CN110849858A - Dissolved oxygen sensitive film light sensing device and fluorescence efficiency detection system - Google Patents
Dissolved oxygen sensitive film light sensing device and fluorescence efficiency detection system Download PDFInfo
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- CN110849858A CN110849858A CN201911255279.7A CN201911255279A CN110849858A CN 110849858 A CN110849858 A CN 110849858A CN 201911255279 A CN201911255279 A CN 201911255279A CN 110849858 A CN110849858 A CN 110849858A
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- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 107
- 239000001301 oxygen Substances 0.000 title claims abstract description 107
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000001514 detection method Methods 0.000 title claims abstract description 35
- 230000005284 excitation Effects 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 230000035807 sensation Effects 0.000 claims abstract description 27
- 229910052724 xenon Inorganic materials 0.000 claims description 11
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 230000002572 peristaltic effect Effects 0.000 claims description 6
- 230000000638 stimulation Effects 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 238000004061 bleaching Methods 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 description 27
- 239000013307 optical fiber Substances 0.000 description 12
- 230000008901 benefit Effects 0.000 description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 239000003269 fluorescent indicator Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 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
- G01N21/62—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
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Optics & Photonics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
A dissolved oxygen sensitive film light sensation device and a fluorescence efficiency detection system are provided, the dissolved oxygen sensitive film light sensation device comprises a light sensation seat, a water inlet and a water outlet are arranged on the light sensation seat, and dissolved oxygen circulating water is filled in the dissolved oxygen sensitive film light sensation seat; the transparent window is arranged on the side wall of the light sensation seat, and the light source enters the light sensation seat from the transparent window; and a dissolved oxygen sensitive film disposed in the transparent window for receiving the stimulus of the light source and generating excited fluorescence. The invention can accurately adjust the concentration state of the dissolved oxygen through the dissolved oxygen sensitive film luminescence sensing device, can realize the detection of fluorescence efficiency, can obtain the fluorescence emission efficiency, the optimal excitation wavelength, the maximum emission fluorescence wavelength and the fluorescence service life through analysis, improves the utilization rate of light and reduces the bleaching of the dissolved oxygen sensitive film.
Description
Technical Field
The invention relates to the field of physical optics, in particular to a dissolved oxygen sensitive film light sensing device and a fluorescence efficiency detection system.
Background
The fluorescence method for detecting the concentration of the dissolved oxygen has the advantages of no need of electrolyte, no interference and no need of frequent calibration; the advantages of no oxygen consumption, no flow rate limitation and the like make the detection mode become a trend. Most scholars generally select blue light as the excitation light, but some scholars find that the fluorescence effect generated by green light is better in related researches, thereby indicating that the optimal excitation light wavelengths corresponding to different oxygen sensitive materials are different.
Most studies on the characteristics of the oxygen-sensitive membrane have focused on salinity, temperature, pressure, PH in water or concentration of a fluorescent indicator in the oxygen-sensitive membrane, and researchers have studied the difference in the fluorescence efficiency of the oxygen-sensitive membrane caused by the difference in excitation wavelength. For the detection of the fluorescence efficiency of the dissolved oxygen-sensitive membrane, the fluorescence efficiency generated at each wavelength is different because different oxygen-sensitive substances have different fluorescence characteristics. For the excitation light with low efficiency, if the expected fluorescence is generated, the intensity of the excitation light must be enhanced, but the excitation light with too high intensity can generate the bleaching phenomenon of the oxygen-sensitive indicator, and further can influence the service life of the oxygen-sensitive membrane. In the prior art, the wavelength of the exciting light is often selected, a plurality of light sources with different wavelengths are often used, or a fluorescence spectrophotometer is used for detection, so that the oxygen-containing concentration in water is difficult to adjust, the operation is complicated, and the optimal wavelength can be missed. The invention provides a dissolved oxygen sensitive membrane fluorescence efficiency detection device, which can accurately detect the optimal excitation light wavelength, fluorescence emission efficiency, maximum emission fluorescence wavelength, fluorescence service life and the like of an oxygen sensitive membrane, improves the utilization rate of light, and has certain benefits for reducing the bleaching of the dissolved oxygen sensitive membrane.
