CN108132214B - Method for rapidly detecting heavy metals in water based on super-infiltration microchip - Google Patents
Method for rapidly detecting heavy metals in water based on super-infiltration microchip Download PDFInfo
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- CN108132214B CN108132214B CN201810049539.4A CN201810049539A CN108132214B CN 108132214 B CN108132214 B CN 108132214B CN 201810049539 A CN201810049539 A CN 201810049539A CN 108132214 B CN108132214 B CN 108132214B
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 28
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- 238000000034 method Methods 0.000 title claims abstract description 17
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- 238000001514 detection method Methods 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
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- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical group CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 claims description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 2
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- 238000010586 diagram Methods 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
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- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1813—Specific cations in water, e.g. heavy metals
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Abstract
A method for rapidly detecting heavy metals in water based on a super-infiltration microchip belongs to the field of material preparation and chemical detection and analysis. Firstly, hydrophobic silica particles and fluorosilane react in an ethanol solution to prepare a super-hydrophobic silica suspension; then coating the suspension on one side of a double-sided adhesive tape to obtain a super-hydrophobic surface; and finally, carrying out plasma etching in a designated area to obtain super-hydrophilic micropores to obtain a super-infiltrated chip, and adhering the super-infiltrated chip to a specific substrate device by using the viscosity of the adhesive tape. The super-wetting chip can concentrate and enrich the color reagent on the super-hydrophilic micropores, the prepared super-wetting chip can fix the detected liquid on the super-hydrophilic sites through simple dipping operation, and the colorimetric detection is realized by utilizing the detection reagent fixed on the hydrophilic sites. The method not only solves the problem of high cost of the traditional instrument analysis method, but also solves the problem of complex operation of the chemical analysis method, and is suitable for rapid field detection of aqueous solution.
Description
Technical Field
The invention relates to the field of material preparation and chemical detection and analysis, in particular to a method for rapidly detecting heavy metals in water based on a super-infiltration microchip.
Background
Water pollution is one of the most serious environmental problems facing the world today. With the development of industry and the improvement of human living standard, more and more pollutants are thrown into natural water bodies, and the normal operation of an ecological system is threatened. Wherein, heavy metals in water such as hexavalent chromium can invade human body through digestion, respiratory tract, skin and mucosa, thus being harmful to human health.
The rapidness and the simplicity are always one of the targets pursued by the detection technology. Currently, detection technologies commonly used for detecting heavy metal ions in water, such as instrumental analysis methods (atomic absorption spectrometry, ultraviolet-visible spectrophotometry and voltammetry), require complex instruments and operation methods, are not portable, and have high requirements on professional levels of operators; chemical analysis methods (chemical titration method and colorimetric method) are simple in equipment, but still need tedious sampling, titration and oscillation operations, and are time-consuming and labor-consuming.
Generally, one defines a superhydrophobic interface as an interface with a contact angle greater than 150 ° and a superhydrophilic interface as an interface with a contact angle less than 5 °. The super-wetting microchip designs super-hydrophobic and super-hydrophilic on the same material, and achieves the effects of capturing and fixing micro-droplets by utilizing two extreme interface states. Wherein, the super-hydrophilic micropores can effectively attract the liquid drops, and the super-hydrophobic areas around the micropores can effectively limit the movement of the liquid drops.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for rapidly detecting heavy metals in water quality based on a super-infiltration microchip.
A method for rapidly detecting heavy metals in water quality based on a super-infiltration microchip comprises the following steps: the device comprises a substrate device, a double-sided adhesive tape and a super-hydrophobic nano silicon dioxide coating; the substrate is one or more of metal, rubber, glass and ceramic; one side of the double-sided tape is release paper, and the other side of the double-sided tape is adhesive; the super-hydrophobic nano-silica coating is coated on one surface of the release paper of the double-sided adhesive tape by a linear coating method, and super-hydrophilic micropores are arranged at specific positions on the coating.
