CN108663351A - A kind of super object detection method of heavy metal-polluted soil - Google Patents

A kind of super object detection method of heavy metal-polluted soil Download PDF

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Publication number
CN108663351A
CN108663351A CN201810461425.0A CN201810461425A CN108663351A CN 108663351 A CN108663351 A CN 108663351A CN 201810461425 A CN201810461425 A CN 201810461425A CN 108663351 A CN108663351 A CN 108663351A
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China
Prior art keywords
heavy metal
electrochromic
ion
detection method
film
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CN201810461425.0A
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Chinese (zh)
Inventor
郭素文
郑岩
陈磊
全丽华
陈君燕
耿树范
范宏伟
刘洁
周金水
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SHANGHAI DONGZHOU INDUSTRIAL Co Ltd
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SHANGHAI DONGZHOU INDUSTRIAL Co Ltd
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Priority to CN201810461425.0A priority Critical patent/CN108663351A/en
Publication of CN108663351A publication Critical patent/CN108663351A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence

Abstract

A kind of super object detection method of heavy metal-polluted soil of the present invention.The present invention by using heavy metal ion conductive characteristic, utilize the structural advantage of electrochromic device, soil to be measured is passed through into drying, the techniques such as acidolysis are configured to detection stoste, at kit both ends plus by the discoloration rate probability of measurement device being initial discoloration rate after voltage;The sample solution that need to be tested is added in anode after colour fading, conductive heavy metal ion in sample moves to cathode under the action of electric current by ionic membrane, then charge transfer is realized to the increase and decrease of discoloration rate to electrochromic material, then by measuring discoloration rate compared with initial discoloration rate, the testing result of qualitative, quantitative is obtained.The testing result of quick visualization may be implemented in the present invention, and equipment is light, and monitoring is simple for process, it is easy to carry about with one, Soil Testing has powerful advantage in the wild, while in sewage heavy metal analysis, and the public safety fields such as food heavy metal analysis have preferable application prospect.

