CN112362588A - VOC gas detection system and detection method - Google Patents
VOC gas detection system and detection method Download PDFInfo
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- CN112362588A CN112362588A CN202011169169.1A CN202011169169A CN112362588A CN 112362588 A CN112362588 A CN 112362588A CN 202011169169 A CN202011169169 A CN 202011169169A CN 112362588 A CN112362588 A CN 112362588A
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
Abstract
A VOC gas detection system and a detection method. The detection system comprises: a light source; the gas detection device comprises a closed container and an optical fiber, wherein the closed container is provided with a gas inlet and a gas outlet; the optical fiber is provided with an evanescent wave optical fiber structure so that light entering the optical fiber structure can be transmitted out in an evanescent field mode, a region with the evanescent wave optical fiber structure on the optical fiber is fixed in the closed container and is loaded with a metal oxide semiconductor material, two ends of the optical fiber extend out of the closed container, and one end of the optical fiber is connected with the light source; the signal receiving device is connected with one end of the optical fiber far away from the light source and is arranged to receive an output power signal from the optical fiber; and the data processing device is connected with the signal receiving device. The VOC gas detection system and the detection method can realize on-site, rapid, efficient and continuous detection of VOC, and the lower limit of detectable concentration is low.
Description
Technical Field
The present application relates to, but is not limited to, the field of VOC detection, and more particularly, to a VOC gas detection system and method.
Background
VOC (volatile organic compounds) refers to volatile organic compounds with low boiling points such as formaldehyde, xylene and acetone, and the long-term contact and inhalation of the volatile organic compounds by a human body can cause adverse effects on the health of the human body, so that the realization of efficient and rapid detection of the VOC is very important in working and living environments. The existing VOC detection methods mainly comprise a gas chromatography method, a chemical conversion method and the like, but the methods have the defects of difficult field detection, long detection period, high detectable concentration lower limit and the like. Therefore, there is a need for a method for detecting VOCs in situ, rapidly, efficiently and continuously.
Disclosure of Invention
The application provides a VOC gas detection system and detection method, and this VOC gas detection system and detection method can realize on the spot, quick, high-efficient and continuous detection to VOC, and detectable concentration lower limit is low moreover, and detection system simple structure.
The application provides a gaseous detecting system of VOC, gaseous detecting system of VOC includes:
a light source;
a gas detection device comprising a closed container and an optical fiber; the closed container is provided with an air inlet and an air outlet; the optical fiber is provided with an evanescent wave optical fiber structure, the evanescent wave optical fiber structure can enable light entering the optical fiber structure to be transmitted out in an evanescent field mode, an area with the evanescent wave optical fiber structure on the optical fiber is fixed in the closed container, metal oxide semiconductor materials are loaded on the area, two ends of the optical fiber extend out of the closed container, and one end of the optical fiber is connected with the light source;
a signal receiving device connected to an end of the optical fiber remote from the light source and arranged to receive an output power signal from the optical fiber; and
and the data processing device is connected with the signal receiving device.
In an embodiment of the present application, the light source may be an ultraviolet light source.
In an embodiment of the present application, the light source may be a laser capable of emitting ultraviolet light, and an output jumper of the laser is coupled to one end of the optical fiber in a fusion manner.
In embodiments of the present application, the optical fiber may be a tapered fiber or a D-fiber.
In embodiments of the present application, the tapered optical fiber may have a beam waist diameter of 5-20 μm, and when the optical fiber is a tapered optical fiber, the metal oxide semiconductor material is loaded on the tapered surface of the tapered optical fiber.
In the embodiment of the application, the cladding thickness of the polished region of the D-type optical fiber can be 0-5 microns, and when the optical fiber is the D-type optical fiber, the metal oxide semiconductor material is loaded on the surface of the polished region of the D-type optical fiber.
In an embodiment of the present application, the metal oxide semiconductor material may be TiO2Or ZnO.
