CN113008856A - Oil composition detection device based on tunable fluorescence method - Google Patents
Oil composition detection device based on tunable fluorescence method Download PDFInfo
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- CN113008856A CN113008856A CN202110301450.4A CN202110301450A CN113008856A CN 113008856 A CN113008856 A CN 113008856A CN 202110301450 A CN202110301450 A CN 202110301450A CN 113008856 A CN113008856 A CN 113008856A
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- 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
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- 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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Abstract
本发明提供一种基于可调谐荧光法的油品成分检测装置，聚光透镜背离二向色分光镜的一侧面对油品，紫外光激发油品发射荧光，与紫外光相平行的荧光通过聚光透镜汇聚在焦点上；光纤准直器将荧光准直为平行光；光环形器的第一端口与光纤准直器通过光纤连接，光纤光栅与光环形器的第二端口连接，第三端口与光纤连接，光纤光栅将宽谱荧光过滤至特定波长的窄带荧光；荧光探测器的感光平面与第三端口通过光纤连接，将光信号转换为电信号。本发明提出的技术方案的有益效果是：通过对可调谐紫外光源和可调谐光纤光栅的光路设计，对待测油品成分的荧光响应进行波长扫描，获取油品成分的荧光响应曲线，与标准油品荧光响应曲线进行比对，获取油品成分含量信息。
The invention provides an oil component detection device based on a tunable fluorescence method. The side of the condenser lens facing away from the dichroic beam splitter faces the oil, and the oil is excited by ultraviolet light to emit fluorescence, and the fluorescence parallel to the ultraviolet light passes through the condenser. The optical lens converges on the focal point; the optical fiber collimator collimates the fluorescence into parallel light; the first port of the optical circulator is connected to the optical fiber collimator through an optical fiber, the fiber grating is connected to the second port of the optical circulator, and the third port Connected with the optical fiber, the fiber grating filters the broad-spectrum fluorescence to the narrow-band fluorescence of a specific wavelength; the photosensitive plane of the fluorescence detector is connected with the third port through the optical fiber, and the optical signal is converted into an electrical signal. The beneficial effects of the technical scheme proposed by the present invention are: through the optical path design of the tunable ultraviolet light source and the tunable fiber grating, the fluorescence response of the oil component to be measured is subjected to wavelength scanning, and the fluorescence response curve of the oil component is obtained, which is consistent with the standard oil component. The fluorescence response curves of the products were compared to obtain the content information of the oil products.
Description
Technical Field
The invention relates to the technical field of oil product component detection, in particular to an oil product component detection device based on a tunable fluorescence method.
Background
With the rapid development of national economy, the demand of people for energy is continuously increased, and oil resources are more and more frequently exploited, so that the threat of oil leakage to the environment is increased day by day. Petroleum and chemical products are inevitably leaked during production, transportation and storage, and the leaked petroleum or chemical products enter water bodies such as rivers, lakes, seas and the like to cause huge damage to the local ecological environment. Therefore, the real-time, rapid and effective monitoring and the identification of the components of the leaked substances for the leakage of the petroleum and the chemical products in the water body are key technical problems which are urgently needed to be solved in the field of environmental protection. At present, the technical development of revealing oil monitoring devices based on an ultraviolet fluorescence method is gradually mature, but the technical problem that real-time detection and effective identification are carried out on the components of the revealed oil is urgent to solve.
Common methods for detecting the components of the leaked oil products include two major types, namely physical and chemical analysis methods and spectral analysis methods. The chemical analysis method is relatively complex to operate, can be only carried out in a professional laboratory in most cases, has high requirements on professional quality of detection personnel, and has complex detection process, long time consumption and high detection cost although the detection result is accurate; the spectral analysis method is mainly based on methods such as an ultraviolet fluorescence method, an infrared spectrophotometry method and the like, has high sensitivity, is easy to operate instruments and equipment, and is widely applied at the present stage, but the method is mainly applied to online real-time alarm of leakage conditions and states of oil products in a water area, and is lack of component analysis of the oil products at present.
In the spectral analysis method, instrument equipment based on an ultraviolet fluorescence method is compact in structure and high in detection precision, when ultraviolet light is irradiated on an oil sample, electrons in molecules absorb energy and transit from a ground state to an excited state, the electrons can transit from the excited state to the ground state due to instability of the excited state, the energy is emitted from the transition process in a light emitting mode with the wavelength longer than that of the absorbed light, and the method is characterized in that the excited light is ultraviolet light, and the emitted light is blue-violet fluorescence with the wavelength longer and the frequency lower. The ultraviolet fluorescence method needs to emit ultraviolet light and detect incident excited fluorescence, if one device simultaneously completes the two functions, two light paths are generally needed to be separated, and the position of a detection target can only be the intersection point of the two light paths, so that the use of the detection device has certain limitation.
Disclosure of Invention
In view of the above, to solve the above problems, embodiments of the present invention provide an oil composition detection apparatus based on a tunable fluorescence method.
