CN202159032U - Flatbed moving boundary color development electrophoretic apparatus for detecting heavy metal ions in water - Google Patents
Flatbed moving boundary color development electrophoretic apparatus for detecting heavy metal ions in water Download PDFInfo
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- CN202159032U CN202159032U CN 201120286008 CN201120286008U CN202159032U CN 202159032 U CN202159032 U CN 202159032U CN 201120286008 CN201120286008 CN 201120286008 CN 201120286008 U CN201120286008 U CN 201120286008U CN 202159032 U CN202159032 U CN 202159032U
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Abstract
The utility model relates to a flatbed moving boundary color development electrophoretic apparatus for detecting heavy metal ions in water. The apparatus combines flatbed electrophoresis, supramolecular derivative selecting color development and color development moving boundary electrophoresis methods, adopts the modifiable property and the space structure size controllability of supramolecular substance to form metal ions and supramolecular charged molecular groups with high mass, and adopts electrophoresis moving boundary to perform color development zone concentration mobile display to perform resolution and detection after the metal ions and the supramolecular charge molecular groups are selectively combined with metal ions to be tested. A three-dimensional square groove is arranged on an insulating card or a card processed by chemical inert material, the bottom and the periphery of the square groove do not leak, the length of the groove is 10 to 1000 mm, the width is 1 to 5 mm, and the height is 0.1 to 3 mm; and two inert electrodes are respectively arranged at two ends of the groove. The apparatus overcomes the problem of thermal convection of a free electrophoresis apparatus, ensures that the advantages, simpleness and quick speed of the free moving boundary electrophoresis apparatus are sufficiently achieved, can detect the concentrations of heavy metal ions, cadmium, mercury, lead and chromium in water, realizes the purpose of the expected design, and has practical application value.
Description
Technical field
The utility model belongs to the analytical chemistry field, particularly relates to the flat board that is used for detecting the water heavy metal ion and moves boundary's colour developing electrophoretic apparatus.
Background technology
China is developing country, and distribute extensive, the huge resource-hungry manufacturing enterprise of quantity are arranged.Heavy metals such as lead, cadmium, mercury, chromium are widely used in the commercial production flow process, like battery and electronic devices and components, printing and dyeing and metallurgy industry etc., bring serious heavy metal pollution to environment.In recent years heavy metal pollution events incidence such as China's lead, cadmium, mercury sharply rise, and the harm that causes is startling, have caused that government department pays much attention to, and the heavy metal pollution system of accountability has been carried out in a plurality of provinces, investigates the legal liabilities that pollute the people.Heavy metal pollution becomes the significant problem in environmental health field, in " the 12 " planning of announcing recently, also it is classified as one of main project of environmental pollution improvement.
Heavy metal refers generally to density greater than 4.5g/cm
3Metal, have 45 kinds approximately, like copper, lead, zinc, iron, cobalt, nickel, manganese, cadmium, mercury, chromium, tungsten, molybdenum, gold, silver etc.Although iron, manganese, copper, zinc etc. are the needed trace elements of vital movement, most of heavy metal is not that vital movement institute is essential like lead, mercury, cadmium, chromium etc., and all heavy metals are all toxic to human body above finite concentration.Heavy metal representative aspect environmental pollution typically refers to the significant heavy metal elements of bio-toxicity such as lead, mercury, cadmium, chromium and metalloid arsenic.Because therefore heavy metal can not directly be discharged as all causing environmental pollution in river, lake, ocean or the soil by biodegradation.Heavy metal in the environment finally gets into human body through the enrichment and the biological magnification of food chain, and forms long-term the murder by poisoning.
Up to now, set up the contents of many kinds of heavy metal ion detection method, like atomic absorption spectrum, atomic emission spectrum, biochemical sensor etc.Yet these methods all have its drawback, as sample need pre-service, service condition complicated, can't realize on-the-spotly detecting, detection speed is slow, detect and cost an arm and a leg etc.The act.std method that China's heavy metal detects has: atomic absorption spectrophotometry, atomic fluorescence (AFS), dithizone-extraction AAS, catalysis oscilloscopic polarography.Preceding two kinds of method accuracy and sensitivity are all than higher, and instrument and equipment that still need be large-scale, expensive also carries out in the laboratory, and the length that expends time in can't realize field quick detection.Dithizone-extraction AAS complex operation, and the organic extraction reagent that uses has carcinogenesis, seldom utilization in real work.The catalysis oscilloscopic polarography need be equipped with special-purpose instrument and electrode system.