In an embodiment of the present application, the signal receiving device may be a power probe.
The application also provides a VOC gas detection method, which is carried out by adopting the VOC gas detection system, and comprises the following steps:
processing the optical fiber to form an evanescent wave optical fiber structure, so that the light entering the evanescent wave optical fiber structure can be transmitted out in the form of an evanescent field;
loading a metal oxide semiconductor material on the surface of the area with the evanescent wave optical fiber structure on the processed optical fiber;
fixing an area with an evanescent wave optical fiber structure on an optical fiber loaded with a metal oxide semiconductor material in a closed container, respectively connecting two ends of the optical fiber with a light source and a signal receiving device, and connecting the signal receiving device with a data processing device;
and starting a light source, a signal receiving device and a data processing device, respectively introducing gas to be detected and pure air from an air inlet of the closed container under the same laser input power, and judging whether the gas to be detected contains VOC gas and the content of the VOC gas according to a processing result of the data processing device.
In an embodiment of the application, the manner of loading the metal oxide semiconductor material on the surface of the region having the evanescent wave optical fiber structure on the processed optical fiber may be a hydrothermal method or an atomic layer deposition method.
In an embodiment of the application, the determining whether the gas to be detected contains the VOC gas and the content of the VOC gas according to the processing result of the data processing device may include:
calculating response signals of the output power of the optical fiber: s ═ P/P0(ii) a Wherein S represents a response signal of the output power of the optical fiber; p and P0Respectively indicating the stable output power of the optical fiber detected by the probe when the gas to be detected and the pure air are respectively introduced under the same laser input power;
if the response signal S is greater than 1 or S <1, indicating that the gas to be detected contains VOC gas; if S is approximately equal to 1, indicating that the gas to be detected does not contain VOC gas;
and when the gas to be detected contains the VOC gas, substituting the response signal S into the relational equation according to the relational equation between the content of the VOC gas and the response signal obtained in advance to obtain the concentration of the VOC gas in the gas to be detected.
In an embodiment of the present application, after obtaining the response signal S and before calculating the VOC gas content in the gas to be detected, the VOC gas detection method may further include:
and testing in advance to obtain response signals under the action of the VOC gas samples with different concentrations, and then fitting to obtain a relational equation between the VOC gas concentrations and the VOC gas concentrations.
In the embodiments of the present application, the fitting may be performed by interpolation or least squares.
In the embodiment of the present application, the software used for the fitting may be Excel or SPSS.
The VOC gas detection system and the detection method have the following advantages:
(1) the output power of the optical fiber is obviously influenced by the refractive index of the metal oxide semiconductor material loaded on the surface, so that the detection sensitivity is ensured; (2) the surface area of the optical fiber surface loaded with the metal oxide semiconductor material is small, so that the optical power density is high, the density of generated carriers is high, and the response speed is high; (3) the optical fiber is used as a light source, a carrier of the metal oxide semiconductor material and a transmission medium of a signal, and light generated by the light source is a light source which acts with the metal oxide semiconductor material on the surface of the optical fiber and is a source of a light signal for detection, so that the complexity of a detection system is greatly reduced;
when ultraviolet band light is used as a light source, the following advantages are also provided: (4) the detection is not required to be carried out at high temperature, and the practicability of the detection technology can be improved.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. Other advantages of the present application may be realized and attained by the instrumentalities and combinations particularly pointed out in the specification and the drawings.
Drawings
The accompanying drawings are included to provide an understanding of the present disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the examples serve to explain the principles of the disclosure and not to limit the disclosure.
Fig. 1 is a schematic structural view of a VOC gas detection system according to an embodiment of the present application;
fig. 2 is a partially enlarged view of a VOC gas detection system employing tapered optical fibers according to an embodiment of the present application.
