CN116429741A - Portable fluorescence detection module and method for detecting pollutants - Google Patents
Portable fluorescence detection module and method for detecting pollutants Download PDFInfo
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- G—PHYSICS
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- 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
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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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
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Abstract
The invention belongs to the technical field of fluorescence sensing, and particularly relates to a portable fluorescence detection module and a method for detecting pollutants. The portable fluorescence detection module of the invention comprises: the light source module comprises an LED lamp and a TIR lens, wherein the TIR lens is used for collimating light rays emitted by the LED lamp; the detection module comprises an excitation filter, a fluorescence sensitive element, a beam converging lens and an emission filter which are sequentially arranged; and the signal processing module is used for performing signal processing on the second wavelength light beam. In the portable fluorescence detection module, key components such as the excitation filter, the fluorescence sensing element, the beam-converging lens, the emission filter and the like in the light source module and the detection module are in modularized design, so that the portable fluorescence detection module can be replaced conveniently. The portable fluorescence detection module can be used for detecting liquid and gas samples.
Description
Technical Field
The invention belongs to the technical field of fluorescence sensing, and particularly relates to a portable fluorescence detection module and a method for detecting pollutants.
Background
Currently, the number of users using smart phone devices worldwide has broken through 50 million people. Smartphones have become an important tool in people's daily lives. With the development of technology, smart phones are already a mobile multifunctional miniaturized computer with independent operating systems and storage spaces, and can be used for installing various application programs provided by service providers by users themselves and realizing wireless access and signal transmission through a mobile communication network.
The fluorescence detection method is one of the detection methods with highest sensitivity in all detection methods at present, and has high selectivity and stability. Fluorescence spectroscopy, which is an emission spectrum, is a method of reflecting properties of a substance from spectral information. The fluorescence intensity is linear with the molecular density in a certain range, so that the fluorescent probe can be used for quantitative analysis of substances.
However, the existing fluorescence and fluorescence spectrum detection system has large instrument volume, and can not meet the requirements of users on rapidness, real-time, convenient carrying and simple use. Therefore, the volume of the fluorescence detection equipment is miniaturized, the photoelectric detection technology and the mobile application development technology are combined, and the fluorescence detection is faster and quicker by utilizing the control function, the quick data processing capability and the various networking functions of the smart phone, so that the fluorescence detection is an urgent need of the type of instrument at present.
However, the current portable fluorescence detection system can only realize one detection mode of gas or liquid, has insufficient functions, and is more difficult to realize detection of various different substances by using different excitation wavelengths. When multiple samples are required to be detected, multiple sensors are required to be used, and detection is not convenient enough. The fluorescence detector based on the smart phone has more single function, and usually only single fluorescent substance detection is realized. In addition, there is a problem in that focusing of the emission light path is difficult when assembling.
Accordingly, there is a need to provide an improved solution to the above-mentioned deficiencies of the prior art.
Disclosure of Invention
The invention aims to provide a portable fluorescence detection module and a method for detecting pollutants, which are used for solving or improving at least one of the problems that the existing fluorescence detection system can only realize detection of gas or liquid, has poor detection convenience, has single function and is difficult to focus an emission light path during assembly.
In order to achieve the above object, the present invention provides the following technical solutions: a portable fluorescence detection module includes: the light source module comprises an LED lamp and a TIR lens, wherein the TIR lens is used for collimating light rays emitted by the LED lamp; the detection module comprises an excitation filter, a fluorescence sensitive element, a beam-converging lens and an emission filter which are sequentially arranged, wherein the excitation filter is used for receiving emergent light of the TIR lens and filtering the emergent light to generate a first wavelength light beam, the fluorescence sensitive element is used for contacting a sample to be detected and generating fluorescence under the excitation of the first wavelength light beam, the beam-converging lens is used for converging the fluorescence emitted by the fluorescence sensitive element, and the emission filter is used for receiving the emergent light of the beam-converging lens and filtering the emergent light to generate a second wavelength light beam; and the signal processing module is used for performing signal processing on the second wavelength light beam.
Preferably, the beam converging lens comprises a Fresnel lens and a biconcave lens; the Fresnel lens is arranged between the fluorescent sensing element and the biconcave lens.