Some other still be in research state laboratory method; Like stripped atomic emission spectrums (ICP-AES) such as inductive coupling plasma mass (ICP-MS) analytical technology, inductive coupling, high performance liquid chromatography, immunoassay, biology sensor method, enzyme inhibition method etc.; Or need large-scale, expensive instrument and equipment to detect in the laboratory; Or be difficult to prepare the monoclonal antibody of metallic ion, all can not realize the scene of heavy metal ion, fast, detection by quantitative.
Therefore; If can set up a kind of to heavy metal ion in the water fast, accurately, quantitative detecting method cheaply; The early stage proposition environmental hazard early warning of polluting; Will be for hygienic quality supervision monitoring provide reliable index foundation, to preserving the ecological environment and human health has very important significance.
The utility model successfully provides heavy metal ion fast detecting pick-up unit in a kind of brand-new water, and promptly flat board moves boundary's colour developing electrophoresis.Adopt the pick-up unit in the utility model, can realize at short notice (generally being no more than 10min) to heavy metal ion in the water make the scene, fast, detection by quantitative.
Summary of the invention
After utilizing the supermolecule developer that heavy metal ion is carried out specificity selection, colour developing, in dull and stereotyped direct current electrophoresis, the complexing material of this colour developing can directedly move, and gathers a certain zone in the electrophoresis tank, and macroscopic variation takes place.There are correlativity in the area features of color development area and tested concentration of heavy metal ion.This is a kind of brand-new heavy metal ion detection method, and promptly flat board moves boundary's colour developing electrophoresis, and its English name is Plate Moving Coloring Electrophoresis, is abbreviated as PMCEP.
The technical scheme of the utility model is following:
On the card of insulation or chemical inert material processing, the three-dimensional square groove of a horizontal upper shed is set, the bottom and around ne-leakage, this flute length is that 10～1000mm, the wide 1～5mm of being, height are 0.1～3mm; An inert electrode is respectively established at two ends, and one positive one is negative.
Described insulation or chemical inert material are specific inductive capacity＞2kV/mm non electrically conductive material.Preferred insulation or chemical inert material are tygon, polycarbonate, polymethylmethacrylate, dimethyl silicone polymer, polypropylene, glass or quartz.
Operation steps is following:
1) according to the practical methods needs of the metallic ion that will detect, with modified to this metallic ion have the supermolecule chromogenic reagent of high selectivity or regulate electrically, the damping fluid of pH value, add flat board and move the boundary and develop the color in the electrophoresis tank horizontal positioned;
2) successively tens of microlitre detected water sample and chromogenic reagent are added in the disk electrophoresis groove, make the interior reagent mix of groove even, evenly launch;
3) with power supply positive and negative electrode positive and negative electrode in the corresponding electrophoresis tank respectively, connect two electrodes, be adjusted to detection voltage, Current Control in 10mA, energized;
4) when color development area long side direction in the groove in 60s, change＜during 0.5mm, be regarded as reaction terminating; With the length of color development area in the ruler measuring flume, calculate the color development area area;
5) will go up a pacing and calculate the curve equation of substitution correlation activities as a result, calculate the concentration of metallic ion in the sample.
To be metallo-chelate, complex compound, porphyrin, crown ether, cyclodextrin, calixarenes or cup hat be combined into charging property with tested metallic ion to described modifiability supermolecule and make molecular weight improve the complex compound more than 1 times.
The utility model is first with supermolecule specificity selective system, disk electrophoresis, macroscopic view colour developing, the ingenious combination of moving boundary electrophoresis method; Utilize the modifiability of supermolecule material (crown ether, calixarenes etc.) to reach high selectivity to metallic ion; Make itself and metal form the charged particle group of big quality; Change metallic ion in the past because the situation that quality too little, the relatively quantity of electric charge own is big, electrophoresis can't resolved detection, and on existing theoretical basis, designed miniature PMCEP device first.