Further, the preparation method of the super-wetting microchip is as follows:
step one, preparing a super-hydrophobic nano silicon dioxide suspension: sequentially adding hydrophobic nano-silica particles and low-surface-energy substances into an absolute ethyl alcohol solution, magnetically stirring at room temperature for 20-30min, and then performing ultrasonic treatment for 20-30min to obtain a super-hydrophobic nano-silica suspension;
step two, preparation of the super-infiltration microchip: coating the super-hydrophobic nano-silica suspension liquid obtained in the step one on one side of release paper of a double-sided adhesive tape by using a wire bar coater, and air-drying at room temperature to volatilize a solvent to obtain a super-hydrophobic nano-silica coating; performing plasma etching on a photomask plate for 5-8min, forming super-hydrophilic micropores through the area of the holes on the photomask plate, and obtaining a super-wetting chip by using the other areas as super-hydrophobic areas;
and step three, attaching the super-infiltrated microchip obtained in the step two to equipment.
Further, the surface of the hydrophobic nano silicon dioxide is modified by polydimethylsiloxane, and the low surface energy substance is 1H,1H,2H, 2H-perfluorooctyltriethoxysilane.
Further, the coating thickness can be controlled to be 100-; the photomask plate is clamped and fixed on the super-hydrophobic silicon dioxide coating through the long tail clamp.
Furthermore, the invention relates to a method for rapidly detecting heavy metal in water quality based on a super-infiltration microchip, which adopts a colorimetric method to detect heavy metal ions in water quality. The heavy metal ions include divalent nickel, hexavalent chromium, and divalent copper ions.
Further, dropping heavy metal detection reagent on the super-hydrophilic micropores of the super-wetted microchip, naturally drying at room temperature, and depositing and enriching effective components in the detection reagent on the super-hydrophilic micropores along with solvent volatilization
Furthermore, the substrate equipment adhered with the super-wetting microchip is directly dipped with the heavy metal solution, droplets of the heavy metal solution are captured and fixed through the super-hydrophilicity of the micropores and the super-hydrophobicity of the non-micropore area, the droplets are enriched in the super-hydrophilicity micropore area, and effective components in the detection reagent and heavy metal ions in the solution undergo colorimetric reaction to generate color signals, so that the detection purpose is achieved.
The invention utilizes the interface difference of the super-hydrophobic and super-hydrophilic on the microchip, directly dips the detected liquid without sampling after the detection reagent is concentrated and fixed on the super-hydrophilic micropores, and can achieve the detection purpose by a colorimetric method. The method solves the problem of high cost of the traditional instrument analysis method and the problem of complex operation of the chemical analysis method, and is suitable for rapid field detection of aqueous solution.
Drawings
FIG. 1 is a scanning electron microscope characterization of the superhydrophobic silica coating.
Figure 2a shows the super wetting microchip super hydrophobic surface contact angle characterization chart.
FIG. 2b is a graph showing the contact angle of the super-hydrophilic micropores in the super-wetted microchip
Figure 3 shows the super wetting microchip contact angle comparison of real object.
FIG. 4a shows a schematic representation of a super-wetted microchip on tweezers.
FIG. 4b shows a schematic representation of a super-wetted microchip on a glass rod.
Figure 4c shows the glove super immersion microchip physical map.
FIG. 5a is a schematic diagram of a drop capture by a super-wetted microchip in a nested fashion.
FIG. 5b is a schematic representation of the drop capture by the super-wetted microchip in a pull-up fashion.
FIG. 5c is a schematic representation of the dipping mode of droplet capture by the super-wetted microchip.
Figure 6 shows a histogram of the volume of droplets captured by different hydrophilic pore sizes.
FIG. 7 is a schematic diagram showing the concentration and enrichment process of heavy metal analytes in super-wet micro-pores.
FIG. 8 is a schematic diagram of the present invention for providing rapid detection of heavy metals.
FIG. 9a is a pictorial representation of a sample prepared for nickel detection in accordance with the present invention.
FIG. 9b is a diagram of a nickel test dipping motion embodiment provided by the present invention.
FIG. 9c is a diagram of a nickel detection chromogenic reaction entity provided by the present invention.
FIG. 10 is a scattering diagram of the gray value versus the concentration of the nickel coloration reaction provided by the present invention.
Fig. 11 is a scatter diagram showing a gray value versus a concentration of a chromium color reaction according to the present invention.
FIG. 12 is a scattergram of a gray value versus a concentration of a copper color reaction according to the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings. It is noted that this summary includes, but is not limited to, the following detailed description, and similar techniques and methods should be considered within the scope of the present invention.
