CN112858177A - Heavy metal ion on-line measuring chip based on micro-fluidic extraction technique - Google Patents
Heavy metal ion on-line measuring chip based on micro-fluidic extraction technique Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/26—Treatment of water, waste water, or sewage by extraction
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Abstract
The invention discloses a heavy metal ion online detection chip based on a microfluidic extraction technology, which comprises six groups of composite micro-droplet generation and extraction channels which are symmetrically arranged in parallel, a composite micro-droplet collection main channel at the middle position and an optical fiber sensor buried at the left end, wherein the main body of the chip is bonded with a glass substrate by polydimethylsiloxane; the composite micro-droplet and extraction channel which are symmetrically arranged in parallel are divided into two parts, namely a cross-shaped channel which is positioned at the upper end and can generate the composite micro-droplet, a snake-shaped channel which is positioned at the lower end and is used for extracting heavy metal ions by the composite micro-droplet, and the main channel at the middle position comprises a channel for collecting the composite micro-droplet and a channel of an optical fiber sensor integrated at the left end; fiber sensing uses two common single mode fibers aligned in a microfluidic channel. The heavy metal ion online detection chip based on the microfluidic extraction technology has the outstanding advantages of high efficiency, easiness in control, online rapid monitoring and the like.
Description
Technical Field
The invention belongs to the technical field of microfluidic chips, and particularly relates to a heavy metal ion online detection chip based on a microfluidic extraction technology.
Background
Microfluidic chips are an emerging research technology for operating liquids on the micrometer, even nanometer scale. Generally, microfluidic chips are integrated with microchannels having various functions, and the microchannels respectively form different functional unit areas to form a small laboratory with a definite division of labor. The optical fiber sensor has the outstanding advantages of corrosion resistance, electromagnetic interference resistance, high precision, compact structure and the like, and has been greatly researched in the aspects of biomedical measurement and environmental protection. The optical fiber absorbance detection based on the Belronbo law is combined with a micro-scale channel, can realize detection, and has high precision and sensitivity. The increase of industrial activities discharges sewage containing pollutants such as heavy metal ions, organic dyes, and medicines into aquatic environments, causing serious environmental deterioration. Currently, there are many methods of purifying water, such as chemical coagulation, photodegradation, precipitation, flocculation, membrane separation, ion exchange, etc., but most organic molecules and heavy metal contaminants are stable, small in size and non-biodegradable, and thus difficult to eliminate from wastewater.
Preschool et al (CN 106582599A) prepared graphene oxide from graphite powder by Hummers' method, prepared into solution, adjusted pH, heated, and frozen to obtain bulk photocatalytic carbon aerogel material, which can reduce chromium ions in wastewater under irradiation of sunflower. However, the photocatalytic material has low sewage treatment efficiency and can reduce chromium ions in the wastewater singly; congeevaram S (Congeevaram S, Dhanarani S, Park J, et al. Bioperspective of chromium and nickel by means of metallic resistance and bacterial isolates [ J ]. Journal of halogenated materials 2007,146(1-2):270-277) et al use fungi and bacteria to remove chromium and nickel ions from industrial wastewater, but microbial treatment of industrial wastewater is severely affected by temperature, pH, and heavy metal ion concentration, and thus it is of current interest to researchers to develop a rapid, efficient, and convenient method for treating wastewater.
Disclosure of Invention
The invention aims to solve the technical problem of providing a heavy metal ion online detection chip based on a microfluidic extraction technology, and compared with the existing water purification method, the heavy metal ion online detection chip achieves high-efficiency mass transfer rate by utilizing a large amount of composite bubbles generated by a microfluidic chip and is used for treating sewage. Two single-mode fibers are butted, light penetrates through a tested sample, and partial light is absorbed to obtain the absorbance of the extracted wastewater, so that the aim of monitoring the concentration of heavy metal ions is fulfilled.
The technical scheme adopted by the invention for solving the technical problems is as follows: the chip comprises a composite micro-droplet generation and extraction channel, a composite micro-droplet collection main channel and an optical fiber sensor, wherein the composite micro-droplet generation and extraction channel is arranged in parallel and symmetrically, the composite micro-droplet collection main channel is arranged in the middle of the composite micro-droplet collection main channel, and the optical fiber sensor is embedded at one end of the composite micro-droplet collection main channel; the composite micro-droplet and extraction channel which are symmetrically arranged in parallel are divided into two parts, namely a cross-shaped channel which is positioned at the upper end and can generate the composite micro-droplet, a snake-shaped channel which is positioned at the lower end and is used for extracting heavy metal ions by the composite micro-droplet, and the main channel at the middle position comprises a channel for collecting the composite micro-droplet and a channel of an optical fiber sensor integrated at one end; fiber sensing uses two common single mode fibers aligned in a microfluidic channel.