Metal ion detection device in the utility model and uncomplicated, manipulate very easy: the miniature plate electrophoresis apparatus (card) of a subband inert electrode, power are that several watts adjusting pressuring dc power, is measuring accuracy the ruler instrument of 0.1mm.
Miniature plate electrophoresis apparatus (card): electrophoresis apparatus is made on the edge insulator chip material; The plate substrate material can be PVC (tygon), PC (polycarbonate), PMMA (polymethylmethacrylate), PDMS (dimethyl silicone polymer), PP (polypropylene), glass, quartz etc., also can be the nonconducting chemical inert material of other specific inductive capacity＞2kV/mm.For good in electrophoresis time heat radiation, be unlikely and in electrophoresis tank, cause hot flow-disturbing, the thermal conductivity of material more than 0.15W/mK for well.
The disk electrophoresis groove is the embedding rectangular parallelepiped groove on this insulation cassette material that crouches, and inside is smooth, bright and clean, and flute length is 10～1000mm; Wide is 1～5mm, and the degree of depth is 0.1～3mm, and there are two vertical inert electrodes of sheet at two ends; One positive one is negative, shown in annex map 1-4.During reaction, liquid contacts conduction well in the groove with electrode, no any seepage in the whole rectangular parallelepiped groove.
Adjusting pressuring dc power: general tunable voltage dc power supply can satisfy request for utilization, power≤15W, and voltage≤100V can regulate continuously.Because voltage, electric current also are the conditions that detection needs control, so power supply needs configuration voltages, current indicator.For safe handling, devices such as short circuit insurance, ground connection need be set also.
The technical scheme and the method for inspection explanation of invention
Select respectively to cadmium, mercury, lead, the good supermolecule material of chromium ion selectivity; It is carried out-R side group modifying and decorating; Make it be carried at the group that just develops the color under the specific pH condition; Set up the supermolecule color development system, so both reached the specificity of this four metal ion species is selected, have intuitively when having realized detection again simultaneously, macroscopic chromogenic reaction.Detected water sample and supermolecule developer are added respectively in the disk electrophoresis groove; Metallic ion in the water sample combines with developer, under the effect of DC electric field, carries out the swimming of certain hour; Generally be no more than 10min, make charged substance that show color gather a certain zone in the electrophoresis tank.According to the color development area area, can calculate the concentration of metallic ion in the detected water sample.
Draw through overtesting, there are following relation: Y=A+kS in concentration of metal ions and color development area area in the detected water sample, and wherein Y representes the concentration of metallic ion in the water sample, and unit is mg/L; A is the formula constant term, when being formulated by working curve in the concrete detection method and confirm, corresponding to the simple constant term of regression curve; K is a constant, and area coefficient is corresponding to the concentration independent variable function coefficients that returns working curve; S is final color development area area.When color development area S is rectangle or when square of rule, available simple formula Y=A+kX calculates the relation of colour developing district and tested ionic weight, and X representes color development area length; When color development area when not advising shape; Then the color development area area among the Y=A+kS need be used the calculating of
formula; M, n are the para-curve coefficient of irregular color development area, and measurement gets when the test of the standard working curve of formulating method.
The miniature plate moving boundary electrophoresis groove that the utility model designed; Liquid feeding thin (generally being no more than 1.0mm) in detecting time slot; The area of dissipation that has certain length and width simultaneously; So rely on during electrophoresis the natural circulation of liquid level air can reach radiating effect, overcome the heat radiation convection problem of free electrophoresis, make free moving boundary electrophoresis simply, advantage shows performance completely fast.Through the actual tests checking, this method can detect the concentration of heavy metal ion cadmium, mercury, lead, chromium in the water sample, reaches the purpose of utility model desired design, has actual application value.
Description of drawings
Fig. 1: the utility model device synoptic diagram.
Fig. 2: the supermolecule chromogenic reagent synoptic diagram of in PVC card upper flat plate electrophoresis tank, annotating during use.
Fig. 3: add water sample synoptic diagram to be checked.
Fig. 4: synoptic diagram as a result develops the color behind the electrophoresis.