Detailed Description
To make the objects, technical solutions and advantages of the present application more apparent, embodiments of the present application will be described in detail below with reference to the accompanying drawings. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
Metal oxide semiconductor material (TiO)2ZnO, etc.) has strong adsorption effect on VOC gas, and can effectively adsorb VOC in an external medium to the surface of the material and diffuse and permeate into the interior of the material. Some volatile organic compounds can react with the metal oxide semiconductor material and be consumedElectrons generated by the metal oxide semiconductor material or electrons injected into the metal oxide semiconductor material influence the properties of the metal oxide semiconductor material such as conductivity, refractive index and the like, a detection signal is generated, and the purpose of detection is achieved. However, the VOC detection using the metal oxide semiconductor material still has the following problems: the lower detection limit is dozens to hundreds of ppm magnitude, and the sensitivity is still to be improved; secondly, in order to enhance the adsorption of the metal oxide semiconductor material to the VOC and increase the electron concentration inside the material, the detection needs to be performed under high temperature conditions, which results in an increase in the number of detection additional devices and a decrease in the operability of the detection system in different environments.
The embodiment of the application provides a VOC gas detection system, as shown in FIG. 1, this VOC gas detection system includes:
a light source 1;
a gas detection device including a closed container 2 and an optical fiber 3; the closed container is provided with an air inlet 21 and an air outlet 22, the air inlet 21 is respectively connected with the conveying pipes of the gas to be detected 100 and the pure air 200 through a first valve 23 and a second valve 24, and the air outlet 22 controls air exhaust through a third valve 25; the optical fiber 3 is provided with an evanescent wave optical fiber structure, the evanescent wave optical fiber structure can enable light entering the optical fiber structure to be transmitted out in an evanescent field mode, an area with the evanescent wave optical fiber structure on the optical fiber is fixed in the closed container 2 and is loaded with a metal oxide semiconductor material, two ends of the optical fiber 3 extend out of the closed container 2, and one end of the optical fiber is connected with the light source 1;
a signal receiving device 4, wherein the signal receiving device 4 is connected with one end of the optical fiber 3 far away from the light source and is arranged to be capable of receiving an output power signal from the optical fiber 3; and
and the data processing device 5 is connected with the signal receiving device 4 through the data processing device 5.
The VOC gas detection system adopts the technology of loading the metal oxide semiconductor material on the optical fiber and combining the evanescent field, and when the VOC gas and the metal oxide semiconductor material act, the VOC gas can be obviously influencedThe concentration and the distribution of electrons in the metal oxide semiconductor material and on the surface of the metal oxide semiconductor material can change the refractive index of the metal oxide semiconductor material, and meanwhile, due to the action of an evanescent field of the optical fiber, the optical fiber is very sensitive to the change of the refractive index of the metal oxide semiconductor material loaded on the surface of the optical fiber, so that the side transmittance value, namely loss, of the optical fiber is obviously influenced, and the output power value of the optical fiber is further changed. And a signal receiving device and a data processing device are adopted to monitor the output power of the optical fiber in real time. The response signal can be calculated using the following formula: s ═ P/P0Wherein P and P0The stable output power of the optical fiber detected by the probe when the gas to be detected and the pure air are respectively introduced under the same laser input power can reflect the influence of the gas to be detected on the refractive index of the metal oxide semiconductor material on the surface of the optical fiber.
In the embodiment of the present application, the light source 1 may be an ultraviolet light source.
When an ultraviolet light source is adopted, under the action of ultraviolet waveband light, electrons in a valence band of the metal oxide semiconductor material can jump into a conduction band, so that free electrons are formed in the conduction band, holes are formed in the valence band, a large number of electrons and holes can be generated, the detection process can be carried out at normal temperature, the response speed can be increased, and the practicability and the applicability of the detection technology can be effectively enhanced.
In the embodiment of the present application, the light source 1 may be a laser capable of emitting ultraviolet light, and an output jumper 11 of the laser may be coupled to one end of the optical fiber 3 in a fusion manner.
In the embodiment of the present application, the optical fiber 3 may be a tapered optical fiber or a D-type optical fiber.