According to the technical scheme, photoetching is adopted for manufacturing the channel mask, the substrate is a silicon wafer, the used photoresist is SU-8 photoresist, the channels are subjected to secondary photoetching, and the depths of the primary photoetching and the secondary photoetching are 125-300 mu m.
According to the technical scheme, the PDMS is poured into a mask plate to be heated and cured, oxygen is used as plasma cleaning gas in bonding with a glass substrate after being taken out, the vacuum degree is maintained at 26-29Pa, the radio frequency power is 50-60W, and the glow discharge cleaning time is 60-120 s.
According to the technical scheme, two cross-shaped channels are arranged in each group of micro-fluid channels, the first type is used for generating bubbles of nitrogen-in-oil, and the sizes of oil, nitrogen inlet and outlet channels are respectively 300-; the other is used for further wrapping the air bubbles in the water on the basis of the first type to form water-oil-nitrogen composite micro-droplets, and the sizes of the oil and air bubbles, the inlet and outlet channels of the waste water are respectively 300-500 mu m, 200-400 mu m and 50-100 mu m.
According to the technical scheme, a semicircular connection design is adopted in a snake-shaped channel for extracting heavy metal ions, and the length, width and semicircular diameter of the channel are respectively 10-18mm, 300-.
According to the technical scheme, in the channel of the integrated optical fiber sensor, the length and the width of the channel are respectively 4mm-10mm and 200-; the length and width of the main channel after the composite micro-droplets are collected and the wastewater is treated are 60-100mm and 1-5mm respectively.
According to the technical scheme, the concentration of heavy metal ions in the extracted wastewater is tested through absorbance by optical fiber sensing, a mode of butting two common single-mode optical fibers is adopted, and two end faces are cut into smooth planes by an optical fiber cutter.
Firstly, a high-precision mask is manufactured, then a substrate is manufactured on a silicon wafer by using a photoetching technology, and a chip is manufactured on the silicon wafer substrate by using Polydimethylsiloxane (PDMS). The cross-shaped channel is adopted to generate composite bubbles to extract heavy metal ions in the wastewater in the snake-shaped channel, and meanwhile, the integrated optical fiber is used for carrying out on-line monitoring on the treated wastewater.
The invention utilizes the difference of solubility or distribution coefficient of metal ions in water and the high-hydrophobicity extractant to transfer the metal ions from the wastewater into the high-hydrophobicity extractant. Solvent extraction usually requires a multistage process to achieve the extraction effect due to high mass transfer resistance during extraction and low specific surface area between liquid phases. The composite bubbles generated in the microfluidic chip are utilized to increase the contact surface area of the water-high hydrophobic extractant, and the stirring effect is achieved in the flowing process, so that the high-speed mass transfer rate is achieved in the microfluidic chip, and the effect of rapid extraction is achieved; the method is characterized in that two single-mode fibers are butted, light penetrates through a tested sample, and partial light is absorbed to obtain the absorbance of the extracted wastewater, so that the absorbance is converted into the concentration of the extracted heavy metal ions.
The invention has the following beneficial effects: 1) the invention uses a large amount of composite bubbles generated by the micro-fluidic chip to increase the specific surface area between liquid phases, and uses the stirring effect in the flow to achieve high-speed mass transfer efficiency and realize rapid extraction.
2) The invention realizes on-line detection by butting the common single-mode optical fiber in the microfluidic channel and well combining the common single-mode optical fiber with the microfluidic chip.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
fig. 1 is a schematic structural diagram of a microfluidic chip in an embodiment of the present invention.
FIG. 2 is a schematic structural diagram of a nitrogen-in-oil bubble micro-flow channel and a water-oil-nitrogen composite bubble micro-flow channel generated in the embodiment of the invention.
