.01ppb.Test result is shown in Fig. 2.
embodiment 2
Adopt the concentration of spun gold galvanochemistry microelectrode test arsenic from underwater.Adopt galvanochemistry square wave anodic stripping voltammetry to analyze, scaling method is standard addition method.End liquid: N
2h
42HCl(4g/L), accumulating potential :-0.35V, enrichment time: 90s, equilibration time: 20s.By 5mL underground water and 5mL N
2h
4at the bottom of 2HCl, liquid mixes, accumulating potential :-0.35V, enrichment time: 90s, equilibration time: 20s.Drip successively trivalent arsenic standard solution, solution concentration increases progressively from 10ppb to 100ppb, and by current-responsive, the concentration that detects arsenic from underwater is 102.12ppb (adopting inductivity coupled plasma mass spectrometry test result is 105ppb).Test result as shown in Figure 3.
Claims (9)
1. a spun gold galvanochemistry microelectrode, comprises an insulating electrode rod, it is characterized in that, one end of described insulating electrode rod is connected with copper conductor, and the other end is connected with Herba Anoectochili roxburghii, and described copper conductor is connected by the electrocondution slurry being placed in insulating electrode rod with Herba Anoectochili roxburghii.
2. spun gold galvanochemistry microelectrode as claimed in claim 1, is characterized in that, described insulating electrode cover is taper, and cone tip part connects Herba Anoectochili roxburghii.
3. spun gold galvanochemistry microelectrode as claimed in claim 2, is characterized in that, the cone tip of described taper insulating electrode cover scribbles fluid sealant.
4. spun gold galvanochemistry microelectrode as claimed in claim 3, is characterized in that, described fluid sealant is epoxy resin, phenolics, organic siliconresin or unsaturated polyester resin.
5. spun gold galvanochemistry microelectrode as claimed in claim 3, is characterized in that, described in lean out cone tip seal glue Herba Anoectochili roxburghii length be no more than 5 millimeters.
6. spun gold galvanochemistry microelectrode as claimed in claim 5, is characterized in that, described insulating electrode cover is the hollow cone structure of acid and alkali-resistance material.
7. the method for making of spun gold galvanochemistry microelectrode described in a claim 6, it is characterized in that, first one end of Herba Anoectochili roxburghii is inserted to the tip of insulating electrode cover hollow tube, with fluid sealant, insulating electrode is overlapped again to the tip seal of hollow tube, normal temperature cure fluid sealant, then inject electrocondution slurry, make one end of overlapping the copper conductor of other end insertion from taper insulating electrode pass through the adhesion of electrocondution slurry phase with the Herba Anoectochili roxburghii termination that is inserted into taper hollow polypropylene pipe, curing conductive slurry, pruning Herba Anoectochili roxburghii makes the Herba Anoectochili roxburghii length that leans out taper insulating electrode cover cone tip seal glue be no more than 5 millimeters.
8. spun gold galvanochemistry microelectrode as claimed in claim 7, is characterized in that described Herba Anoectochili roxburghii diameter 5-20 micron.
9. spun gold galvanochemistry microelectrode or adopt the application of the spun gold galvanochemistry microelectrode that method for making obtains described in claim 7 as claimed in claim 1, is characterized in that the detection as the working electrode in electrochemical analysis method for water arsenic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410215779.9A CN104062336A (en) | 2014-05-21 | 2014-05-21 | Golden wire electrochemical microelectrode, manufacturing method and application of golden wire electrochemical microelectrode |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410215779.9A CN104062336A (en) | 2014-05-21 | 2014-05-21 | Golden wire electrochemical microelectrode, manufacturing method and application of golden wire electrochemical microelectrode |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106033071A (en) * | 2015-03-10 | 2016-10-19 | 中国科学院生物物理研究所 | New Carbon Fiber Electrodes for Patch Clamp Electrochemical Technique Systems |
| CN107102044A (en) * | 2017-05-03 | 2017-08-29 | 西南科技大学 | Sensing electrode for detecting uranyl ions in water and methods of making and using the same |
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| US5120421A (en) * | 1990-08-31 | 1992-06-09 | The United States Of America As Represented By The United States Department Of Energy | Electrochemical sensor/detector system and method |
| CN1731166A (en) * | 2005-08-15 | 2006-02-08 | 厦门大学 | Gold amalgam microelectrode and preparation method thereof |
| CN101685091A (en) * | 2008-09-24 | 2010-03-31 | 西北师范大学 | Method of manufacturing an ultra-microelectrode |
| CN102590302A (en) * | 2011-01-13 | 2012-07-18 | 同济大学 | Method for producing gold nanoarray ultramicroelectrode |
| CN102621204A (en) * | 2012-03-28 | 2012-08-01 | 西北师范大学 | Precious metal ultramicroelectrode and preparation method thereof |
-
2014
- 2014-05-21 CN CN201410215779.9A patent/CN104062336A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5120421A (en) * | 1990-08-31 | 1992-06-09 | The United States Of America As Represented By The United States Department Of Energy | Electrochemical sensor/detector system and method |
| CN1731166A (en) * | 2005-08-15 | 2006-02-08 | 厦门大学 | Gold amalgam microelectrode and preparation method thereof |
| CN101685091A (en) * | 2008-09-24 | 2010-03-31 | 西北师范大学 | Method of manufacturing an ultra-microelectrode |
| CN102590302A (en) * | 2011-01-13 | 2012-07-18 | 同济大学 | Method for producing gold nanoarray ultramicroelectrode |
| CN102621204A (en) * | 2012-03-28 | 2012-08-01 | 西北师范大学 | Precious metal ultramicroelectrode and preparation method thereof |
Non-Patent Citations (1)
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|---|
| 付静: "水环境重金属检测的电化学传感器的研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106033071A (en) * | 2015-03-10 | 2016-10-19 | 中国科学院生物物理研究所 | New Carbon Fiber Electrodes for Patch Clamp Electrochemical Technique Systems |
| CN106033071B (en) * | 2015-03-10 | 2019-05-28 | 中国科学院生物物理研究所 | Novel carbon fiber electrode suitable for patch-clamp electrochemical techniques system |
| CN107102044A (en) * | 2017-05-03 | 2017-08-29 | 西南科技大学 | Sensing electrode for detecting uranyl ions in water and methods of making and using the same |
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Application publication date: 20140924 |
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