Description

A kind of super object detection method of heavy metal-polluted soil
Technical field
The invention belongs to electrochemistry environmental testing application.
Background technology
With the aggravation of continuous development and the environmental pollution of modern industrial technology, in recent years, soil contamination problem increasingly draws Play the attention of people.Especially heavy metal contamination, the content of minor metallic element in the soil are more than background value, excessive heavy Too high levels caused by product can eventually lead to food security.It is by food chain approach in plant, animal and human body inner product It is tired, serious threat is all constituted to ecological environment, food security and health.Therefore, reinforce to farmland soil heavy metals It is monitored and controlled, is of great significance for effective prevention and control heavy metal pollution.
Traditional heavy metal-polluted soil detection method is to be sampled Hou Song specialized laboratories to soil, using atomic absorption light Spectrometry (AAS), atomic emission spectrometry (AES), inductively coupled plasma mass spectrometry (ICP-MS) etc. are detected.These sides Method all have preferable detection sensitivity and accuracy, but major defect be equipment instrument is big, expensive, analysis time is long, Flow is complicated.China's national territorial area is vast, be badly in need of a kind of quick, cheap, easy to operation method to heavy metal pollution of soil into The quick detect and assess of row.Chinese patent CN107271395A discloses a kind of high precision soil heavy metal analysis device, including Sampler, sectioning, detection device and analysis process system and data system, the sampler include sampler barrel, cut Mouthful device, supporting rack and regulating device, sampler barrel are linked together by connecting seat and regulating device, supporting rack by support base and Several support bar groups are at supporting rod is separately mounted to support base bottom end and is supported, and sectioning includes drawing mechanism and sanction Cutting apparatus, the drawing mechanism and cutting means are arranged inside sampler barrel, detection device include cleaning device, detection cell and Spectrum detection device, the detection cell and spectrum detection device are installed in fixed seating face.Testing result of the present invention is accurate, just Fast sampling and detection are carried out in the soil to different depth, contributes to people to understand soil regime in time, contributes to soil Protection and improvement, are worthy to be popularized.The invention can accurately detect the exceeded content of heavy metal in soil, but characterization processes are multiple Miscellaneous, equipment cost is more high-leveled and difficult with mass.
The present invention will be waited for by using the conductive characteristic of heavy metal ion using the structural advantage of electrochromic device It surveys soil and is configured to detection stoste by techniques such as drying, acidolysis, pass through measurement device after kit both ends are plus voltage Discoloration rate probability is initial discoloration rate;The sample solution that need to be tested is added in anode after colour fading, the conductive huge sum of money in sample Belong to ion and cathode is moved to by ionic membrane under the action of electric current, charge transfer is realized to electrochromic material then and is changed colour The increase and decrease of rate obtains the testing result of qualitative, quantitative then by measuring discoloration rate compared with initial discoloration rate.
The testing result of quick visualization may be implemented in the present invention, and equipment is light, and monitoring is simple for process, is easy to take Band, in the wild Soil Testing have powerful advantage, while in sewage heavy metal analysis, the public peace such as food heavy metal analysis There is preferable application prospect in full field.
Invention content
A kind of super object detection method of heavy metal-polluted soil;It includes two layers of electrode of electrochromic structure, and conductive ion is molten Liquid, by the electrochromic film of ion film process;By will treated between electrochromic film is placed in two layers of electrode, will with just The electrode definition of pole connection is anode, is cathode by the electrode definition being connect with cathode;By treated, conductive ion is placed in sun Polar region domain, by treated, electrochromic material is placed in cathode zone;Anode is added as an aqueous solution after soil treatment to be measured Region adds certain voltage at the two poles of the earth after being sufficiently mixed uniformly, qualitative, quantitative is obtained by observing the discoloration of cathode Testing result.
A kind of super object detection method of heavy metal-polluted soil;Electrochromic structure described in it is that two layers of electrode is placed in reagent Box both ends connect positive and negative anodes, conductive base are added between kit positive and negative anodes the two poles of the earth, conductive base is selected as transparent and leads It is one or more in the transparent transparent conductive film of electrolemma, graphene or nano-silver thread transparent conductive film, selected transparent electrode The change colour efficiency of testing result is not influenced;Then the knot for realizing heavy metals exceeding standard detection by the way that voltage is added between the two poles of the earth Fruit.
A kind of super object detection method of heavy metal-polluted soil;Conductive ion solution described in it be with contain conductive ion lithium, The salt of sodium is dissolved in aqueous solution, is configured to certain density conductive ion solution and anode region is added, then add in cathode zone Enter excessive electrochromic material, conductive ion is moved to cathode according to current direction from anode after electrode both ends are powered, and occurs Color change, when detecting in sample containing heavy metal ion, color change is deepened after energization, according to changing for discoloration To the testing result of qualitative, quantitative.
A kind of super object detection method of heavy metal-polluted soil;PVB carriers described in it pass through using propene carbonate as solvent system It is standby at carrier paste, it is electrochromic material PEDOT, Prussian blue, one or more in nanometer tungsten oxide, then will be electric Electrochromic film is prepared by hot pressing mode after causing off-color material to be added in carrier paste by a certain percentage;Then electroluminescent Each compound one layer of ionic membrane of color shifting film surface, only allow cationic ion by by other substances such as anion can not pass through, it is real Single side controllable color change is showed.