Preferably, the detection module further comprises a reaction cavity, wherein a fluorescent sensing element fixing groove is formed in the reaction cavity, and the fluorescent sensing element is detachably arranged in the fluorescent sensing element fixing groove.
Preferably, the light source module further comprises a power supply electrically connected with the LED lamp through a constant voltage circuit module; the light source module further comprises a housing, the housing is provided with an inner cavity for accommodating the power supply, the constant voltage circuit module, the LED lamp and the TIR lens, and the housing is communicated with the detection module.
Preferably, the fluorescence sensing element is a gas fluorescence sensing element, the gas fluorescence sensing element comprises a quartz substrate and a fluorescence sensing film arranged on the surface of the quartz substrate, and the fluorescence sensing film is prepared by soaking and drying a film material by adopting a solution containing a fluorescence sensing material; and the reaction cavity is provided with an air inlet and an air outlet.
Preferably, the fluorescence sensing element is a liquid fluorescence sensing element, and the liquid fluorescence sensing element comprises a cuvette and a fluorescence sensing material solution arranged in the cuvette.
Preferably, the portable fluorescence detection module further comprises a fixing clamp, and the detection module is connected with the signal processing module through the fixing clamp.
The invention also provides a method for detecting the concentration of pollutants, which adopts the following technical scheme: a method for detecting the concentration of pollutants adopts the portable fluorescence detection module to detect.
Preferably, the sample to be detected is a gas pollutant, wherein the gas pollutant contains nitrobenzene, and the concentration of nitrobenzene in the gas pollutant is 0-30mg/L; or the sample to be detected is nitrobenzene solution, and the concentration of nitrobenzene in the nitrobenzene solution is 0-100mg/L; the composition of the fluorescence sensitive element comprises a fluorescence sensitive material, and the fluorescence sensitive material is MOFs.
Preferably, the center wavelength of the excitation filter is 280nm, and the bandwidth is 10nm; the center wavelength of the emission filter is 545nm, and the bandwidth is 20nm.
The beneficial effects are that:
in the portable fluorescence detection module, key components such as the excitation filter, the fluorescence sensing element, the beam-converging lens, the emission filter and the like in the light source module and the detection module are in modularized design, so that the portable fluorescence detection module can be replaced conveniently. The portable fluorescence detection module can be used for detecting liquid and gas samples.
In addition, the portable fluorescence detection module uses coaxial focusing detection, the beam converging lens converges the emitted light rays emitted by the fluorescence sensitive element, the converged light rays are concentrated and uniformly distributed, and an accurate measurement result can be obtained without complex calibration when the signal processing module and the detection module are assembled.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. Wherein:
FIG. 1 is a schematic diagram of the overall structure of a portable fluorescence detection module according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing an exploded structure of a light source module and a detection module of a portable fluorescence detection module according to an embodiment of the present invention;
FIG. 3 is a cross-sectional view of a light source module and a detection module of a portable fluorescence detection module according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of a detection module of a portable fluorescence detection module according to an embodiment of the present invention;
FIG. 5 is a light transmission path diagram of a portable fluorescence detection module according to an embodiment of the present invention in a liquid contaminant detection mode;
FIG. 6 is a diagram illustrating a light transmission path of a portable fluorescence detection module according to an embodiment of the present invention in a gas contaminant detection mode;
FIG. 7 is a graph showing the change in fluorescence intensity (excitation wavelength 282 nm) of a nitrobenzene solution of different concentrations detected by the portable fluorescence detection module of the present invention in example 1;
FIG. 8 is a graph showing the correspondence between fluorescence intensity and solution concentration (excitation wavelength 282 nm) when the portable fluorescence detection module of the present invention is used to detect nitrobenzene solution in example 1;
FIG. 9 is a graph showing the change in fluorescence intensity (excitation wavelength: 282 nm) of the portable fluorescence detection module according to the present invention in example 2 when detecting nitrobenzene gases of different concentrations;
FIG. 10 shows the correspondence between fluorescence intensity and gas concentration (excitation wavelength: 282 nm) when nitrobenzene gas is detected by the portable fluorescence detection module according to the present invention in example 2.