In an embodiment of the present application, a diameter of a beam waist region of the tapered optical fiber may be 5 to 20 micrometers, and when the optical fiber is a tapered optical fiber, a region having an evanescent wave optical fiber structure on the optical fiber is a tapered region 31 of the tapered optical fiber, that is, the metal oxide semiconductor material is loaded on a surface of the tapered region 31 of the tapered optical fiber.
In the embodiment of the present application, the thickness of the cladding layer in the polished section of the D-type optical fiber may be 0 to 5 micrometers (at this time, the thickness of the cladding layer removed by polishing may be 50 to 60 micrometers), and when the optical fiber is a D-type optical fiber, the region having the evanescent wave optical fiber structure on the optical fiber is the polished section of the D-type optical fiber, that is, the metal oxide semiconductor material is loaded on the polished section surface of the D-type optical fiber.
In an embodiment of the present application, the metal oxide semiconductor material may be TiO2Or ZnO.
In an embodiment of the present application, the signal receiving device may be a power probe.
The embodiment of the present application further provides a VOC gas detection method, which is performed by using the above-mentioned VOC gas detection system, and includes:
processing the optical fiber to form an evanescent wave optical fiber structure, so that the light entering the evanescent wave optical fiber structure can be transmitted out in the form of an evanescent field;
loading a metal oxide semiconductor material on the surface of the area with the evanescent wave optical fiber structure on the processed optical fiber;
fixing an area with an evanescent wave optical fiber structure on an optical fiber loaded with a metal oxide semiconductor material in a closed container, respectively connecting two ends of the optical fiber with a light source and a signal receiving device, and connecting the signal receiving device with a data processing device;
and starting a light source, a signal receiving device and a data processing device, respectively introducing gas to be detected and pure air from an air inlet of the closed container under the same laser input power, and judging whether the gas to be detected contains VOC gas and the content of the VOC gas according to a processing result of the data processing device.
In an embodiment of the application, the manner of loading the metal oxide semiconductor material on the surface of the region having the evanescent wave optical fiber structure on the processed optical fiber may be a hydrothermal method or an atomic layer deposition method.
In an embodiment of the application, the determining whether the gas to be detected contains the VOC gas and the content of the VOC gas according to the processing result of the data processing device may include:
if the response signal S is greater than 1 or S <1, indicating that the gas to be detected contains VOC gas; if the response signal S is approximately equal to 1, indicating that the gas to be detected does not contain VOC gas;
and when the gas to be detected contains the VOC gas, substituting the response signal S into the relational equation according to the relational equation between the content of the VOC gas and the response signal obtained in advance to obtain the concentration of the VOC gas in the gas to be detected.
In an embodiment of the present application, after obtaining the response signal S and before calculating the VOC gas content in the gas to be detected, the VOC gas detection method may further include:
and testing in advance to obtain response signals under the action of the VOC gas samples with different concentrations, and then fitting to obtain a relational equation between the VOC gas concentrations and the VOC gas concentrations.
In the embodiments of the present application, the fitting may be performed by interpolation or least squares.
In the embodiment of the present application, the software used for the fitting may be Excel or SPSS.
When the metal oxide semiconductor material is TiO2In the meantime, the method for detecting the VOC gas is suitable for detecting the VOC gas containing formaldehyde, chloroform and the like; when the metal oxide semiconductor material is ZnO, the VOC gas detection system is suitable for detecting VOC gas containing ethanol and the like.
