CN112730357A - Optical sensing film for detecting two-dimensional distribution of carbon dioxide in sediment - Google Patents
Optical sensing film for detecting two-dimensional distribution of carbon dioxide in sediment Download PDFInfo
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- CN112730357A CN112730357A CN202011492211.3A CN202011492211A CN112730357A CN 112730357 A CN112730357 A CN 112730357A CN 202011492211 A CN202011492211 A CN 202011492211A CN 112730357 A CN112730357 A CN 112730357A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B17/00—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups
- B05B17/04—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods
- B05B17/06—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
- B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/52—Two layers
- B05D7/54—No clear coat specified
- B05D7/544—No clear coat specified the first layer is let to dry at least partially before applying the second layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/52—Two layers
- B05D7/54—No clear coat specified
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Abstract
The invention relates to an optical sensing film for detecting two-dimensional distribution of sediment carbon dioxide, which is characterized in that fluorescent dye and reference dye are uniformly mixed, the two dyes are fixed on the surface of a transparent PET (polyethylene terephthalate) base material through ultrasonic spraying, and then diluted gas permeable silicone rubber is coated on a sensing layer to serve as a protective layer; placing the prepared optical sensing film between sediment/soil and a film containing wall, obtaining an emission image of the optical sensing film through a CCD camera under the irradiation of 475nm exciting light, and obtaining two-dimensional space distribution of carbon dioxide in the sediment through a green (G) channel fluorescence ratio method and a red (R) channel fluorescence ratio method for extracting the image; by adding the reference dye, the stability of the membrane is improved without depending on a single fluorescent dye with poor light stability and water stability, and the reference effect is realized to reduce background interference, so that higher detection precision is obtained.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of detection of carbon dioxide in water body sediments, and particularly relates to a preparation method of a carbon dioxide planar optical sensing film.
[ background of the invention ]
Carbon cycle is a major focus of scientific research in recent years, and deposits are an important part of the global carbon cycle, including remineralization of organic carbon and dissolution and precipitation of calcium carbonate, which produce or consume CO2，HCO-3，CO23 and H +, so the sediment-water interface generally has a steep CO2A gradient; in addition, the life activities of the roots of aquatic plants and large benthonic animals in the sediment also cause CO in the sediment2There is a very high temporal and spatial heterogeneity of the distribution.
Based on CO in the deposit2The distribution has the characteristic of high space-time heterogeneity, and the current common test means, such as a microelectrode and an optical fiber sensor, have limitations; the microelectrode method and the optical fiber sensor have the characteristics of high resolution, high precision and in-situ measurement, and are commonly used for detecting CO in sediments2Obtaining CO from the deposit by a single point measurement2The microelectrode method and the optical fiber sensor are expensive and complicated to operate, and cannot acquire the sediment CO in real time2Two-dimensional distribution information.
Development of planar optical sensors to CO in deposits2Provides a new way to detect CO through a fluorescent sensing membrane2The concentration is converted into a measurable photochemical signal, and CO in the sediment can be converted2And performing two-dimensional visual presentation on the distribution. At present, quaternary ammonium salt/quaternary ammonium base is often used as a phase transfer agent, HPTS/TOA + PTS 4-is used as an optical indicator to prepare CO2A light pole; when CO in the air2Entering into environment medium (usually water body), forming carbonic acid and then generating deprotonation process to cause change of pH of environment medium, and calculating concentration of each ion in system and reaction equilibrium constant to obtain CO2Partial pressure of (a); however, the HPTS/TOA + PTS 4-indicator is more sensitive to light and water in the environmentLeading to the situation that the fluorescence of the finished film is easy to be continuously weakened,
therefore, it is an urgent need in the art to provide an optical sensing film that is simple and efficient and can ensure the performance of the sensor.