Reference numerals:
1-a light source module; 2-a detection module; 3-fixing clips; 4-a signal processing module; 5-a first wavelength beam; 6-a second wavelength beam;
101-a housing; 102-a power supply; 103-LED lamps; 104-a TIR lens;
20-mounting box; 201-excitation filter grooves; 202-an excitation filter; 203-air inlet; 204-top cover; 205-emission filter; 206-fresnel lens; 207-biconcave lens; 208-an emission filter recess; 209-biconcave lens groove; 210-fresnel lens groove; 211-fluorescent sensitive element fixing grooves; 211A-a first fixing plate; 211B-a second fixing plate; 211C-a third fixing plate; 211D-square grooves; 211E-I shaped grooves; 212-an air outlet; 213-reaction chamber; 214-fluorescent sensor;
301-a threaded mounting hole; 302-fixing screws.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the invention, fall within the scope of protection of the invention.
In the description of the present invention, it should be understood that references to orientation descriptions such as upper, lower, front, rear, left, right, etc. are based on the orientation or positional relationship shown in the drawings, are merely for convenience of description of the present invention and to simplify the description, and do not indicate or imply that the apparatus or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
In the description of the present invention, a number means one or more, a number means two or more, and greater than, less than, exceeding, etc. are understood to not include the present number, and above, below, within, etc. are understood to include the present number. The description of the first and second is for the purpose of distinguishing between technical features only and should not be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of the technical features indicated.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, features defining "first" and "second" may explicitly or implicitly include one or more features.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the term "connected" should be construed broadly, and for example, it may be a fixed connection or an active connection, or it may be a detachable connection or a non-detachable connection, or it may be an integral connection; may be mechanically connected, may be electrically connected, or may be in communication with each other; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements, indirect communication or interaction relationship between the two elements.
The present invention will be described in detail with reference to examples. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention provides a portable fluorescence detection module aiming at least one of the problems of low detection convenience, single function and difficulty in focusing an emission light path during assembly of a current fluorescence detection system, wherein the detection of gas or liquid can only be realized. Referring to fig. 1 to 4, a portable fluorescence detection module according to an embodiment of the present invention includes: the light source module 1 comprises an LED lamp 103 and a TIR lens 104, wherein the TIR lens 104 is used for collimating light rays emitted by the LED lamp 103; the detection module 2 comprises an excitation filter 202, a fluorescence sensing element 214, a beam-converging lens and an emission filter 205 which are sequentially arranged, wherein the excitation filter 202 is used for receiving emergent light of the TIR lens 104 and filtering the emergent light to generate a first wavelength light beam 5, the fluorescence sensing element 214 is used for contacting a sample to be detected and generating fluorescence under excitation of the first specific wavelength light beam 5, the beam-converging lens is used for converging the fluorescence emitted by the fluorescence sensing element 214, and the emission filter 205 is used for receiving emergent light of the beam-converging lens and filtering the emergent light to generate a second wavelength light beam 6; the signal processing module 4, the signal processing module 4 is configured to perform signal processing on the second wavelength light beam 6 (emitted by the emission filter 205).
In the portable fluorescence detection module, key components such as the excitation filter 202, the fluorescence sensing element 214, the beam converging lens, the emission filter 205 and the like in the light source module 1 and the detection module 2 are in a modularized design, so that the portable fluorescence detection module can be replaced conveniently, and detection of different samples is realized. In addition, in the light source module 1, the TIR lens 104 is used for collimating the light rays of the LED lamp 103, so that the light source utilization rate is improved, the excitation requirement can be met even if the low-power LED lamp 103 is used, and further the problem that the light source module 1 heats seriously due to the fact that the power is too high is avoided.
In addition, the portable fluorescence detection module of the present invention uses coaxial focusing detection, the beam converging lens converges the emitted light rays emitted by the fluorescence sensitive element 214, the converged light rays are concentrated and uniformly distributed, and when the signal processing module 4 and the detection module 2 are assembled, accurate measurement results can be obtained without complex calibration.
Preferably, the excitation filter and the emission filter 205 are both bandpass filters.
