CN112295622A - Integrated chip for total phosphorus digestion and real-time online detection based on optical flow control technology - Google Patents
Integrated chip for total phosphorus digestion and real-time online detection based on optical flow control technology Download PDFInfo
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- CN112295622A CN112295622A CN202011157269.2A CN202011157269A CN112295622A CN 112295622 A CN112295622 A CN 112295622A CN 202011157269 A CN202011157269 A CN 202011157269A CN 112295622 A CN112295622 A CN 112295622A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- 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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- 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
- G01N21/03—Cuvette constructions
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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
- G01N21/03—Cuvette constructions
- G01N21/05—Flow-through cuvettes
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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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
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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
- 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
- G01N21/03—Cuvette constructions
- G01N2021/0325—Cells for testing reactions, e.g. containing reagents
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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
- G01N2021/752—Devices comprising reaction zones
Abstract
The invention discloses an integrated chip for total phosphorus digestion and real-time online detection based on an optical flow control technology, which comprises: the device comprises a microfluid chip, a rapid digestion channel, a color development mixing channel and a Z-shaped optical fiber flow cell, wherein the rapid digestion channel, the color development mixing channel and the Z-shaped optical fiber flow cell are arranged on the microfluid chip; the rapid digestion channel is formed by coiling a hollow-core photonic crystal fiber; a heater is arranged below the rapid digestion channel; the fast digestion channel is connected with the color development mixing channel, and the color development mixing channel is connected with the optical fiber flow cell. The integrated chip for rapid total phosphorus pretreatment and real-time detection based on the optofluidic technology has the outstanding advantages of high efficiency, easiness in preparation, rapid online monitoring and the like.
Description
Technical Field
The invention relates to an optical flow control chip technology, in particular to an integrated chip for total phosphorus digestion and real-time online detection based on the optical flow control 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. Among them, its application in water quality monitoring and detection has attracted wide attention, including detection of heavy metal ions, microorganisms, inorganic salts, and the like. In recent years, online detection of phosphorus has attracted attention and researchers have attempted to make breakthroughs using optofluidic technology.
A photocatalytic microreactor for phosphorus digestion was devised in 2015 in Jianghua (Tong, J.; Dong, T.; Bian, C.; Wang, M.; Wang, F.; Bai, Y.; Xia, S.an integrated photocatalytic microfluidic platform for inhibition of total phosphorus microorganisms J.micromech.Microeng.2015,25,025006). Adding TiO into the mixture2The film was fixed in a microreactor irradiated with ultraviolet rays to photocatalytically digest a phosphorus sample. However, in the case of a non-flow system, it is necessary to extract a digested phosphorus sample from a chip and then measure it using an ultraviolet-visible spectrometer, wherein the phosphorus sample is susceptible to the environment and complicated operations, and thus there are many measurement errors. Moreover, the digestion efficiency of the photocatalytic microreactor is low. Thereafter, Zhu dream (Zhu, J.M.; Shi, Y.; Zhu, X.Q.; Yang, Y.; Jiang, F.H.; Sun, C.J.; ZHao, W.H.; Han, X.T. Optofludic marine phosphor detection with enhanced absorption using a Fabry-Perot resonator. Lab Chip 2017,17, 4025-. It can rapidly carry out orthophosphoric reactionThe acid salt reacts in a color development way, the detection time is reduced to be within 10 seconds, and the detection accuracy can be improved by the micro-cavity design. However, most of the phosphorus in nature cannot undergo a direct color reaction except orthophosphate, and usually requires a pretreatment. Based on the above recognition, it is currently of interest to researchers to design optofluidic systems that integrate integrated phosphor pretreatment and monitoring.
Disclosure of Invention
The invention aims to solve the technical problem of providing an integrated chip for total phosphorus digestion and real-time online detection based on an optical flow control technology aiming at the defects in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: an integrated chip for total phosphorus digestion and real-time online detection based on an optical flow control technology comprises: the device comprises a microfluid chip, a rapid digestion channel, a color development mixing channel and a Z-shaped optical fiber flow cell, wherein the rapid digestion channel, the color development mixing channel and the Z-shaped optical fiber flow cell are arranged on the microfluid chip;
the rapid digestion channel is formed by coiling a hollow-core photonic crystal fiber; a heater is arranged below the rapid digestion channel;
the fast digestion channel is connected with the color development mixing channel, and the color development mixing channel is connected with the optical fiber flow cell.
According to the scheme, the color development mixing channel is a zigzag design channel, and the color development channel consists of four groups of micro mixer channel units.
According to the scheme, the main body of the microfluidic chip is bonded by PDMS and a glass substrate.
According to the scheme, the height of the channel in the color developing mixing channel is 150 mu m.