Example 1
(1) Making optical fiber into tapered optical fiber
Manufacturing the tapered optical fiber: one end of a section of optical fiber is in fusion-splicing coupling with an output jumper of a laser, and the other end of the optical fiber is cut flatly by a cutter and then placed in a power probe (namely the probe connected with a power meter). Removing a small section of coating layer by using a core stripping clamp, placing the area with the coating layer removed above an oxyhydrogen flame gun head, fixing two ends of the area with the coating layer removed on a clamp of a tapering machine, drawing the optical fiber towards two sides at a constant speed by using a stepping motor, recording the numerical change displayed by a power meter in the drawing process, and taking the ratio of the difference between the initial power value displayed before drawing and the power value after tapering and the initial power value as the loss of the tapered optical fiber, namely the side light transmittance. The selection of different stretching lengths can result in tapered fibers with different lateral transmittances. When the lateral light transmittance is not 0, the light in the optical fiber is shown to be transmitted out of the optical fiber in the form of an evanescent field.
(2) Growing metal oxide semiconductor material TiO in the taper zone of the tapered optical fiber by a hydrothermal method2
The nano material has smaller size and larger specific surface area, so that the action area of the metal oxide semiconductor material and the gas to be detected can be effectively enlarged, and the detection sensitivity is improved. This example shows the growth of TiO on tapered fibers by hydrothermal method2A nanorod array, comprising:
1) the tapered optical fiber penetrates through the capillary tube and is fixed on a clamp, the tapered area of the tapered optical fiber is suspended to enable the area to be in full contact with reaction liquid, the tapered optical fiber is knotted to be placed in a reaction kettle, and the optical fiber is washed by alcohol;
2) dissolving tetrabutyl titanate in isopropanol to prepare a seed solution with the concentration of 75mM, putting the dried and fixed tapered optical fiber into the seed solution for soaking for 3 minutes, taking the tapered optical fiber out of the seed solution, and preserving the temperature of the tapered optical fiber in a muffle furnace at 450 ℃ for 1 hour;
3) preparing a hydrothermal reaction solution, wherein the specific components are 40mL of concentrated hydrochloric acid (the concentration is 36-38 wt.%) +40mL of ultrapure water +1.6mL of tetrabutyl titanate, putting the tapered optical fiber subjected to the heat treatment in the step 2) into a reaction kettle, adding the reaction solution, preserving the heat at 150 ℃ for 7 hours, taking out the reaction solution, and washing the reaction solution with water;
4) putting the tapered optical fiber obtained in the step 3) into a muffle furnace, preserving the heat for 2.5 hours at 500 ℃, and cooling to obtain the tapered zone with TiO grown thereon2A tapered optical fiber of a nanorod array.
(3) Collection of detection signals
Growing TiO on the surface of the cone area prepared in the step (2)2One end of the nanorod array tapered optical fiber is welded with an output jumper of a laser capable of providing single-wavelength ultraviolet light, so that the single-wavelength ultraviolet light is enabled to be weldedCan be transmitted into the tapered optical fiber; the tapered area of the tapered optical fiber is placed in a closed container of the gas detection device, and the two ends of the closed container are sealed and fixed by glue to keep the air tightness. The gas inlet of the closed container selectively feeds gas to be detected or pure air through the first valve or the second valve; the power probe connected to one end of the tapered fiber was connected to a data processing device (a computer in this embodiment). When in detection, the second valve and the third valve are opened first, the first valve is closed, pure air is introduced to ensure that the whole closed container is filled with pure air, then the valves are all closed, the laser light source is turned on, and the stable output power P of the output end of the tapered optical fiber is recorded0(ii) a Then opening the first valve and the third valve, introducing a gas sample to be detected, closing the first valve after ensuring that the closed container is filled with the gas sample to be detected, and recording the stable output power P, P and P of the output end of the tapered optical fiber at the moment0The ratio is the detection signal indicator.
Although the embodiments disclosed in the present application are described above, the descriptions are only for the convenience of understanding the present application, and are not intended to limit the present application. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the disclosure as defined by the appended claims.