In the preferred embodiment of the invention, the converging lens includes a Fresnel lens 206 and a biconcave lens 207; a fresnel lens 206 is arranged between the fluorescent sensitive element and the biconcave lens 207. The portable fluorescence detection module uses coaxial focusing detection, does not comprise complex structures such as a motor, a turntable and the like, uses the thinner Fresnel lens 206 for focusing, reduces the volume of a detection device and reduces the loss of light rays in transmission. The beam converging lens formed by combining the fresnel lens 206 and the biconcave lens 207 is used for converging the emitted light rays emitted by the fluorescent sensing element 214, the converged light rays are concentrated and uniformly distributed, and when the signal processing module 4 (for example, a smart phone can be used as the signal processing module 4) is assembled with the detection module 2, an accurate measurement result can be obtained without complex calibration.
In a preferred embodiment of the present invention, the detection module 2 further includes a reaction chamber 213, wherein a fluorescent sensing element fixing groove 211 is disposed in the reaction chamber 213, and a fluorescent sensing element 214 is detachably disposed in the fluorescent sensing element fixing groove 211.
In a preferred embodiment of the present invention, excitation filter 202, fluorescence sensing element 214, a converging lens (including fresnel lens 206 and biconcave lens 207), emission filter 205, and reaction chamber 213 are assembled within a mounting box 20 having a cavity. Specifically, the mounting box 20 is provided therein with an excitation filter groove 201 (for fixing the excitation filter 202 inside the mounting box 20), a fluorescence sensor fixing groove 211 (for fixing the fluorescence sensor 214 inside the mounting box 20), a converging lens groove (for fixing the converging lens inside the mounting box 20; preferably, the converging lens groove includes a fresnel lens groove 210 and a biconcave lens groove 209 in order to achieve fixation of the fresnel lens 206 and the biconcave lens 207 inside the mounting box 20), an emission filter groove 208 (for fixing the emission filter 205 inside the mounting box 20), and a beam path; the excitation filter groove 201, the fluorescence-sensitive element fixing groove 211, the converging lens groove, and the emission filter groove 208 are in communication with the beam channel (preferably, for example, the beam channel may be formed by opening holes in the walls of the excitation filter groove 201, the fluorescence-sensitive element fixing groove 211, the converging lens groove, and the emission filter groove 208, respectively); the beam path is used for conducting light. The beam path is a structure that allows light inside the mounting box 20 to pass through (light emitted from the light source module 1 can be transmitted in, and light emitted from the emission filter 205 can be transmitted out).
Preferably, the openings of the excitation filter groove 201, the converging lens groove, and the emission filter groove 208 are provided at the upper surface of the mounting box 20 so as to fit the excitation filter 202, the converging lens, and the emission filter 205 in the mounting box 20. In addition, light holes are formed on the walls of the excitation filter groove 201, the beam converging lens groove and the emission filter groove 208, respectively, and the light holes on the walls of the excitation filter groove 201, the beam converging lens groove and the emission filter groove 208 are coaxially arranged so as to form a beam channel allowing light to be conducted in the mounting box 20.
Preferably, the reaction chamber 213 is a light-tight sealed chamber, so as to avoid the influence of light and gas outside the reaction chamber 213 on the detection result. Preferably, the mounting box 20 is provided with a top cover 204 for sealing the reaction cavity 213, and the top cover 204 is matched with the reaction cavity 213 to ensure light shielding and sealing performance of the reaction cavity 213. The top cover 204 is also provided to facilitate adjustment of the fluorescent sensor 214 in the reaction chamber 213 (e.g., when the sample to be measured is changed from liquid to gas (or from gas to liquid), the fluorescent sensor 214 needs to be changed)
More preferably, the fluorescent sensing element fixing groove 211 is formed at the bottom of the mounting case 20 according to the shape and size of the fluorescent sensing element.
The fluorescence sensing element fixing groove 211 can fix a container (such as a cuvette) containing a liquid sample used in liquid detection, can bear a gas fluorescence sensing element used in gas detection, combines a modularized design, reduces the volume of the detection device, can be assembled according to specific requirements, and can meet the requirements of various detection scenes.