According to the scheme, the Z-shaped optical fiber flow cell comprises a PDMS micro-cavity and multimode optical fibers which are connected with two ends of the micro-cavity and provided with optical fiber collimators at the ports.
According to the scheme, inlets are formed in the left side and the right side of the front end of the rapid digestion channel and the color development mixing channel, and a waste water outlet is formed in the rear end of the optical fiber flow pool.
A total phosphorus digestion and real-time online detection method using the integrated chip comprises the following steps:
1) injecting the initial sample and the digestion solution from two inlets of the rapid digestion channel respectively, mixing, entering the rapid digestion channel, heating to 90 ℃ by a micro heater, generating a high-temperature high-pressure environment in the digestion channel, and oxidizing the initial sample by the digestion solution;
2) continuously flowing the digested liquid to be detected into the color development channel, introducing color developers A and B from two inlets of the color development mixing channel, and fully mixing in the color development channel to generate color development reaction;
3) and (3) the liquid to be detected after the color development is finished flows into an optical flow cell, the light intensity of the liquid to be detected is measured by using a light source with the wavelength of 880nm, and the concentration of the liquid to be detected is obtained through conversion of a standard curve.
The invention has the following beneficial effects:
the integrated chip for rapid total phosphorus pretreatment and real-time detection based on the optofluidic technology has the outstanding advantages of high efficiency, easiness in preparation, capability of realizing online rapid monitoring and the like.
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 an embodiment of the present invention;
FIG. 2 is a schematic plan view of a microfluidic color channel according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of an optical flow cell configuration according to an embodiment of the present invention;
in the figure, 1 — initial sample inlet; 2-digestion liquid inlet; 3, the color developing agent A enters the inlet; 4-inlet of color-developing agent B; 5-clearing up the channel; 6-a color channel; 7-an optical flow cell; 8-a liquid outlet; 31-a fiber collimator; 32-a multimode optical fiber; 33-quartz plate; 34-lens.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following 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.
As shown in fig. 1 and fig. 2, an integrated chip for total phosphorus digestion and real-time online detection based on optofluidic technology includes: the device comprises a microfluid chip, a rapid digestion channel, a color development mixing channel and a Z-shaped optical fiber flow cell, wherein the rapid digestion channel, the color development mixing channel and the Z-shaped optical fiber flow cell are arranged on the microfluid chip;
the rapid digestion channel is formed by coiling a hollow-core photonic crystal fiber; a heater is arranged below the rapid digestion channel;
the fast digestion channel is connected with the color development mixing channel, and the color development mixing channel is connected with the optical fiber flow cell.
The color-rendering mixing channel is a zigzag design channel, and the color-rendering channel consists of four groups of micro mixer channel units.
The main body of the microfluidic chip is bonded by PDMS and a glass substrate, and the height of the channel in the chromogenic mixing channel is 150 μm.
Referring to fig. 3, the Z-type optical fiber flow cell includes a PDMS micro-cavity and a multimode optical fiber connected to two ends of the micro-cavity and having two ports with optical fiber collimators. The length, width and height of the PDMS micro-cavity size of the middle part are respectively 10mm, 1.5cm and 1.5 cm; two ends of the micro-cavity are connected with two multimode fibers with ports provided with fiber collimators, and a transparent quartz plate (5mm multiplied by 100 mu m) is arranged between the two multimode fibers; the multimode optical fiber is a chromium-plated optical fiber with the core diameter of 200 mu m, and the Numerical Aperture (NA) is 0.22.
The left side and the right side of the front end of the rapid digestion channel and the color development mixing channel are both provided with inlets, and the rear end of the optical fiber flow pool is provided with a wastewater outlet.
A total phosphorus digestion and real-time online detection method using the integrated chip comprises the following steps:
1) injecting the initial sample and the digestion solution from two inlets of the rapid digestion channel respectively, mixing, entering the rapid digestion channel, heating to 90 ℃ by a micro heater, generating a high-temperature high-pressure environment in the digestion channel, and oxidizing the initial sample by the digestion solution;
2) continuously flowing the digested liquid to be detected into the color development channel, introducing color developers A and B from two inlets of the color development mixing channel, and fully mixing in the color development channel to generate color development reaction;
3) and (3) the liquid to be detected after the color development is finished flows into an optical flow cell, the light intensity of the liquid to be detected is measured by using a light source with the wavelength of 880nm, and the concentration of the liquid to be detected is obtained through conversion of a standard curve.
In the following examples, all the reagents are commercially available chemical reagents unless otherwise specified.