A kind of super object detection method of heavy metal-polluted soil;Pass through measuring appliance after kit both ends are plus voltage described in it The discoloration rate probability of part is initial discoloration rate;Be added the sample solution that need to test in anode after colour fading, in sample in lead Electric heavy metal ion moves to cathode under the action of electric current by ionic membrane, then gives charge transfer to electrochromic material reality The now increase of discoloration rate, electrochromism kit are powered after the completion of detection, and the kit after discoloration is sharp under the irradiation of light source With CCD systematic surveys light by being defined as discoloration rate, then by measuring discoloration rate compared with initial discoloration rate, according to discoloration The change of rate obtains the testing result of qualitative, quantitative.
Description of the drawings
Fig. 1 electrochemical detecting reagent boxes,
Fig. 2 electrochromic films,
Structure is in figure:
1 anode,
2 cathodes,
3 electrochromic films,
4 conductive ions,
5 electrochromic materials,
6 adding mouths,
7 ionic membranes.
Specific implementation mode
A kind of super object detection method of heavy metal-polluted soil;It includes two layers of electrode of electrochromic structure, and conductive ion is molten Liquid, by the electrochromic film of ion film process;By will treated between electrochromic film is placed in two layers of electrode, will with just The electrode definition of pole connection is anode, is cathode by the electrode definition being connect with cathode;By treated, conductive ion is placed in sun Polar region domain, by treated, electrochromic material is placed in cathode zone;Its detection method is after kit both ends are plus voltage It is defined as initial discoloration rate by the discoloration rate probability of measurement device;Discoloration restores to original state after colour fading, then will Pedotheque to be measured using acidic solution hydrolysis sample, is added anode region, fills as an aqueous solution after drying after processing Divide and add certain voltage at the two poles of the earth after mixing, when containing heavy metal ion in aqueous solution, passes through the change for observing cathode Pornographic condition obtains the testing result of qualitative, quantitative.
A kind of super object detection method of heavy metal-polluted soil;Electrochromic structure described in it is that two layers of electrode is placed in reagent Box both ends connect positive and negative anodes, conductive base are added between kit positive and negative anodes the two poles of the earth, conductive base is selected as transparent and leads It is one or more in the transparent transparent conductive film of electrolemma, graphene or nano-silver thread transparent conductive film, selected transparent electrode For the KPT-3 models that Shanghai Keyan Opto-electrical Technology Co., Ltd provides, transmitance reaches 85% or more, the discoloration to testing result Efficiency does not influence;Then the result for realizing heavy metals exceeding standard detection by the way that voltage is added between the two poles of the earth.
A kind of super object detection method of heavy metal-polluted soil;Conductive ion solution described in it be with contain conductive ion lithium, The salt of sodium is dissolved in aqueous solution, is configured to certain density conductive ion solution and anode region is added, then add in cathode zone Enter excessive electrochromic material, conductive ion is moved to cathode according to current direction from anode after electrode both ends are powered, and occurs Color change, when detecting in sample containing heavy metal ion, color change is deepened after energization, according to changing for discoloration To the testing result of qualitative, quantitative.
A kind of super object detection method of heavy metal-polluted soil;PVB carriers described in it pass through using propene carbonate as solvent system It is standby at carrier paste, it is electrochromic material PEDOT, Prussian blue, one or more in nanometer tungsten oxide, then will be electric Electrochromic film is prepared by hot pressing mode after causing off-color material to be added in carrier paste by a certain percentage;Then electroluminescent Each compound one layer of ionic membrane of color shifting film surface, only allow cationic ion by by other substances such as anion can not pass through, it is real Single side controllable color change is showed.
A kind of super object detection method of heavy metal-polluted soil;Pass through measuring appliance after kit both ends are plus voltage described in it The discoloration rate probability of part is initial discoloration rate;The sample solution that need to be tested, the conduction in sample is added in anode after colour fading Heavy metal ion moves to cathode under the action of electric current by ionic membrane, then realizes charge transfer to electrochromic material The increase of discoloration rate obtains the testing result of qualitative, quantitative then by measuring discoloration rate compared with initial discoloration rate.
A kind of super object detection method of heavy metal-polluted soil;The DC voltage for adding 1-3V at kit both ends first, passes through The discoloration rate for measuring cathode zone is defined as initial discoloration rate, and as with reference to standard, then plus backward voltage is until fade to just Beginning state;Then anode region is added in test sample after treatment, is sufficiently mixed 3-5min, then add voltage, by In the presence of ionic membrane, only cation can be reached cathode zone generation metachromasia by ionic membrane, define change at this time Color rate is sample discoloration rate, by obtaining the testing result of qualitative, quantitative compared with initial discoloration rate.
A kind of super object detection method of heavy metal-polluted soil;The testing result of quick visualization may be implemented in the present invention, and Equipment is light, and monitoring is simple for process, is easy to carry about with one, Soil Testing has powerful advantage, while disease in vitro in the wild The public safety fields such as detection field, sewage heavy metal analysis, food heavy metal analysis have preferable application prospect, Ke Yishi Now fast and accurately Visual retrieval detection method.
Advantage of the present invention
Preparation process is simple compared with prior art by the present invention, by being simply hot pressed into film preparation core devices structure, cost It puts into low.
Present invention process process operating process controllability is higher, and entire inspection can be directly prepared by microelectronic packaging process Test agent box is easy to industrialize continuous production.
Present invention process environmental requirement is simple, only need under vacuum be completed during package curing, institute Low with production cost, process controllability is high.
Of the present invention is nontoxic and pollution-free material, in production process will not generation environment harm, electrolyte Ion uses the technique of film-forming, substantially increases its security performance used, improves reuse efficiency, reducing makes Use cost.
Make after illustrating above for the present invention, to one skilled in the art it is to be understood that the subject area not In the case of deviateing the spirit and scope of the present invention, any changes and improvements made for the present invention are all in the scope of the present invention It is interior.