In the preferred embodiment of the present invention, the light source module 1 further includes a power supply 102 (preferably, the light source module 1 further includes a constant voltage circuit module adapted to the power supply 102), and the power supply 102 is electrically connected to the LED lamp 103 through the constant voltage circuit module; the light source module 1 further includes a housing 101, the housing 101 having an inner cavity accommodating a power supply 102, a constant voltage circuit module, an LED lamp 103, and a TIR lens 104, the housing 101 being in communication with the detection module 2 (so that outgoing light of the TIR lens 104 can be received by the detection module 2. Specifically, light conduction can be achieved by way of starting holes in the housing 101 and the detection module 2, respectively). The arrangement of the power supply 102 in the light source module 1 is helpful to solve the problem that the fluorescent detection device is inconvenient for outdoor use. The power source 102 may be a conventional or rechargeable button cell. The LED lamp 103 is a full spectrum white light LED or an ultraviolet LED or other special wavelength LED.
Preferably, the housing 101 of the light source module 1 is fixedly connected with the mounting box 20 of the detection module 2 (for example, a threaded connection manner may be adopted); the housing 101 is provided with a first through hole, and the mounting box 20 is provided with a second through hole, and the first through hole is communicated with the second through hole so as to conduct outgoing light of the light source module 1 to the detection module 2.
In the preferred embodiment of the present invention, the fluorescence sensing element 214 is a gas fluorescence sensing element, and the gas fluorescence sensing element comprises a quartz substrate and a fluorescence sensing film arranged on the surface of the quartz substrate, wherein the fluorescence sensing film is prepared by soaking and drying a film material by adopting a solution containing a fluorescence sensing material; the mounting box 20 is provided with an air inlet 203 and an air outlet 212 (the air inlet 203 and the air outlet 212 are respectively communicated with the reaction cavity 213; preferably, a micro air pump is arranged at the air inlet 203 so that air or gas to be detected enters the reaction cavity 213, and the gas to be detected is fully contacted with the fluorescence sensitive element, so that the detection effect is ensured). Referring to fig. 3 and 6, the portable fluorescence detection module of the present invention, when detecting a gas sample (in a gas sample detection mode): firstly, selecting a light source module 1 and an optical filter (an excitation optical filter and an emission optical filter) according to the property of a sample to be detected, and assembling a detection device; and then the micro air pump at the air inlet 203 and the air outlet 212 is operated to make the gas to be tested fully contact with the gas fluorescence sensitive element. Light rays emitted by the LEDs are collimated and converged by the TIR lens 104 and then become uniform parallel light beams, the uniform parallel light beams are irradiated on the excitation filter 202, the excitation filter 202 filters the light beams to generate first-wavelength light beams 5, and the first-wavelength light beams serve as excitation light and are irradiated on the gas fluorescence sensitive element. The gas fluorescence sensitive element is excited to generate fluorescence, and the fluorescence is converged into concentrated and uniform light through the Fresnel lens 206 and the biconcave lens 207, the concentrated and uniform light irradiates on the emission filter 205, and the stray light is filtered by the emission filter 205 to generate a second-wavelength light beam 6; the second wavelength light beam 6 irradiates the signal processing module 4 (for example, a smart phone may be used as the signal processing module 4, so that the second wavelength light beam 6 irradiates an ambient light sensor of the smart phone), and the concentration of the sample to be measured is obtained by analysis by the signal processing module 4 (for example, a smart phone may be used as the signal processing module 4).
In a preferred embodiment of the present invention, the fluorescent sensing element is a liquid fluorescent sensing element comprising a cuvette and a solution of a fluorescent sensing material arranged in the cuvette. Referring to fig. 5, the portable fluorescence detection module of the present invention is used for detecting a liquid sample (in a liquid sample detection mode): firstly, a light source module 1 and a light filter (an excitation light filter and an emission light filter) are selected according to the property of a sample to be detected, a detection device is assembled, then detection is started, light rays emitted by an LED are collimated and converged by a TIR lens 104 and then become uniform parallel light beams, the uniform parallel light beams are irradiated on an excitation light filter 202, the excitation light filter 202 filters and generates a first wavelength light beam 5 which is used as excitation light and irradiates on a cuvette containing the sample to be detected, fluorescence generated by the sample is converged by a Fresnel lens 206 and a biconcave lens 207 and becomes uniform light rays, the concentrated and uniform light rays irradiate on an emission light filter 205, and the emission light filter 205 filters stray light to generate a second wavelength light beam 6; the second wavelength light beam 6 irradiates on an ambient light sensor of the smart phone (for example, the smart phone can be used as the signal processing module 4, so that the second wavelength light beam 6 irradiates on the ambient light sensor of the smart phone), and the signal processing module 4 (for example, the smart phone can be used as the signal processing module 4) analyzes to obtain the concentration of the sample to be detected.