FIG. 3 is a schematic diagram of a "snake" channel structure for rapidly extracting heavy metal ions in an embodiment of the present invention
Fig. 4 is a schematic diagram of a channel of two single-mode optical fibers in butt joint and an integrated optical fiber sensor according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the embodiment of the invention, as shown in fig. 1-4, the heavy metal ion online detection chip based on the microfluidic extraction technology comprises a composite micro-droplet generation and extraction channel, a composite micro-droplet collection main channel and an optical fiber sensor, wherein the composite micro-droplet generation and extraction channel is arranged in parallel and symmetrically, the composite micro-droplet collection main channel is arranged in the middle of the composite micro-droplet generation and extraction channel, and the optical fiber sensor is embedded at one end of the composite micro-droplet collection main; the composite micro-droplet and extraction channel which are symmetrically arranged in parallel are divided into two parts, namely a cross-shaped channel which is positioned at the upper end and can generate the composite micro-droplet, a snake-shaped channel which is positioned at the lower end and is used for extracting heavy metal ions by the composite micro-droplet, and the main channel at the middle position comprises a channel for collecting the composite micro-droplet and a channel of an optical fiber sensor integrated at one end; fiber sensing uses two common single mode fibers aligned in a microfluidic channel. The manufacturing of the channel mask adopts photoetching, the substrate adopts a silicon wafer, the used photoresist is SU-8 photoresist, the channels are subjected to secondary photoetching, and the depths of the primary photoetching and the secondary photoetching are 125-300 mu m. Pouring PDMS into a mask plate for heating and curing, taking out and using oxygen as plasma cleaning gas in bonding with the glass substrate, maintaining the vacuum degree at about 26-29Pa, the radio frequency power at 50-60W, and the glow discharge cleaning time at 60-120 s. Two cross-shaped channels are arranged in each group of micro-fluid channels, the first type is used for generating bubbles of nitrogen-in-oil, and the sizes of oil and nitrogen inlet and outlet channels are respectively 300-; the other is used for further wrapping the air bubbles in the water on the basis of the first type to form water-oil-nitrogen composite micro-droplets, and the sizes of the oil and air bubbles, the waste water inlet and outlet channels are respectively 300-500 mu m, 200-400 mu m and 50-100 mu m. In the 'snake-shaped' channel for extracting heavy metal ions, a semicircular connection design is adopted, and the length, width and semicircular diameter of the channel are respectively 10-18mm, 300-. In the channel of the integrated optical fiber sensor, the length and the width of the channel are respectively 4mm-10mm and 200-; the length and width of the main channel after the composite micro-droplets are collected and the wastewater is treated are 60-100mm and 1-5mm respectively.
The preparation method of the chip for the online detection of the heavy metal ions in the embodiment comprises the following steps:
1) designing a microfluidic chip through Auto CAD, wherein a designed microstructure channel 1 consists of six groups of composite micro-droplet generation and extraction channels which are symmetrically arranged in parallel, a composite micro-droplet collection main channel at the middle position and an upper-lower symmetrical channel integrating optical fiber sensing, the six groups of composite micro-droplet generation and extraction channels which are symmetrically arranged in parallel are divided into two parts, one is a cross-shaped channel which is positioned at the upper end and can generate composite micro-droplets, the cross-shaped structure in the microfluidic channel is two, the other is a channel 2 for generating bubbles of nitrogen-in-oil, and the sizes of oil, nitrogen inlet and outlet channels are respectively 300 mu m, 200 mu m and 20 mu m; a 'snake-shaped' channel at the lower end of which a composite liquid drop extracts heavy metal ions can generate a 'cross-shaped structure' channel of composite bubbles is a channel 3 which further wraps the bubbles in water on the basis of the first channel to form composite micro-drops of water, oil and nitrogen, wherein the sizes of an oil inlet channel, an oil bubble channel, a waste water inlet channel and a waste water outlet channel are 257 microns, 200 microns and 100 microns respectively. The other is a 'snake-shaped' channel 4 which is arranged at the lower end and used for extracting heavy metal ions, wherein the extraction speed can be accelerated by adopting a semicircular design, and the length, the width and the semicircular diameter of the channel are respectively 18mm, 500 mu m and 350 mu m. The length and the width of a channel 5 of the integrated optical fiber sensor are respectively 4mm and 200 mu m; the length and width of the main channel 6 after the composite bubbles are collected and the wastewater is treated are 83mm and 1mm respectively.
2) And (2) spin-coating SU8-50 negative photoresist on the silicon wafer to obtain the mask, wherein the front rotating speed is 500r/s and the time is 18s when the photoresist is homogenized, and the back rotating speed is 2800r/s and the time is 30 s. And in the pre-baking stage, after the glue homogenizing is finished, baking at 65 ℃ for 5min, and then baking at 95 ℃ for 12 min. Aligning the prepared mask plate under an ultraviolet lithography machine, exposing the silicon wafer coated with the photoresist, performing post-baking treatment after exposure, baking for 90s at 65 ℃, and baking for 6min at 95 ℃. After the completion, the photoresist outside the microstructure is removed by using an ultraviolet photoetching developing solution, and finally, the film is hardened for 3min at 150 ℃, so that the structure is firmer.
3) And (3) carrying out secondary photoetching on the template prepared on the silicon wafer in the step 2) by the same step.
4) And (3) manufacturing the PDMS flat chip, namely mixing PDMS and a curing agent according to the mass ratio of 10:1, fully stirring the mixture until uniform small bubbles exist in the mixture, and pouring a certain amount of uniformly mixed PDMS on the silicon wafer template manufactured in the step (3). Placing in an oven, heating to 90 deg.C, and vacuumizing.