Example 1
Step one, 0.015g of hydrophobic silica particles modified by polydimethylsiloxane and 0.02g of 1H,1H,2H, 2H-perfluorooctyltriethoxysilane are sequentially added into 0.98g of absolute ethanol solution. And magnetically stirring or vortex vibrating at room temperature for 30min, and performing ultrasonic treatment for 30min to obtain the super-hydrophobic silica suspension.
And step two, shearing a small piece of double-sided adhesive tape, sucking the suspension liquid to drop on one surface of the adhesive tape release paper in a proper amount, and uniformly coating the adhesive tape release paper by using a wire bar coater with the model of 100 microns. Standing at room temperature for 5min until the ethanol is completely volatilized, and generating a layer of super-hydrophobic coating on the surface of the adhesive tape. And (3) taking a photomask plate, clamping the photomask plate on a double-sided adhesive tape coated with a super-hydrophobic silicon dioxide coating by using a long tail clamp, and etching for 8min in a plasma cleaning machine. Forming super-hydrophilic micropores in the area of the holes on the light transmitting mask plate, wherein the contact angle of water drops is 0 degree; the other areas are still super-hydrophobic areas, the contact angle of a water drop is 152.5 +/-1.9 degrees, and a super-wetting chip is formed.
And step three, attaching the super-infiltrated microchip prepared in the step two to cleaned tweezers, glass rods or gloves.
Analysis of the performance of the super-wetted microchips and their droplet capture:
(1) taking a proper amount of aqueous solution dyed by dye respectively in a disposable dropper, a beaker and a plastic cover. The dropper is squeezed to make the aqueous solution drop on the tweezers with the super-wet micro-core, and the glass rod and the gloves with the super-wet micro-core are used for pulling the beaker to dip the aqueous solution on the plastic cover. The results all observed a certain amount of dye solution on the superhydrophilic microwells, indicating that the superwetted microchip was able to capture droplets from liquids of different morphologies.
(2) By controlling the hole diameter of the photomask plate, the super-hydrophilic hole diameters of the microchips are respectively 0.5-2.5mm, the microchips are dipped in the dye solution and then are dried by absorbent paper, and the volume of the captured liquid drops is calculated by weighing the mass difference between the absorbent paper before and after water absorption. The results show that the larger the pore size of the superhydrophilic micropores, the larger the corresponding volume of the captured droplets.
Example 2
Heavy metals nickel, chromium and copper were detected using commercially available kits. Adding 4 mu L of nickel detection reagent 1 (main component ammonia water-ammonium chloride buffer solution) into a clean test tube, adding 2 mu L of nickel detection reagent 2 (main component dimethylglyoxime), and shaking up to obtain nickel detection solution. Measuring 2 mu L of detection solution, dripping the detection solution on the super-hydrophilic micropores of the microchip, naturally drying at room temperature, and enriching the detection substances in the detection solution on the micropores. The microchip-attached glove was dipped in 70mg/L of a nickel ion standard solution. The super-hydrophilic assay site on the microchip (see FIG. 9a), the drop after dip capture (see FIG. 9b) gradually developed a stable wine red color, demonstrating the feasibility of the present invention.
Based on the concept of verification, 5 μ L of nickel standard solution with the concentration of 5,10,20,30,40,60 and 70mg/L is respectively dripped into the micropore array enriched with the nickel detection reagent, and the liquid drops in each micropore show different colors. After the camera takes a picture, the grey value of each liquid drop is read by ImageJ software to obtain a curve graph of the grey value and the concentration of the nickel.
In a clean test tube, 4. mu.L of chromium detection reagent 1 (main component phosphate buffer), 0.002g of colorimetric agent powder (main component diphenylcarbodihydrazide), was added and shaken well to dissolve. 2. mu.L of the above mixture was measured and dropped on the super-hydrophilic micropores of the microchip, and after air-drying, 5. mu.L of standard potassium chromate solutions having concentrations of 0,0.5,1.0,2.0,4.0,6.0, and 9.0mg/L were respectively dropped on the micropores. In another clean test tube, 4. mu.L of copper detection solution 1 (sodium tetraborate buffer solution as main component) and 2. mu.L of detection solution 2 (bicyclohexanoneoxalyl dihydrazone as main component) were added successively and shaken up to obtain detection solution. Measuring 1.5 mul of the mixed detection solution, adding the mixed detection solution to the super-hydrophilic micropores of the microchip, air-drying, and respectively dropwise adding 6 mul of copper standard solutions with the concentrations of 0,1,2,3,6,8 and 12 mg/L. Finally, a similar image processing method was used to obtain a plot of the gray scale value versus the concentration of chromium and copper.