Referring to fig. 4, in a preferred embodiment of the present invention, the fluorescent sensing element fixing grooves 211 include a gas fluorescent sensing element fixing groove and a liquid fluorescent sensing element fixing groove. Preferably, the fluorescent sensing element fixing groove comprises a first fixing plate 211A, a second fixing plate 211B and a third fixing plate 211C, and the structures of the first fixing plate 211A and the second fixing plate 211B are arranged in a mirror symmetry way; after the first, second and third fixing plates 211A, 211B and 211C are assembled, square grooves 211D having square cross sections (taken in the direction from left to right (A-A) in fig. 4) and I-shaped grooves 211E having "I" -shaped cross sections are simultaneously formed. Wherein, the square groove 211D may be used for placing a cuvette (liquid fluorescence sensor) so as to fix the liquid fluorescence sensor; the I-shaped groove 211E may be used to place a gas fluorescent sensor so as to facilitate fixation of the gas fluorescent sensor.
Referring to fig. 1-3, in a preferred embodiment of the present invention, the portable fluorescence detection module further includes a fixing clip 3, and the detection module 2 (mounting box 20) is connected to the signal processing module 4 through the fixing clip 3. Preferably, the detection module 2 (the mounting box 20) is provided with a through hole for allowing the second wavelength light beam 6 to pass therethrough, and the through hole is disposed corresponding to the fixing clip 3 (so that the second wavelength light beam 6 emitted through the through hole is received by the signal processing module 4). Specifically, to better realize the fixation of the signal processing module 4, the fixing clip 3 is L-shaped, one end of the fixing clip 3 is connected with the mounting box 20, and a space for accommodating the signal processing module 4 is formed between the other end and the mounting box 20; the fixing clamp 3 is provided with a threaded mounting hole 301, the signal processing module 4 is arranged in the space between the mounting box 20 and the fixing clamp 3, then a fixing screw 302 is arranged in the threaded mounting hole 301, and the fixing screw 302 is screwed to be abutted against the surface of the signal processing device, so that the fixing of the signal processing device can be realized.
Preferably, the signal processing module 4 is a mobile phone (the mobile phone has an ambient light sensor to collect and analyze the second wavelength light beam 6 to obtain the concentration of the sample to be measured).
The invention also provides a method for detecting the concentration of the pollutant, and the method for detecting the concentration of the pollutant adopts the portable fluorescence detection module for detection.
In the preferred embodiment of the method for detecting the pollutants, the sample to be detected is the gas pollutants, the gas pollutants contain nitrobenzene, and the concentration of the nitrobenzene in the gas pollutants is 0-30mg/L; or the sample to be detected is nitrobenzene solution, and the concentration of nitrobenzene in the nitrobenzene solution is 0-100mg/L; the fluorescent sensitive material is MOFs. MOFs fluorescent detection technology is a technology for detecting and identifying a sample to be detected by utilizing the change of basic photophysical properties such as excited state service life, fluorescence anisotropy, fluorescence spectrum shape and characteristic spectrum, fluorescence intensity, fluorescence polarization and the like generated after a substance to be detected reacts with a corresponding fluorescent substance. The MOFs has the advantages of being applied to the portable fluorescence detection module for detecting organic pollutants: the detection sensitivity is high, the selectivity is good, the detection can be recycled after simple cleaning such as ethanol cleaning, and the detection has good stability.
In a preferred embodiment of the method of detecting contaminants of the present invention, the excitation filter 202 has a center wavelength of 280nm and a bandwidth of 10nm; the center wavelength of the emission filter 205 was 545nm and the bandwidth was 20nm.
Preferably, the fluorescent sensitive material is Tb-MOFs, and Tb-MOFs is adopted as a component part of the fluorescent sensitive element in the portable fluorescent detection module for detecting the paranitrobenzene, so that the sensitivity of detecting the concentration of the paranitrobenzene gas is improved, and the fluorescent detection limit of the paranitrobenzene gas can reach 2.443mg/L, which is obviously superior to the prior art.