Annotate: among the figure "+,-" respectively expression come from the positive and negative electrode of conventional dc power supply; Between the positive and negative polarities binding post, dashed region is represented added sample or test solution in the use on the PVC card, the real black region on corresponding Fig. 4, and this district's color changes behind the expression electrophoresis.
Embodiment
As shown in Figure 1, this device is the miniature plate electrophoresis tank, adopts PVC insulation card, establishes the square groove that the length and width height is about 50.0mm * 3.0mm * 1.0mm on the card, reaches bottom surface flat-satin, sealing ne-leakage all around.Positive and negative inert electrode is established, external direct current power supply, average voltage 2～20V/cm in two ends in the groove.
As required, can select tygon, polycarbonate, polymethylmethacrylate, dimethyl silicone polymer, polypropylene, glass or quartz for use in insulation or chemical inert material.
The three-dimensional square groove of card, the bottom and around ne-leakage, it is that 10～1000mm, the wide 1～5mm of being, height are 0.1～3mm that this groove can be set to length; An inert electrode is respectively established at two ends, and one positive one is negative.
This Device Testing method practical implementation step is following:
The first step: according to the practical methods needs of the metallic ion that will detect; This metallic ion is had the supermolecule chromogenic reagent of high selectivity or regulates damping fluid electrical, the pH value with modified; Adding flat board moves in boundary's colour developing electrophoresis tank; Horizontal positioned is avoided because of device tilts to cause liquid level interruption between the both positive and negative polarity, shown in accompanying drawing 2;
Second step: successively tens of microlitre detected water sample and chromogenic reagent are added in the disk electrophoresis groove, make the interior reagent mix of groove even, make its even expansion, shown in accompanying drawing 3;
The 3rd step: with positive and negative electrode in the corresponding electrophoresis tank of power supply positive and negative electrode difference, connect two electrodes, be adjusted to detection voltage, Current Control begins the electrophoresis timing in the time of energized in 10mA;
The 4th step: when color development area long side direction in the groove in 60s, change＜during 0.5mm, be regarded as reaction terminating.With the length of color development area in the ruler measuring flume, calculate the color development area area;
The 5th step: will go up a pacing and calculate the curve equation of substitution correlation activities as a result, and calculate the concentration of metallic ion in the sample.
Adopt the supermolecule in the utility model to select flat board to move boundary's colour developing electrophoresis method, successful implementation is to quick, the detection by quantitative of cadmium, lead, mercury, chromium ion in the water.
Embodiment 1 adopts cadmium ion and cadion to form 1: 4 co-ordination complex, successfully realizes quick, detection by quantitative to cadmium ion in the water sample:
During detection, add cadion (Cadion, CAS number: 5392-67-6) the ammoniacal liquor damping fluid of solution 20 μ l, 1M (regulating pH value to 11) and detected water sample 10 μ l; After mixing, solution shows darkviolet, the electronegative property of cadmium ion complex compound; After connecting the direct supply of 75V, 8mA; Through the electrophoresis of 2～10min, the district of sepia colour developing intuitively occurs and move, finally gather near the positive electrode region.Through measuring the length of color development area, can calculate the testing result of cadmium in the water sample.
Experimental result shows: be fixed as at the disk electrophoresis well width under the situation of 2mm, the colour developing section length satisfied relational expression: Y=0.15+0.1X basically after concentration of cadmium ions and electrophoresis moved the boundary in the water sample, and correlation coefficient r is 0.8977.In the formula: Y is a concentration of cadmium ions in the detected water sample, and unit is mg/L, and X is the colour developing section length, and unit is mm.20 μ l sampling, sensing range is 0.010～5.0mg/L.The accuracy of method and precision: when the sample concentration of cadmium ions was 0.1mg/L, the relative error of measurement was 6%, and RSD (relative standard deviation) is 2%.
Embodiment 2 utilizes the crown ether supermolecule that the specificity of metallic ion is selected, and process successfully realizes quick, detection by quantitative to lead ion in the water after modifying and carrying the colour developing group:
Modify methyl thymol blue (MTB) fast eolor base in the scion grafting with phendioxin 8-crown ether-6; Do solubilizer with ethanol; In hexamethylenetetramine-hydrochloride buffer medium of pH=6,, generate blue lead ion complex compound with lead generation chromogenic reaction; Complex compound positively charged property, disk electrophoresis setback line colour developing district is near negative electrode region.