5) Taking down the PDMS with the microstructure after the curing in the step 4), and punching holes at a nitrogen inlet 7 of the micro-channel, a nickel ion-containing wastewater inlet 8, an extracting agent 2-ethylhexyl phosphate mono-2-ethylhexyl phosphate inlet 9 and a wastewater outlet 10 which is compounded with micro-droplets and treated.
6) And removing the coating layer of the optical fiber by using an optical fiber wire stripper, obtaining a smooth end face by using an optical fiber cutter, and simultaneously processing two single-mode optical fibers.
7) And (3) putting the PDMS with the microstructure and the punched holes obtained in the steps (1) to (6) and the glass substrate into a plasma cleaning machine, wherein oxygen is used as plasma cleaning gas in the cleaning process, the vacuum degree is maintained to be about 27Pa, the radio frequency power is 50W, and the glow discharge cleaning time is 60 s. After cleaning, the manufactured optical fiber is placed at the position of the channel 5 in the PDMS, and is bonded with the glass substrate, whether the two optical fibers 11 are aligned in the channel 5 or not is ensured by observing in a microscope and using an aligner, and after bonding, the bonding part of the optical fiber sensing probe and the channel is sealed by using curing glue. Finally, the optical fibers are proved to be strictly aligned by detecting the signals of the feedback spectrum.
Wherein the reagents without specific description are all commercial chemical reagents.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (7)
1. A heavy metal ion on-line detection chip based on a microfluidic extraction technology is characterized by comprising a composite micro-droplet generation and extraction channel, a composite micro-droplet collection main channel and an optical fiber sensor, wherein the composite micro-droplet generation and extraction channel is arranged in parallel and symmetrically, the composite micro-droplet collection main channel is arranged in the middle of the composite micro-droplet collection main channel, and the optical fiber sensor is embedded in one end of the composite micro-droplet collection main channel; the composite micro-droplet and extraction channel which are symmetrically arranged in parallel are divided into two parts, namely a cross-shaped channel which is positioned at the upper end and can generate the composite micro-droplet, a snake-shaped channel which is positioned at the lower end and is used for extracting heavy metal ions by the composite micro-droplet, and the main channel at the middle position comprises a channel for collecting the composite micro-droplet and a channel of an optical fiber sensor integrated at one end; fiber sensing uses two common single mode fibers aligned in a microfluidic channel.
2. The chip for on-line detection of heavy metal ions based on microfluidic extraction technology as claimed in claim 1, wherein the trench mask is fabricated by photolithography, the substrate is made of silicon wafer, the photoresist used is SU-8 photoresist, the trench is subjected to secondary photolithography, and the depth of the primary and secondary photolithography is 125 μm-300 μm.
3. The heavy metal ion online detection chip based on the microfluidic extraction technology as claimed in claim 1, wherein the PDMS is poured into a mask for heating and curing, oxygen is used as plasma cleaning gas in bonding with the glass substrate after being taken out, the vacuum degree is maintained at 26-29Pa, the radio frequency power is 50-60W, and the glow discharge cleaning time is 60-120 s.
4. The on-line detection chip for heavy metal ions based on the microfluidic extraction technology as claimed in claim 1 or 2, wherein there are two "cross" channels in each set of microfluidic channels, the first is used to generate bubbles of nitrogen-in-oil, and the sizes of the channels at the oil inlet and the nitrogen outlet are respectively 300-; the other is used for further wrapping the air bubbles in the water on the basis of the first type to form water-oil-nitrogen composite micro-droplets, and the sizes of the oil and air bubbles, the inlet and outlet channels of the waste water are respectively 300-500 mu m, 200-400 mu m and 50-100 mu m.
5. The chip for the on-line detection of heavy metal ions based on the microfluidic extraction technology as claimed in claim 1 or 2, wherein the "snake-shaped" channel for heavy metal ions during extraction is configured by a semicircular connection, and the length, width and semicircular diameter of the channel are respectively 10-18mm, 300-800 μm and 200-350 μm.
6. The chip for the on-line detection of heavy metal ions based on the microfluidic extraction technology as claimed in claim 1 or 2, wherein the length and width of the channel dimension in the channel of the integrated optical fiber sensor are respectively 4mm-10mm and 200-; the length and width of the main channel after the composite micro-droplets are collected and the wastewater is treated are 60-100mm and 1-5mm respectively.
7. The heavy metal ion on-line detection chip based on the microfluidic extraction technology as claimed in claim 1 or 2, wherein the optical fiber sensing is to test the concentration of heavy metal ions in the extracted wastewater through absorbance, a mode of butt joint of two common single-mode optical fibers is adopted, and two end faces are cut into smooth planes by an optical fiber cutting knife.
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