Disclosure of Invention
In view of the above, one of the main objectives of the present invention is to provide a dissolved oxygen sensitive film light sensing device and a fluorescence efficiency detection system, so as to at least partially solve at least one of the above technical problems.
In order to achieve the above object, as one aspect of the present invention, there is provided a dissolved oxygen sensitive film light-sensing device comprising:
the light sensation seat is provided with a water inlet and a water outlet and is filled with dissolved oxygen circulating water, and the concentration of the dissolved oxygen in the water is continuously adjustable;
the transparent window is arranged on the side wall of the light sensation seat, and the light source enters the light sensation seat from the transparent window; and
and the dissolved oxygen sensitive film is arranged in the transparent window and is used for receiving the stimulation of the light source and generating excited fluorescence.
As another aspect of the present invention, there is also provided a fluorescence efficiency detection system comprising:
a light source providing excitation light;
the monochromator is used for splitting light emitted by the light source to obtain single-wavelength exciting light;
the first spectrometer is used for detecting the light intensity of the single-wavelength exciting light obtained by the light splitting of the monochromator;
the oxygen-sensitive film light-sensing device is used for receiving a light source and generating excited fluorescence, and simultaneously ensures that the concentration of dissolved oxygen is in a dynamic balance environment;
the second spectrometer is used for detecting the fluorescence intensity generated by the oxygen-sensitive film light sensing device; and
and the computer control device is used for obtaining the fluorescence efficiency and the optimal excitation wavelength under each excitation wavelength according to the light intensity of the excitation light and the light intensity of the fluorescence.
Based on the above technical solution, the dissolved oxygen sensitive film light sensing device and the fluorescence efficiency detection system of the present invention have at least one of the following advantages over the prior art:
1. the invention can accurately adjust the concentration state of the dissolved oxygen and can realize the detection of the fluorescence efficiency by the dissolved oxygen sensitive film luminescence sensing device;
2. the fluorescence emission efficiency, the optimal excitation wavelength, the maximum emission fluorescence wavelength and the fluorescence lifetime can be obtained through analysis, the utilization rate of light is improved, and the bleaching of the dissolved oxygen-sensitive membrane is reduced.
Drawings
FIG. 1 is a schematic diagram of a fluorescence efficiency detection system according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an oxygen-sensitive film light-sensing device according to an embodiment of the present invention.
Description of reference numerals:
100-oxygen sensitive film light sensing device; 200-xenon lamps; 300-monochromator; 301-a stepper motor; 302-stepper motor driver; 400-a first spectrometer; 500-a second spectrometer; 600-computer control means; 101-tetrafluoro base; 102-a transparent window; 103-dissolved oxygen sensitive film; 104-a water inlet; 105-a water outlet; 106-a base; 107-external peristaltic pump; 108-dissolved oxygen circulating water; 109-transparent window fixing sheet.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention provides a detection system for the fluorescence efficiency of a dissolved oxygen-sensitive membrane, and designs a light-sensitive structure of the dissolved oxygen-sensitive membrane, which can accurately detect the optimal excitation light wavelength, the fluorescence emission efficiency, the maximum emission fluorescence wavelength, the fluorescence service life and the like of the oxygen-sensitive membrane, greatly shorten the detection time of the fluorescence membrane, and avoid the bleaching of the oxygen-sensitive membrane under the irradiation of low-efficiency strong light.
The invention discloses a dissolved oxygen sensitive film light sensation device, comprising:
the light sensation seat is provided with a water inlet and a water outlet and is filled with dissolved oxygen circulating water;
the transparent window is arranged on the side wall of the light sensation seat, and the light source enters the light sensation seat from the transparent window; and
and the dissolved oxygen sensitive film is arranged in the transparent window and is used for receiving the stimulation of the light source and generating excited fluorescence.
In some embodiments of the present invention, the material used for the light-sensitive seat comprises polytetrafluoroethylene;
in some embodiments of the invention, the dissolved oxygen-sensitive film comprises an oxygen molecule-permeable film and an oxygen-sensitive material.