Claims (4)
1. The utility model provides a method for short-term test heavy metal in quality of water based on super infiltration microchip, its characterized in that, the constitution from bottom to top of super infiltration microchip includes: the device comprises a substrate device, a double-sided adhesive tape and a super-hydrophobic nano silicon dioxide coating; the substrate equipment is one or more of metal, rubber, glass and ceramic; one side of the double-sided tape is release paper, and the other side of the double-sided tape is adhesive; the super-hydrophobic nano-silica coating coats the super-hydrophobic nano-silica suspension on one surface of the release paper of the double-sided adhesive tape by a linear coating method, and super-hydrophilic micropores are formed in the coating and are used for concentrating and enriching chromogenic substances;
dropping a heavy metal detection reagent on the super-hydrophilic micropores of the super-wetted microchip, naturally drying at room temperature, and depositing and enriching active ingredients in the detection reagent on the super-hydrophilic micropores along with volatilization of a solvent;
the substrate equipment adhered with the super-wetting microchip is directly dipped with the heavy metal solution, droplets of the heavy metal solution are captured and fixed through the super-hydrophilicity of micropores and the super-hydrophobicity of non-micropore areas, the droplets are enriched in the super-hydrophilicity micropore areas, the effective components in the detection reagent and heavy metal ions in the solution generate colorimetric reaction to generate color signals, and the aim of on-site rapid detection is fulfilled;
and (3) detecting heavy metal ions in the water by a colorimetric method, wherein the heavy metal ions comprise divalent nickel, hexavalent chromium and divalent copper ions.
2. The method for rapidly detecting heavy metals in water quality based on the super-infiltration microchip as claimed in claim 1, wherein the preparation method of the super-infiltration microchip is as follows:
step one, preparing a super-hydrophobic nano silicon dioxide suspension: sequentially adding hydrophobic nano-silica particles and low-surface-energy substances into an absolute ethyl alcohol solution, magnetically stirring at room temperature for 20-30min, and then performing ultrasonic treatment for 20-30min to obtain a super-hydrophobic nano-silica suspension;
step two, preparation of the super-infiltration microchip: coating the super-hydrophobic nano-silica suspension liquid obtained in the step one on one side of release paper of a double-sided adhesive tape by using a wire bar coater, and air-drying at room temperature to volatilize a solvent to obtain a super-hydrophobic nano-silica coating; performing plasma etching on a photomask plate for 5-8min, forming super-hydrophilic micropores through the area of the holes on the photomask plate, and forming super-wetting chips by using other areas which are still super-hydrophobic areas;
and step three, attaching the super-wetting microchip obtained in the step two to a substrate device.
3. The method for rapidly detecting heavy metals in water quality based on the super-infiltration microchip as claimed in claim 2, wherein in the first step, the surface of the hydrophobic nano-silica is modified by polydimethylsiloxane, and the low surface energy substance is 1H,1H,2H, 2H-perfluorooctyltriethoxysilane.
4. The method for rapidly detecting the heavy metals in the water quality based on the super-infiltration microchip as claimed in claim 2, wherein in the second step, the coating device can control the thickness of the coating layer to be 100-200 μm; the photomask plate is clamped and fixed on the super-hydrophobic silicon dioxide coating through the long tail clamp.
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| CN108982488A (en) * | 2018-06-11 | 2018-12-11 | 北京科技大学 | The super infiltration perspiration sensor of one kind |
| CN109520977B (en) * | 2018-10-12 | 2021-03-30 | 北京科技大学 | Super-infiltrated nano dendritic gold/graphene microchip for multi-system detection |
| CN109765224A (en) * | 2019-01-02 | 2019-05-17 | 北京科技大学 | A kind of urine sensor of adhesive tape base |
| CN110412008A (en) * | 2019-07-23 | 2019-11-05 | 北京科技大学 | A kind of adhesive tape base portable SERS sensor and its preparation method and application |
| CN112894641B (en) * | 2021-01-14 | 2022-10-14 | 浙江工业大学 | Liquid drop tweezers with super oleophobic oleophylic patterned surface |
| CN113984753B (en) * | 2021-11-04 | 2022-12-02 | 长春美泰仪器有限公司 | Formaldehyde detection test paper, preparation method thereof and formaldehyde detection system |
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