During detection, add phendioxin 8-crown ether-6 liquid 15 μ l, 95% ethanolic solution, 10 μ l, detected water sample 10 μ l after modifying successively, after mixing; Solution shows skipper; After connecting the direct supply of 25V, 4mA, through the electrophoresis of 2～8min, the lead ion complex compound is under electrophoresis drives; Assemble colour developing and move near the negative electrode region the light blue intuitively colour developing of appearance district.Through measuring the length in colour developing district, can calculate testing result plumbous in the water sample.
Experimental result shows, is fixed as at the disk electrophoresis well width under the situation of 2mm, and the colour developing section length satisfied relational expression: Y=0.09+0.47X basically after plumbum ion concentration and electrophoresis moved the boundary in the water sample, and correlation coefficient r is 0.8892.In the formula: Y is the concentration of lead ion in the detected water sample, and unit is mg/L, and X is an electrophoresis colour developing section length, and unit is mm.20 μ l sampling, sensing range is 0.10～10.0mg/L.The accuracy of method and precision: when the sample lead ion content was 0.2mg/L, the relative error of measurement was 5%, and RSD (relative standard deviation) is 3%.
The calixarenes molecule that embodiment 3 utilizes after modifying, successfully realize quick, detection by quantitative to mercury ion in the water:
As third generation main body super molecular compound, calixarenes has unique void structure, through controlling the differential responses condition and introducing suitable substituting group, can fix the conformation that all need.In the derivatization modification reaction of calixarenes; The not only phenyl ring contraposition of the phenolic hydroxyl group of lower edge and upper limb; And the methylene that connects the phenyl ring unit can both carry out various selectivity function modifications; This both can improve the deficiency of the poorly water-soluble of calixarenes own, can strengthen the ability of its complexation of metal ions and neutral molecule again greatly.With calixarenes and 2,4-dinitroaniline colour developing group is connected, when pH=6.5 with mercury ion formation red complex.Complex compound shows slightly electropositivity, and disk electrophoresis setback line colour developing district is near negative electrode region.In this method, the cadmium of content has color interference more than 10 times.
During detection, add successively and connect 2 of modified, 4-dinitroaniline-cup [4] aromatic hydrocarbons liquid 20 μ l, 0.005M dilution heat of sulfuric acid 10 μ l, detected water sample 10 μ l; After mixing, solution shows dark yellow, behind the direct supply of connection 25V, 4mA; Electrophoresis through 2～8min; The mercury ion complex compound is assembled colour developing and is moved near the negative electrode region the red intuitively colour developing of appearance district under electrophoretic action drives.Through measuring the length in colour developing district, can calculate the testing result of mercury in the water sample.
Experimental result shows: be fixed as at the disk electrophoresis well width under the situation of 2mm, the colour developing section length satisfied relational expression: Y=0.09+0.47X basically after ion concentration of mercury and electrophoresis moved the boundary in the water sample, and correlation coefficient r is 0.9011.In the formula: Y is for detecting the concentration of mercury ion in the water sample, and unit is mg/L, and X is an electrophoresis colour developing section length, and unit is mm.20 μ l sampling, sensing range is 0.10～5.0mg/L.The accuracy of method and precision: when the sample mercury ion was 0.5mg/L, the relative error of measurement was 7%, and RSD (relative standard deviation) is 4%.
Embodiment 4 utilizes diphenylcarbazide and hexavalent chromium in acid medium, to form 3: 2 red complexs, successfully realizes quick, detection by quantitative to hexavalent chromium in the water sample:
Because diphenylcarbazide is insoluble in water, does solubilizer with the ethanol diphenylcarbazide, aqueous sulfuric acid is as electrophoretic buffer.During detection, add ethanol diphenylcarbazide solution 20 μ l, 0.2M phosphate buffer 10 μ l, detected water sample 10 μ l successively, after mixing, it is red that solution shows.Ionic complex is electronegative electrically; After connecting the direct supply of 25V, 8mA, through the electrophoresis of 2～10min, the chromium ion complex compound is under the driving of electrophoresis; Assembling colour developing distinguishes and moves near the positive electrode region; The district of kermesinus colour developing intuitively occurs, color development area is that an end para-curve is irregularly shaped, and is shown in Figure 4 like annex.Through test, find that the area in colour developing district becomes the positive correlation proportionate relationship with detected water sample hexavalent chromium content, concern thus, can calculate the testing result of chromium in the water sample.