In some embodiments of the present invention, the dissolved oxygen sensitive film light sensation device further comprises a base for supporting the light sensation seat.
In some embodiments of the invention, the water inlet is connected to an external peristaltic pump.
The invention also discloses a fluorescence efficiency detection system, comprising:
a light source providing excitation light;
the monochromator is used for splitting light emitted by the light source to obtain single-wavelength exciting light;
the first spectrometer is used for detecting the light intensity of the single-wavelength exciting light obtained by the light splitting of the monochromator;
the oxygen-sensitive film light-sensing device is used for receiving a light source and generating excited fluorescence, and simultaneously ensures that the concentration of dissolved oxygen is in a dynamic balance environment;
the second spectrometer is used for detecting the fluorescence intensity generated by the oxygen-sensitive film light sensing device; and
and the computer control device is used for obtaining the fluorescence efficiency and the optimal excitation wavelength under each excitation wavelength according to the light intensity of the excitation light and the light intensity of the fluorescence.
In some embodiments of the invention, the excitation wavelength of the light source is 350 to 550 nanometers.
In some embodiments of the invention, the light source comprises a xenon lamp.
In some embodiments of the invention, the fluorescence efficiency detection system comprises a stepper motor for driving a monochromator.
In some embodiments of the invention, the relationship between the number of steps of the stepper motor and the wavelength of the monochromator beam split satisfies a linear relationship.
In some embodiments of the invention, the first spectrometer has a detection wavelength of 200 to 1160 nanometers;
in some embodiments of the present invention, the detection wavelength of the second spectrometer is 200 to 1160 nanometers.
In one exemplary embodiment, the present invention discloses a detection system for fluorescence efficiency of a dissolved oxygen sensitive membrane, comprising: the system comprises a dissolved oxygen sensitive film light sensing device, a xenon lamp, a monochromator, a stepping motor, a double-path optical fiber (comprising an emission optical fiber and a fluorescence optical fiber), a first spectrometer, a second spectrometer and a computer control device for measuring excitation light and emission spectrum. The dissolved oxygen sensitive film consists of an oxygen molecule permeable film and an oxygen sensitive material and is used for detecting the concentration of oxygen molecules in the solution. The dissolved oxygen sensitive film light sensing device is placed in oxygen-free water, concentration change of dissolved oxygen in the water is adjusted by controlling the amount of sodium sulfite and cobalt chloride added into the oxygen-free water, emitted fluorescence of the dissolved oxygen is detected, the monochromator controls the rotation angle of the grating through the stepping motor, the xenon lamp obtains exciting light with different wavelengths through light splitting and scanning of the monochromator, and the two optical fibers are used for transmitting the intensity of the exciting light and transmitting the intensity of the emitted fluorescence. The dissolved oxygen sensitive film can emit fluorescence with specific wavelength after being irradiated by excitation light. The fluorescence efficiency of the dissolved oxygen-sensitive membrane can be obtained by the intensity ratio of each excitation wavelength to the corresponding fluorescence wavelength, and the optimal excitation wavelength of the oxygen-sensitive membrane can be determined by wavelength scanning.
In another exemplary embodiment, the dissolved oxygen sensitive membrane fluorescence efficiency detection system of the present invention comprises: the system comprises a xenon lamp, a monochromator, a first spectrometer, a second spectrometer, a dissolved oxygen sensitive film light sensing device and a computer control device.
Wherein, dissolve oxygen sensitive membrane light sense device: circulating oxygen-free water driven by a pump and sodium sulfite and cobalt chloride reagents added in the oxygen-free water simulate water samples with different dissolved oxygen concentrations, one surface of an oxygen sensitive film is immersed in the water, oxygen molecules penetrate through the film surface to be combined with a light sensitive material, the other surface of the oxygen sensitive film is connected with a transparent window, the light sensitive surface is irradiated by incident light of an optical fiber through the transparent window, and fluorescence emitted by the dissolved oxygen sensitive film enters a detection optical fiber after passing through the transparent window;
the dissolved oxygen sensitive film light sensation device comprises an oxygen-free water and oxygen concentration circulating adjustment structure, a fixed seat, a transparent window and the like, can simulate the change state of the dissolved oxygen concentration and is connected with the excitation light and the second spectrometer, and the detection of the fluorescence luminous efficiency is realized.