Tb-MOFs used in the following examples were prepared by the following procedure:
(1) Methanol and deionized water are mixed according to the proportion of 1:1 and stirred uniformly to prepare 50% aqueous methanol solution for standby.
(2) Tb (NO) 3 ) 3 ·6H 2 Dissolving O, 1,10-phen, H4btec and sodium hydroxide in the solvent prepared in the step (1) and uniformly stirring; wherein Tb (NO) 3 ) 3 ·6H 2 The molar ratio of O, 1,10-phen and H4btec is 1:1:1; sodium hydroxide is used for adjusting the pH of the mixed solution to about 5.0, the pH is important for the coordination mode of H4btec, and different molecular structures can be generated by different pH values; the solvent in the step (1) provides a reaction environment for the hydrothermal reaction while achieving uniform mixing of the raw materials.
(3) Pouring the mixed solution into a reaction kettle, heating for 12 hours in an oven at 140 ℃, and cooling to obtain white powder.
(4) The white powder obtained was washed several times with deionized water in a suction filter and dried under vacuum at 60 ℃. The Tb-MOFs material is fully ground after removal.
Example 1
The embodiment further describes the portable fluorescence detection module of the invention in combination with the detection of the p-nitrobenzene solution.
In the liquid contaminant detection mode test (i.e., the fluorescent sensor used is a liquid fluorescent sensor; the light transmission path is as shown in FIG. 5), tb-MOFs powder was used for measurement.
According to the fluorescence property of the prepared Tb-MOFs, an ultraviolet LED lamp 103 with the peak wavelength of 285nm is selected as an excitation light source; a filter with a center wavelength of 280nm and a bandwidth of 10nm is used as the excitation filter 202; a band-pass filter with a center wavelength of 545nm and a bandwidth of 20nm was used as the emission filter 205; the portable fluorescence detection module is assembled.
Fluorescent probe solution preparation:
(1) 50mg of Tb-MOFs powder was dispersed in methanol and stirred for 30min using a magnetic stirrer to prepare a Tb-MOFs suspension.
(2) Nitrobenzene solutions (0, 10, 20, 30, 40, 50, 70, 100, 150, 200, 250 mg/L) were prepared at different concentrations.
(3) The nitrobenzene solution with different concentrations is taken by a cuvette, 5mg of Tb-MOFs powder is added and placed in a fluorescent sensitive element fixing groove 211, and the concentration of pollutants can be obtained by measuring the fluorescence intensity of the nitrobenzene solution by using the portable fluorescent detection module. Through experiments, the portable fluorescence detection module has good linearity when detecting nitrobenzene solution with the concentration of 0-100 mg/L. The fluorescence detection limit of the p-nitrobenzene is 1.175mg/L.
FIG. 7 is a graph showing the change in fluorescence intensity (excitation wavelength 282 nm) of the portable fluorescence detection module according to the present invention in example 1 when detecting nitrobenzene solutions of different concentrations;
FIG. 8 shows the correspondence between fluorescence intensity and solution concentration (excitation wavelength: 282 nm) when the portable fluorescence detection module of the present invention detects nitrobenzene solution in example 1.
Example 2
The embodiment further describes the portable fluorescence detection module of the invention in combination with the detection of paranitrobenzene gas.
In the gas contaminant detection mode test (light transmission path is shown in FIG. 6), the measurement was performed using Tb-MOFs fluorescent film.
According to the fluorescence property of the prepared Tb-MOFs, an ultraviolet LED lamp 103 with the peak wavelength of 285nm is selected as an excitation light source; a filter with a center wavelength of 280nm and a bandwidth of 10nm is used as the excitation filter 202; a band-pass filter with a center wavelength of 545nm and a bandwidth of 20nm was used as the emission filter 205; the portable fluorescence detection module is assembled.
And (3) detecting nitrobenzene gas:
(1) Dissolving 40mg of Tb-MOFs in 10ml of methanol, stirring uniformly, dipping a proper amount of solution by using non-woven fabrics, drying to prepare a fluorescence sensitive film, and adhering the sensitive film on a quartz substrate to obtain the gas fluorescence sensitive element.