An integrated chip for rapid total phosphorus pretreatment and real-time detection based on an optical flow control technology is prepared by the following steps:
1. a microfluid color development channel of a chip is designed through Auto CAD, and by combining the drawings of figure 1 and figure 2, the designed color development channel consists of four groups of micro mixer channel units, the size of the channel unit is 50 mu m multiplied by 1mm, a flow cell cavity with the size of 1cm multiplied by 5mm is designed at the rear, and connectors are reserved at two ends so as to integrate the three parts into an integrated chip. Developer a and developer B will enter from inlets 3 and 4. The solution after color development is completed flows into the optical flow cell.
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) 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 the mixture contains uniform small bubbles, pouring a certain amount of uniformly mixed PDMS on the silicon chip template manufactured in the step 3), and placing the flow cell mold on a corresponding position of the silicon chip before pouring. Placing in an oven, heating to 90 deg.C, and vacuumizing.
4. Taking down the solidified PDMS with microstructure, and punching holes at the inlet 3 of the color-developing agent A of the microchannel, the inlet 4 of the color-developing agent B and the outlet 8 of the detected wastewater.
5. And (3) putting the PDMS with the microstructure and the punched holes obtained in the steps (1) to (4) 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, two pieces of quartz glass are placed on the inner wall of the flow cell cavity, and then the PDMS structure is bonded with the glass substrate.
6. A fiber collimator 31 is connected to the multimode fiber port 32 while processing the multimode fiber on the other side. Two corresponding small holes are drilled on both sides of the flow cell cavity of the bonded chip in step 5, and two optical fibers are inserted therein. An optical power meter is used to connect the two multimode fibers and a 5D alignment jig is used to perform the alignment operation at the periphery until the optical power meter reading is maximized.
7. A hollow-core photonic crystal fiber is coiled into a 2.5cm spiral shape, and a plastic tee joint is connected to the front end of the hollow-core photonic crystal fiber by ultraviolet curing adhesive to serve as inlets 1 and 2. The optical fiber was then placed on the front half of the glass substrate and capillary-bonded in front of the chip prepared in step 6. A micro heater with a diameter of 3cm is arranged below the heater. And finishing the manufacturing of the integrated chip.
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. The utility model provides an integrated chip that total phosphorus was cleared up and real-time on-line measuring based on light stream accuse technique which characterized in that includes: the device comprises a microfluid chip, a rapid digestion channel, a color development mixing channel and a Z-shaped optical fiber flow cell, wherein the rapid digestion channel, the color development mixing channel and the Z-shaped optical fiber flow cell are arranged on the microfluid chip;
the rapid digestion channel is formed by coiling a hollow-core photonic crystal fiber; a heater is arranged below the rapid digestion channel;
the fast digestion channel is connected with the color development mixing channel, and the color development mixing channel is connected with the optical fiber flow cell.
2. The integrated chip for total phosphorus digestion and real-time online detection based on the optical flow control technology as claimed in claim 1, wherein the chromogenic mixing channel is a zigzag design channel, and the chromogenic mixing channel is composed of four sets of micro mixer channel units.
3. The integrated chip for total phosphorus digestion and real-time online detection based on the optofluidic technology as claimed in claim 1, wherein the body of the microfluidic chip is bonded by PDMS and a glass substrate.
4. The integrated chip for total phosphorus digestion and real-time on-line detection based on optical flow control technology as claimed in claim 1, wherein the height of the channel in the chromogenic mixing channel is 150 μm.
5. The integrated chip for total phosphorus digestion and real-time online detection based on the optofluidic technology as recited in claim 1, wherein the Z-shaped optical fiber flow cell comprises a PDMS micro-cavity and a multimode optical fiber connected to both ends of the micro-cavity and having two ports with optical fiber collimators.
6. The integrated chip for total phosphorus digestion and real-time online detection based on the optical flow control technology as claimed in claim 1, wherein inlets are arranged on the left and right sides of the front ends of the rapid digestion channel and the color development mixing channel, and a wastewater outlet is arranged on the rear end of the fiber flow cell.
7. A total phosphorus digestion and real-time on-line detection method using the integrated chip of claim 1, comprising the steps of:
1) injecting the initial sample and the digestion solution from two inlets of the rapid digestion channel respectively, mixing, entering the rapid digestion channel, heating to 90 ℃ by a micro heater, generating a high-temperature high-pressure environment in the digestion channel, and oxidizing the initial sample by the digestion solution;
2) continuously flowing the digested liquid to be detected into the color development channel, introducing color developers A and B from two inlets of the color development mixing channel, and fully mixing in the color development channel to generate color development reaction;
3) and (3) the liquid to be detected after the color development is finished flows into an optical flow cell, the light intensity of the liquid to be detected is measured by using a light source with the wavelength of 880nm, and the concentration of the liquid to be detected is obtained through conversion of a standard curve.
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| CN113155821A (en) * | 2021-04-07 | 2021-07-23 | 武汉理工大学 | Total phosphorus real-time online detection chip and method based on photo-thermal material |
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