[ summary of the invention ]
In order to solve the problems, the invention provides a preparation method of an optical sensing film for detecting two-dimensional distribution of carbon dioxide in sediments, which comprises the following steps:
the method comprises the following steps: dissolving ethyl cellulose particles in a mixed solution of ethanol and toluene to obtain a polymer solution, and then adding a fluorescent dye, a reference dye and a phase transfer catalyst into the polymer solution to completely dissolve the polymer solution to obtain a mixed solution of the optical sensing membrane;
step two: spraying the mixed solution of the optical sensing film obtained in the step one on a PET (polyethylene terephthalate) base material by using an ultrasonic spraying device, and forming a sensing layer with the thickness of less than 10 microns after the solvent is evaporated;
step three: and (3) mixing the silicon rubber and the diluent to obtain a silicon rubber solution, and after the sensing layer in the second step is completely dried, coating the silicon rubber solution on the surface of the sensing layer and drying.
Further, the fluorescent dye is a TOA + PTS 4-ion pair, HPTS and TOABr are respectively dissolved in NaOH solution and dichloromethane, the mixed solution is subjected to water bath and vacuum filtration, and the obtained solid is the TOA + PTS 4-ion pair.
Further, the reference dye is solvent orange 63, and the phase transfer catalyst is a TOAOH solution.
Further, the diluent is petroleum ether and xylene in a volume ratio of 1: 1.5-3, and mixing.
Further, the concentration of the ethyl cellulose in the polymer solution in the first step is 20g/L, and the volume ratio of the ethanol to the toluene is 1: 9.
Further, the concentration of the NaOH solution is 0.4g/L, the concentration of HPTS is 0.4g/L, and the concentration of TOABr is 1.7 g/L.
A method of calibrating an optical sensing film, comprising the steps of:
S1：NaCl solution is prepared, and different CO is obtained by adjusting the addition amount of NaHCO32Partial pressure of the solution, measuring the pH and temperature of the solution, and calculating CO by formula2Partial pressure; to be treated with CO2After the partial pressure is stable, the optical sensing film is attached to the inner wall of the transparent container, the optical sensing film is irradiated by an excitation light source, and different CO is obtained by using a CCD camera2Fluorescence images at concentration;
s2 extraction of different CO2And calculating the fluorescence intensity ratio R of the two channels, wherein R is G/R, and performing curve fitting.
Furthermore, the concentration of the NaCl solution is 11.388g/L, and the excitation light source is 475 nm.
Compared with the prior art, the invention has the following beneficial effects:
the optical sensing film prepared by the invention is prepared by uniformly mixing fluorescent dye and reference dye, fixing the two dyes on the surface of a transparent PET (polyethylene terephthalate) base material through ultrasonic spraying, and then coating diluted gas permeable silicone rubber on a sensing layer to be used as a protective layer; placing the prepared optical sensing film between sediment/soil and a film containing wall, obtaining an emission image of the optical sensing film through a CCD camera under the irradiation of 475nm exciting light, and obtaining two-dimensional space distribution of carbon dioxide in the sediment through a green (G) channel fluorescence ratio method and a red (R) channel fluorescence ratio method for extracting the image; by adding the reference dye, the stability of the membrane is improved without depending on a single fluorescent dye with poor light stability and water stability, and the reference effect is realized to reduce background interference, so that higher detection precision is obtained.
[ description of the drawings ]
FIG. 1 shows the optical sensing film of the present invention in different COs2To CO at concentration2The response curve of (a);
FIG. 2 shows an embodiment of the present invention in which the optical sensing film is used in different COs2Fluorescence image extraction at concentration;
FIG. 3 shows an embodiment of the present invention in which the optical sensing film is used in different COs2Images of the change in fluorescence ratio with time at concentration;
FIG. 4 shows an embodiment of the present inventionEXAMPLES obtaining CO in pure deposits by means of optical sensing films2And (4) a two-dimensional dynamic distribution map.
FIG. 5 shows the embodiment of the present invention, in which CO in the sediment of the planted tape grass is obtained through the optical sensing film2And (4) a two-dimensional dynamic distribution map.
[ detailed description ] embodiments
The directional terms of the present invention, such as "up", "down", "front", "back", "left", "right", "inner", "outer", "side", etc., are only directions in the drawings, and are only used to explain and illustrate the present invention, but not to limit the scope of the present invention.
The present invention is further illustrated by the following figures and specific examples, which are to be understood as illustrative only and not as limiting the scope of the invention, which is to be given the full breadth of the appended claims and any and all equivalent modifications thereof which may occur to those skilled in the art upon reading the present specification and which are intended to be within the scope of the appended claims.