Light emitted by a xenon lamp light source is split by a monochromator to obtain exciting light with single wavelength, the exciting light respectively enters a first spectrometer and a dissolved oxygen sensitive film light sensing device through two optical fibers, and a stepping motor controls the rotation angle scanning wavelength of a grating in the monochromator to realize the random adjustment of the exciting wavelength;
wherein the computer control means: the fluorescence of the dissolved oxygen-sensitive film is received by a fluorescence spectrometer after passing through an emission optical fiber, and a fluorescence intensity spectrum is obtained; and the computer control device compares the excitation light spectrum with the fluorescence spectrum, and finally calculates the fluorescence emission efficiency, the optimal excitation light wavelength, the maximum emission fluorescence wavelength and the fluorescence service life of the oxygen-sensitive membrane.
A linear relation exists between the rotating step number n of the stepping motor and the light splitting wavelength lambda of the monochromator, lambda is an + b, and a and b are coefficients and constants obtained by fitting experimental data respectively; and the required single-wavelength exciting light can be accurately found through the linear relation.
The technical solution of the present invention is further illustrated by the following specific embodiments in conjunction with the accompanying drawings. It should be noted that the following specific examples are given by way of illustration only and the scope of the present invention is not limited thereto.
The system for detecting the fluorescence efficiency of the dissolved oxygen sensitive membrane provided by the embodiment, referring to fig. 1, includes: the device comprises a dissolved oxygen sensitive film light sensation device 100, a xenon lamp 200, a monochromator 300, a stepping motor 301, a double-path optical fiber, a first spectrometer 400, a second spectrometer 500 and a computer control device 600 for measuring excitation light and emission spectrum.
Light emitted by a light source of the xenon lamp 200 is split by a monochromator to obtain exciting light with single wavelength, and the exciting light enters the first spectrometer 400 and the dissolved oxygen sensitive film light sensing device 100 through two paths of optical fibers respectively; the stepping motor 301 controls the grating rotation angle scanning wavelength in the monochromator to realize the arbitrary adjustment of the excitation wavelength;
a dissolved oxygen sensitive membrane light sensing device 100 is shown in fig. 2 and comprises a tetrafluoro seat 101, a transparent window 102, a dissolved oxygen sensitive membrane 103, a transparent window fixing plate 109, an external peristaltic pump 107, a base 106, dissolved oxygen circulating water 108, a water inlet 104 and a water outlet 105, wherein the external peristaltic pump 107 drives the circulating anoxic water and sodium sulfite and cobalt chloride reagents added in the circulating anoxic water to simulate water samples with different dissolved oxygen concentrations, one surface of the dissolved oxygen sensitive membrane 103 is immersed in water, oxygen molecules penetrate through the membrane surface to be combined with a light sensitive material, the other surface of the dissolved oxygen sensitive membrane is connected with the transparent window 102, optical fiber incident light irradiates the light sensitive surface through the transparent window 102, and fluorescence emitted by the oxygen sensitive membrane 103 enters a detection optical fiber after passing through the transparent;
the first spectrometer 400 and the second spectrometer 500 respectively receive the light intensity from the emission fiber and the fluorescence fiber, and finally transmit the light intensity to the PC (i.e., the computer control device 600), and the fluorescence emission efficiency, the optimal excitation wavelength, the maximum emission fluorescence wavelength, the fluorescence lifetime, and the like are obtained after calculation and analysis.
Wherein the dissolved oxygen-sensitive film is produced by Aandera company, the wavelength range of the exciting light of the light source is selected between 350-550nm, and the step interval between the single exciting wavelengths is 1 nm. The xenon lamp is powered by a programmable stabilized voltage supply to work under a rated voltage, the models of the first spectrometer 400 and the second spectrometer 500 are both AvaPec-HS 1024x58TEC, and the detection wavelength range is 200nm-1160 nm.