Claims (10)
1. A VOC gas detection system, comprising:
a light source;
a gas detection device comprising a closed container and an optical fiber; the closed container is provided with an air inlet and an air outlet; the optical fiber is provided with an evanescent wave optical fiber structure, the evanescent wave optical fiber structure can enable light entering the optical fiber structure to be transmitted out in an evanescent field mode, an area with the evanescent wave optical fiber structure on the optical fiber is fixed in the closed container, metal oxide semiconductor materials are loaded on the area, two ends of the optical fiber extend out of the closed container, and one end of the optical fiber is connected with the light source;
a signal receiving device connected to an end of the optical fiber remote from the light source and arranged to receive an output power signal from the optical fiber; and
and the data processing device is connected with the signal receiving device.
2. A VOC gas detection system according to claim 1 wherein the light source is an ultraviolet light source.
3. The VOC gas detection system of claim 2 wherein the light source is a laser capable of emitting ultraviolet light, and an output jumper of the laser is fusion spliced to one end of the optical fiber.
4. A VOC gas detection system according to any of claims 1-3 wherein the optical fiber is a tapered or D-fiber;
optionally, the diameter of the beam waist region of the tapered optical fiber is 5-20 microns, and when the optical fiber is the tapered optical fiber, the metal oxide semiconductor material is loaded on the surface of the tapered region of the tapered optical fiber;
optionally, the cladding thickness of the polished region of the D-type optical fiber is 0-5 microns, and when the optical fiber is the D-type optical fiber, the metal oxide semiconductor material is loaded on the surface of the polished region of the D-type optical fiber.
5. A VOC gas detection system according to any of claims 1-3 wherein the metal oxide semiconductor material is TiO2Or ZnO.
6. A VOC gas detection system according to any of claims 1-3 wherein the signal receiving means is a power probe.
7. A VOC gas detection method, wherein the VOC gas detection method is performed using the VOC gas detection system according to any one of claims 1-6, comprising:
processing the optical fiber to form an evanescent wave optical fiber structure, so that the light entering the evanescent wave optical fiber structure can be transmitted out in the form of an evanescent field;
loading a metal oxide semiconductor material on the surface of the area with the evanescent wave optical fiber structure on the processed optical fiber;
fixing an area with an evanescent wave optical fiber structure on an optical fiber loaded with a metal oxide semiconductor material in a closed container, respectively connecting two ends of the optical fiber with a light source and a signal receiving device, and connecting the signal receiving device with a data processing device;
and starting a light source, a signal receiving device and a data processing device, respectively introducing gas to be detected and pure air from an air inlet of the closed container under the same laser input power, and judging whether the gas to be detected contains VOC gas and the content of the VOC gas according to a processing result of the data processing device.
8. The VOC gas detection method of claim 7, wherein the loading of the metal oxide semiconductor material on the surface of the area with the evanescent wave optical fiber structure on the treated optical fiber is performed by a hydrothermal method or an atomic layer deposition method.
9. The VOC gas detection method according to claim 7 or 8, wherein the determining whether the gas to be detected contains VOC gas and the content of VOC gas from the processing result of the data processing device comprises:
calculating response signals of the output power of the optical fiber: s ═ P/P0(ii) a Wherein S represents a response signal of the output power of the optical fiber; p and P0Respectively indicating the stable output power of the optical fiber detected by the probe when the gas to be detected and the pure air are respectively introduced under the same laser input power;
if the response signal S is greater than 1 or S <1, indicating that the gas to be detected contains VOC gas; if S is approximately equal to 1, indicating that the gas to be detected does not contain VOC gas;
and when the gas to be detected contains the VOC gas, substituting the response signal S into the relational equation according to the relational equation between the content of the VOC gas and the response signal obtained in advance to obtain the concentration of the VOC gas in the gas to be detected.
10. The VOC gas detection method according to claim 9, further comprising, after obtaining the response signal S and before calculating the VOC gas content in the gas to be detected:
testing in advance to obtain response signals under the action of VOC gas samples with different concentrations, and then fitting to obtain a relation equation between the VOC gas concentrations and the VOC gas concentrations;
optionally, the fitting is performed by interpolation or least squares;
optionally, the fitting is performed using software such as Excel or SPSS.
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