Example 1
The invention detects CO in sediment2The preparation method of the optical sensing film with two-dimensional distribution comprises the following steps:
the method comprises the following steps: dissolving 210mg of 8-hydroxypyrene-1, 3, 6-trisulfonic acid sodium salt (8-Hydroxy-1,3, 6-pyrenetrinic acid trisodium salt, HPTS) in 50mL of 0.4g/L NaOH solution, dissolving 219mg of tetraoctylammonium bromide (TOABr) in 50mL of dichloromethane, mixing the two solutions, oscillating, and carrying out vacuum filtration in a water bath kettle to obtain bright yellow-green oil residue, namely CO2The fluorescent dye TOA + PTS 4-ion pair;
step two: weighing 2g of ethyl cellulose particles, adding the ethyl cellulose particles into a mixed solution of 10 ml of ethanol and 90 ml of toluene, and dissolving to prepare a polymer solution; adding 5mL Tetraoctylammonium hydroxide solution (20% in methanol (T)) to the polymer solution; then adding 25mg of TOA + PTS 4-ion pair and 1mg of solvent orange 63 into the polymer solution, and carrying out ultrasonic dissolution to obtain a mixed solution of the optical sensing film;
step three: uniformly mixing the mixed solution, spraying the mixed solution on a polyethylene terephthalate (PET) substrate by using an ultrasonic spraying device, and evaporating a solvent to form a sensing layer with the thickness of less than 10 mu m;
step four: according to m (silicon rubber): v (diluent) ═ 1: 2.5 preparing a silicone rubber solution wherein the diluent is a mixture of petroleum ether and xylene in a ratio of 2: 5 in a volume ratio; after the sensing layer is completely dried, uniformly coating the silicon rubber solution on the sensing layer by using an automatic film scraping machine, and drying for 24 hours; storing in dark condition for use.
Step five: calibrating the optical sensing film:
s1, preparing 11.688g/L NaCl solution, and obtaining different CO by adjusting the dosage of NaHCO32Partial pressure of the solution, measuring the pH and temperature of the solution, and calculating to obtain CO by formula2Partial pressure; to be treated with CO2After the partial pressure is stabilized, CO is added2The sensing membrane is attached to the inner wall of the transparent container, a 475nm excitation light source is used for irradiating the sensing membrane, and a CCD camera is used for acquiring different CO2Fluorescence images at concentration;
s2 extraction of different CO2Calculating the fluorescence intensity ratio R of the red channel R and the green channel G of the fluorescence image under the concentration, wherein R is G/R, performing curve fitting, and performing solution CO2The partial pressure and the ratio r conform to a single exponential decay function:
wherein y is the ratio r and x is CO2The partial pressures, A, t and y0, are constant.
In different CO2To CO at concentration2The response curve of (2) is shown in fig. 1.
Example 2
The optical sensing film was specifically tested for performance as follows:
(1) uniformity: pasting 5cm by 5cm optical sensing film in a self-made glass container, adding pCO2After being stabilized, the standard solution of 40matm is irradiated by an excitation light source to obtain a fluorescence imageAnd then Matlab is used for extracting the red channel and the green channel of the picture, the ratio of the red channel and the green channel is calculated, Origin mapping is used, and the RSD of the optical sensing film at 5cm multiplied by 5cm is calculated to be 0.81 percent, and different CO are calculated2The extraction of the fluorescence image at concentration is shown in FIG. 2.
(2) Reaction time: pCO was prepared by adjusting the amount of NaHCO320mat and pCO2The optical sensing film is attached to the standard solution of 40matm, and pCO is added2In a glass container of 0mat solution, one picture was taken every 10 seconds, and at 5 minutes, the optical sensing film was immediately taken out and put in pCO2In 40mat solution, one picture was taken every 10 seconds, this was repeated 3 times, the pictures were processed with Matlab, and images of the change in fluorescence ratio with time were made with origin, reaction time<40s in different CO2The graph of the change of the lower fluorescence ratio with time is shown in FIG. 3.