The whole operation steps are as follows:
(1) opening an external peristaltic pump 107 to enable dissolved oxygen circulating water to start circulating; after the light source is turned on for 10min, subsequent operation is carried out to ensure that the xenon lamp 200 tends to be stable; the stepping motor 301 is controlled to rotate, and the intensity of the exciting light with the wavelength band of 350-550nm and the interval of 1nm is recorded.
(2) And (3) recording the corresponding fluorescence intensity in the dissolved oxygen-sensitive film light-sensing device 100 while the step (2) is performed, and storing the fluorescence intensity in a computer.
(3) The fluorescence spectrum and the excitation light spectrum are processed as in formula (1), wherein I1Is the intensity of a single wavelength excitation light, I2The fluorescence generated for the corresponding wavelength, a is the proportionality coefficient between the integration times of the two corresponding spectrometers, η is the efficiency of the fluorescence sought, comparing η can find the optimum excitationEmission wavelength, maximum emitted fluorescence wavelength, and fluorescence lifetime.
In summary, it is not feasible to simply compare the fluorescence intensities generated by different wavelengths, and it is necessary to find the optimal excitation light wavelength from the viewpoint of efficiency. The method provided by the invention can meet the requirements, improve the utilization rate of light, reduce the bleaching of the oxygen-sensitive film and prolong the service life of the oxygen-sensitive film.
Those skilled in the art will appreciate that the drawings are only schematic illustrations of preferred embodiments, and the above-described embodiments of the present invention are merely provided for description and do not represent the merits of the embodiments.
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 (10)
1. A dissolved oxygen sensitive film light sensing device, comprising:
the light sensation seat is provided with a water inlet and a water outlet and is filled with dissolved oxygen circulating water;
the transparent window is arranged on the side wall of the light sensation seat, and the light source enters the light sensation seat from the transparent window; and
and the dissolved oxygen sensitive film is arranged in the transparent window and is used for receiving the stimulation of the light source and generating excited fluorescence.
2. The dissolved oxygen sensitive film light sensation device according to claim 1,
the light sensation seat is made of polytetrafluoroethylene;
the dissolved oxygen-sensitive film comprises an oxygen molecule permeable film and an oxygen-sensitive material.
3. The dissolved oxygen sensitive film light sensation device according to claim 1,
the dissolved oxygen sensitive film light sensation device also comprises a base used for supporting the light sensation seat.
4. The dissolved oxygen sensitive film light sensation device according to claim 1,
the water inlet is connected with an external peristaltic pump.
5. A fluorescence efficiency detection system, comprising:
a light source providing excitation light;
the monochromator is used for splitting light emitted by the light source to obtain single-wavelength exciting light;
the first spectrometer is used for detecting the light intensity of the single-wavelength exciting light obtained by the light splitting of the monochromator;
the oxygen-sensitive film photosensitive device of any one of claims 1 to 4, for receiving a light source and generating excited fluorescence while ensuring a dissolved oxygen concentration in a dynamic equilibrium environment;
the second spectrometer is used for detecting the fluorescence intensity generated by the oxygen-sensitive film light sensing device; and
and the computer control device is used for obtaining the fluorescence efficiency and the optimal excitation wavelength under each excitation wavelength according to the light intensity of the excitation light and the light intensity of the fluorescence.
6. The fluorescence efficiency detection system according to claim 5,
the excitation wavelength of the light source is 350 to 550 nanometers.
7. The fluorescence efficiency detection system according to claim 5,
the light source comprises a xenon lamp.
8. The fluorescence efficiency detection system according to claim 5,
the fluorescence efficiency detection system includes a stepper motor for driving a monochromator.
9. The fluorescence efficiency detection system according to claim 5,
the relation between the step number of the stepping motor and the light splitting wavelength of the monochromator meets a linear relation.
10. The fluorescence efficiency detection system according to claim 5,
the detection wavelength of the first spectrometer is 200 to 1160 nanometers;
the detection wavelength of the second spectrometer is 200 to 1160 nanometers.
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Cited By (1)
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