(2) A certain amount of nitrobenzene is put into a closed box, and nitrobenzene gases (0, 10, 20, 30, 50, 100, 150 mg/L) with different concentrations are prepared by heating nitrobenzene.
(3) The designed portable fluorescence detection module is placed in a sealed box, and the fluorescence intensity of nitrobenzene gas is measured, so that the concentration of pollutants can be obtained. Through experiments, the portable fluorescence detection module has good linearity when detecting 0-30mg/L nitrobenzene gas. The fluorescence detection limit of the p-nitrobenzene is 2.443mg/L.
FIG. 9 is a graph showing the change in fluorescence intensity (excitation wavelength: 282 nm) of the portable fluorescence detection module according to the present invention in example 2 when detecting nitrobenzene gases of different concentrations;
FIG. 10 shows the correspondence between fluorescence intensity and gas concentration (excitation wavelength: 282 nm) when the portable fluorescence detection module of the present invention detects nitrobenzene gas in example 2.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. 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 portable fluorescence detection module, comprising:
the light source module comprises an LED lamp and a TIR lens, wherein the TIR lens is used for collimating light rays emitted by the LED lamp;
the detection module comprises an excitation filter, a fluorescence sensitive element, a beam-converging lens and an emission filter which are sequentially arranged, wherein the excitation filter is used for receiving emergent light of the TIR lens and filtering the emergent light to generate a first wavelength light beam, the fluorescence sensitive element is used for contacting a sample to be detected and generating fluorescence under the excitation of the first wavelength light beam, the beam-converging lens is used for converging the fluorescence emitted by the fluorescence sensitive element, and the emission filter is used for receiving the emergent light of the beam-converging lens and filtering the emergent light to generate a second wavelength light beam;
and the signal processing module is used for performing signal processing on the second wavelength light beam.
2. The portable fluorescence detection module of claim 1, wherein the converging lens comprises a fresnel lens and a biconcave lens;
the Fresnel lens is arranged between the fluorescent sensing element and the biconcave lens.
3. The portable fluorescence detection module of claim 1, wherein the detection module further comprises a reaction chamber, wherein a fluorescence sensing element fixing groove is formed in the reaction chamber, and the fluorescence sensing element is detachably arranged in the fluorescence sensing element fixing groove.
4. The portable fluorescence detection module of claim 1, wherein the light source module further comprises a power source electrically connected to the LED lamp through a constant voltage circuit module;
the light source module further comprises a housing, the housing is provided with an inner cavity for accommodating the power supply, the constant voltage circuit module, the LED lamp and the TIR lens, and the housing is communicated with the detection module.
5. The portable fluorescence detection module according to claim 3, wherein the fluorescence sensing element is a gas fluorescence sensing element, the gas fluorescence sensing element comprises a quartz substrate and a fluorescence sensing film arranged on the surface of the quartz substrate, and the fluorescence sensing film is prepared by soaking and drying a film material by adopting a solution containing a fluorescence sensing material;
and the reaction cavity is provided with an air inlet and an air outlet.
6. The portable fluorescence detection module of claim 3, wherein the fluorescence sensor is a liquid fluorescence sensor comprising a cuvette and a solution of a fluorescence sensitive material disposed within the cuvette.
7. The portable fluorescence detection module of claim 3, further comprising a retaining clip, wherein the detection module is coupled to the signal processing module via the retaining clip.
8. A method of detecting a concentration of a contaminant using a portable fluorescence detection module according to any one of claims 1 to 7.
9. The method for detecting the concentration of pollutants according to claim 8, wherein the sample to be detected is a gas pollutant, the gas pollutant contains nitrobenzene, and the concentration of nitrobenzene in the gas pollutant is 0-30mg/L; or alternatively, the first and second heat exchangers may be,
the sample to be detected is nitrobenzene solution, and the concentration of nitrobenzene in the nitrobenzene solution is 0-100mg/L;
the composition of the fluorescence sensitive element comprises a fluorescence sensitive material, and the fluorescence sensitive material is MOFs.
10. The method of detecting a concentration of a contaminant according to claim 9, wherein said excitation filter has a center wavelength of 280nm and a bandwidth of 10nm;
the center wavelength of the emission filter is 545nm, and the bandwidth is 20nm.
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