Examples of the experiments
Gather the deposit column appearance and the water sample in taihu lake, cut deposit column appearance layering and mixing sieve, get rid of benthos and big particulate matter etc, then add the deposit sample of layering in the cuboid organic glass box of one side detachable, and add lake water and cultivate, after the deposit is stable for 2 weeks, take out the upper cover water, and unpack the one side of dismantling of organic glass box apart, paste the optical sensing membrane of preparation on the detachable organic glass board, then install this organic glass board again, after stabilizing a period, move the organic glass box to the darkroom and acquire the fluorescence image.
According to the method, the CO of the sediment-water interface can be obtained after calculation and drawing2And (4) two-dimensional dynamic distribution. The result shows that the optical sensing film can obtain CO2Gradient distribution at sediment-water interface (see FIG. 4), and CO in the root zone sediment of Sweetgrass2The distribution characteristics (see figure 5) are that the eel grass has higher oxygen secretion capacity which can promote the respiration of rhizosphere microorganisms, so that CO is generated2The partial pressure is increased; in addition, the micro-dynamic state of the sediment-water interface and the root system can be obtained simultaneously, and the requirement of CO in the sediment/soil micro-interface environment can be met2Dynamic state ofAnd (6) detecting.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. An optical sensing film for detecting two-dimensional distribution of carbon dioxide in sediment is characterized in that a preparation method of the optical sensing film comprises the following steps:
the method comprises the following steps: dissolving ethyl cellulose particles in a mixed solution of ethanol and toluene to obtain a polymer solution, and then adding a fluorescent dye, a reference dye and a phase transfer catalyst into the polymer solution to completely dissolve the polymer solution to obtain a mixed solution of the optical sensing membrane;
step two: spraying the mixed solution of the optical sensing film obtained in the step one on a PET (polyethylene terephthalate) base material by using an ultrasonic spraying device, and forming a sensing layer with the thickness of less than 10 microns after the solvent is evaporated;
step three: and (3) mixing the silicon rubber and the diluent to obtain a silicon rubber solution, and after the sensing layer in the second step is completely dried, coating the silicon rubber solution on the surface of the sensing layer and drying.
2. The method for preparing an optical sensing film for detecting two-dimensional distribution of carbon dioxide in sediment according to claim 1, wherein the fluorescent dye is a TOA + PTS 4-ion pair, and the solid obtained by dissolving HPTS and TOABr in NaOH solution and dichloromethane respectively, water bath and vacuum filtration of the mixed solution is TOA + PTS 4-ion pair.
3. The method as claimed in claim 1, wherein the reference dye is solvent orange 63, and the phase transfer catalyst is a TOAOH solution.
4. The method for preparing the optical sensing film for detecting the two-dimensional distribution of the carbon dioxide in the sediment according to claim 1, wherein the diluent is petroleum ether and xylene, and the volume ratio of the petroleum ether to the xylene is 1: 1.5-3, and mixing.
5. The method for preparing an optical sensing film for detecting two-dimensional distribution of carbon dioxide in sediment according to claim 1, wherein the concentration of ethyl cellulose in the polymer solution in the first step is 20g/L, and the volume ratio of ethanol to toluene is 1: 9.
6. The method for preparing an optical sensing film for detecting two-dimensional distribution of carbon dioxide in sediment according to claim 1, wherein the concentration of the NaOH solution is 0.4g/L, the concentration of HPTS is 0.4g/L, and the concentration of TOABr is 1.7 g/L.
7. A calibration method applied to the optical sensing film of claim 1, wherein the calibration method comprises the steps of:
s1: NaCl solution is prepared, and different CO is obtained by adjusting the addition amount of NaHCO32Partial pressure of the solution, measuring the pH and temperature of the solution, and calculating CO by formula2Partial pressure; to be treated with CO2After the partial pressure is stable, the optical sensing film is attached to the inner wall of the transparent container, the optical sensing film is irradiated by an excitation light source, and different CO is obtained by using a CCD camera2Fluorescence images at concentration;
s2 extraction of different CO2And calculating the fluorescence intensity ratio R of the two channels, wherein R is G/R, and performing curve fitting.
8. The method for calibrating an optical sensing film according to claim 7, wherein the concentration of the NaCl solution is 11.388g/L, and the excitation light source is 475 nm.
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