Claims (7)

1. a kind of super object detection method of heavy metal-polluted soil;It includes two layers of electrode of electrochromic structure, conductive ion solution, By the electrochromic film of ion film process;By will treated between electrochromic film is placed in two layers of electrode, will be with anode The electrode definition of connection is anode, is cathode by the electrode definition being connect with cathode;By treated, conductive ion is placed in anode Region, by treated, electrochromic material is placed in cathode zone;Anode region is added as an aqueous solution after soil treatment to be measured Domain adds certain voltage at the two poles of the earth after being sufficiently mixed uniformly, qualitative, quantitative is obtained by observing the discoloration of cathode Testing result.
2. a kind of super object detection method of heavy metal-polluted soil as described in claim 1;Electrochromic structure described in it is will Two layers of electrode is placed in kit both ends, connects positive and negative anodes, conductive base, conductive base is added between kit positive and negative anodes the two poles of the earth Be selected as it is one or more in the transparent transparent conductive film of ITO nesa coating, graphene or nano-silver thread transparent conductive film, so The result for realizing heavy metals exceeding standard detection by the way that voltage is added between the two poles of the earth afterwards.
3. a kind of super object detection method of heavy metal-polluted soil as described in claim 1;Conductive ion solution described in it be with Salt containing conductive ion lithium, sodium is dissolved in aqueous solution, and conductive ion is moved according to current direction and transmitted after electrode both ends are powered Charge realizes metachromatism.
4. a kind of super object detection method of heavy metal-polluted soil as described in claim 1;Described in it by ion film process Electrochromic film be using PVB as carrier material, by electrochromic material and carrier material after mixing hot pressing be prepared into it is electroluminescent Color-changing membrane, then in each compound one layer of ionic membrane of electrochromism film surface, only allow cationic ion by anion etc. other Substance can not pass through, and realize single side controllable color change.
5. the electrochromic film Jing Guo ion film process as claimed in claim 4;PVB carriers described in it pass through with carbonic acid third Enester is that solvent is prepared into carrier paste, electrochromic material PEDOT, Prussian blue, in nanometer tungsten oxide one kind or It is a variety of, electrochromism is prepared by hot pressing mode after being then added to electrochromic material in carrier paste by a certain percentage Film.
6. a kind of super object detection method of heavy metal-polluted soil as described in claim 1;Being added at kit both ends described in it After voltage by the discoloration rate probability of measurement device be initial discoloration rate;It is molten in anode the sample that need to test to be added after colour fading Liquid, in sample in conductive heavy metal ion cathode is moved to by ionic membrane under the action of electric current, then by charge transfer The increase and decrease of discoloration rate is realized to electrochromic material, then by measuring discoloration rate compared with initial discoloration rate, is obtained qualitative Quantitative testing result, while in sewage heavy metal analysis, the public safety fields such as food heavy metal analysis, which have, preferably answers Use foreground.
7. a kind of super object detection method of heavy metal-polluted soil as described in claim 1, the energization of electrochromism kit has detected Cheng Hou, by the kit after discoloration under the irradiation of light source using CCD systematic surveys light by being defined as discoloration rate, according to discoloration The change of rate obtains the testing result of qualitative, quantitative.
CN201810461425.0A 2018-05-15 2018-05-15 A kind of super object detection method of heavy metal-polluted soil Pending CN108663351A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111812082A (en) * 2020-07-01 2020-10-23 淮阴工学院 Photoelectrochemistry electrochromism indirect analysis and detection device and manufacturing method thereof
CN114729920A (en) * 2019-10-29 2022-07-08 P.E.S.科技有限公司 Analysis system for volatile organic compounds in soil

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Publication number Priority date Publication date Assignee Title
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CN104407041A (en) * 2014-11-25 2015-03-11 苏州市欧博锐自动化科技有限公司 Method for automatic detection of concentration of heavy metal ions in soil and soil remediation
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114729920A (en) * 2019-10-29 2022-07-08 P.E.S.科技有限公司 Analysis system for volatile organic compounds in soil
CN111812082A (en) * 2020-07-01 2020-10-23 淮阴工学院 Photoelectrochemistry electrochromism indirect analysis and detection device and manufacturing method thereof

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