Experimental result shows; Be fixed as at the disk electrophoresis well width under the situation of 2mm; The colour developing section length satisfied relational expression: Y=0.05+0.21S basically after hexavalent chromium concentration and electrophoresis moved the boundary in the water sample; Wherein
m equals constant 0.47, n equals constant 0.5, correlation coefficient r is 0.9372.In the formula: Y is for detecting the concentration of hexavalent chromium in the water sample, and unit is mg/L, and X is an electrophoresis colour developing section length, and unit is mm.20 μ l sampling, sensing range is 0.07～2.0mg/L.The accuracy of method and precision: when chromium ion concentration was 0.25mg/L in the sample, the relative error of measurement was 4%, and RSD (relative standard deviation) is 2%.
Realized respectively in the test of the utility model the fast quantification of cadmium, lead, mercury, chromium in the water is detected, the detection of each simple sample can be accomplished in 10min, and obtains accurate result.Easy and simple to handle, even without the people of specialty chemical knowledge,, also can in several minutes, accomplish the detection task according to easy operation instructions.This method has simple, quick, quantitative, economic advantage, has on-the-spot practicality, can satisfy the requirement of laboratory and on-the-spot check and analysis.
The above instance only is to be the embodiment that proves absolutely that the utility model is lifted, and the protection domain of the utility model is not limited thereto.Being equal to that the technician in present technique field is done on the utility model basis substitutes or conversion, all within the protection domain of the utility model.The protection domain of the utility model is as the criterion with claims.
Claims (3)
1. flat board moves boundary colour developing electrophoresis and is used for underwater gold and belongs to ion detection device; It is characterized in that on the dull and stereotyped card of insulation or chemical inert material processing; The cube square groove of a horizontal upper shed is set; The bottom and around ne-leakage, this flute length is that 10～1000mm, the wide 1～5mm of being, height are 0.1～3mm; An inert electrode is respectively established at two ends: one just, one negative.
2. device as claimed in claim 1 is characterized in that described insulation or chemical inert material are specific inductive capacity＞2kV/mm non electrically conductive material.
3. device as claimed in claim 1 is characterized in that described insulation or chemical inert material are tygon, polycarbonate, polymethylmethacrylate, dimethyl silicone polymer, polypropylene, glass or quartz.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102411025A (en) * | 2011-08-08 | 2012-04-11 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Flat-bed moving boundary color development electrophoresis and device for detecting heavy metal ions in water |
| CN103323503A (en) * | 2012-03-22 | 2013-09-25 | 宁波大学 | Electrical enhancement absorption coloration method for rapid on-site detection of cooper ions in aqueous solution, and apparatus thereof |
| CN103512929A (en) * | 2012-06-18 | 2014-01-15 | 宁波大学 | Electric enhanced color development method and device thereof for rapid detection of lead ions or ferrous ions |
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2011
- 2011-08-08 CN CN 201120286008 patent/CN202159032U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102411025A (en) * | 2011-08-08 | 2012-04-11 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Flat-bed moving boundary color development electrophoresis and device for detecting heavy metal ions in water |
| CN103323503A (en) * | 2012-03-22 | 2013-09-25 | 宁波大学 | Electrical enhancement absorption coloration method for rapid on-site detection of cooper ions in aqueous solution, and apparatus thereof |
| CN103323503B (en) * | 2012-03-22 | 2015-06-17 | 宁波大学 | Electrical enhancement absorption coloration method for rapid on-site detection of cooper ions in aqueous solution, and apparatus thereof |
| CN103512929A (en) * | 2012-06-18 | 2014-01-15 | 宁波大学 | Electric enhanced color development method and device thereof for rapid detection of lead ions or ferrous ions |
| CN103512929B (en) * | 2012-06-18 | 2015-08-19 | 宁波大学 | The electricity of a kind of quick detection lead ion or ferrous ion strengthens coloration method and device thereof |
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Granted publication date: 20120307 Termination date: 20130808 |