The embodiment of the invention provides an oil product component detection device based on a tunable fluorescence method, which comprises the following steps:
the tunable ultraviolet light source is used for generating ultraviolet light with different wavelengths to form incident light;
the dichroic spectroscope forms an angle of 45 degrees with the incident light, and the incident light irradiates the dichroic spectroscope to form reflected light;
the condensing lens is arranged perpendicular to the reflected light, one side of the condensing lens, which is far away from the dichroic spectroscope, faces the oil product, the reflected light vertically irradiates the condensing lens and then irradiates the oil product, the oil product is excited to emit fluorescence, the fluorescence is scattered in all directions from the oil surface, and the fluorescence parallel to the reflected light is converged on the focus of the condensing lens;
the entrance port of the optical fiber collimator is arranged at the focus and collimates the fluorescence into parallel light;
the device comprises an optical circulator and a tunable fiber grating, wherein a first port of the optical circulator is connected with an optical fiber collimator through an optical fiber, the adjustment of the fiber grating corresponds to the adjustment of an ultraviolet light source, the fiber grating is connected with a second port of the optical circulator, the fiber grating filters fluorescence incident from the first port, the filtered fluorescence is emitted from a third port of the optical circulator, and the third port is connected with the optical fiber; and the number of the first and second groups,
and the light sensing plane of the fluorescence detector is connected with the third port through an optical fiber so as to convert the optical signal into an electric signal.
Further, the ultraviolet light source device further comprises an ultraviolet light filter, and the ultraviolet light filter is arranged between the ultraviolet light source and the dichroic spectroscope.
Further, the optical fiber collimator also comprises a fluorescent filter, and the fluorescent filter is arranged between the dichroic spectroscope and the optical fiber collimator.
Further, the fluorescence detector is a photomultiplier tube.
Furthermore, the photomultiplier is connected with an amplifying circuit, and the amplifying circuit converts the weak current signal into a voltage signal and amplifies the voltage signal.
Furthermore, the photomultiplier is connected with a voltage conversion circuit, and the voltage is inverted to obtain a positive voltage signal.
Furthermore, the photomultiplier is connected with a filter circuit, and the inverted voltage signal is filtered by the filter circuit to remove high-frequency noise.
Furthermore, the photomultiplier is connected with an analog-to-digital conversion circuit, and digital signals are obtained through analog-to-digital conversion.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: because the wavelengths of the excitation ultraviolet light and the emission fluorescence light of different components of the leaked oil product correspond to each other pairwise, the components of the leaked oil product can be measured by adopting a fluorescent oil product component analysis algorithm through the corresponding relation. The coaxial light path can make the fluorescence detector absorb fluorescence energy as far as possible while simplifying the light path structure, the distance between the target to be detected and the device can be changed within a certain range, the application scene is more flexible and changeable, the device user can complete the detection of the target to be detected quickly, the operation difficulty and complexity of the device are reduced, and the detection precision is improved simultaneously. The method comprises the steps of designing a transmitting-receiving coaxial light path by adopting optical devices such as a tunable ultraviolet light source and a tunable fiber grating, carrying out accurate adaptation on the wavelength of the tunable device, carrying out wavelength scanning on the fluorescence response of the oil product component to be detected, obtaining the fluorescence response curve of the oil product component, and comparing the fluorescence response curve with the fluorescence response curve of a standard oil product by an oil product component analysis algorithm to obtain the oil product component content information.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of an oil product component detection device based on a tunable fluorescence method provided by the invention.
In the figure: the device comprises a photomultiplier tube 1, a second optical fiber 2.1, a first optical fiber 2.2, an optical circulator 3, an optical fiber grating 4, an optical fiber collimator 5, a fluorescent filter 6, a dichroic spectroscope 7, an ultraviolet filter 8, an ultraviolet light source 9 and a condensing lens 10.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, an embodiment of the present invention provides an oil product component detection apparatus based on a tunable fluorescence method, including an ultraviolet light source 9, a dichroic beam splitter 7, a condenser lens 10, a fiber collimator 5, an optical circulator 3, a fiber grating 4, and a fluorescence detector.
The tunable ultraviolet light source 9 generates ultraviolet light with different wavelengths to form incident light, the dichroic spectroscope 7 forms an angle of 45 degrees with the incident light, the dichroic spectroscope 7 shows a reflection characteristic to ultraviolet waveband light beams and shows a transmission characteristic to fluorescence waveband light beams, the reflectivity of the ultraviolet light and the transmissivity of fluorescence are close to 100%, and the incident light irradiates the dichroic spectroscope 7 at 45 degrees and is reflected at 45 degrees to form reflected light. The ultraviolet filter 8 is arranged between the ultraviolet light source 9 and the dichroic spectroscope 7, the ultraviolet filter 8 is arranged perpendicular to incident light, and the incident light can filter stray light except for specific wavelength after vertically passing through the ultraviolet filter 8.
For different oil products, the excitation ultraviolet light with different wavelengths can obtain the emission fluorescence with different wavelengths, and in order to detect various hydrocarbon substances in one oil sample, ultraviolet light with multiple wavelengths is needed to excite the sample and detect the emission fluorescence with specific wavelength under the excitation light. The ultraviolet light source 9 is a tunable ultraviolet light source to generate ultraviolet light with different wavelengths, and the ultraviolet light irradiates the oil product to excite the oil product to generate fluorescence with corresponding wavelengths. The tunable ultraviolet light source 9 may employ a plurality of ultraviolet LED arrays with different wavelengths, and in this embodiment, the tunable ultraviolet light source 9 employs an ultraviolet laser with adjustable wavelength, and controls a resonant cavity of the tunable ultraviolet laser through an external driving circuit to drive the ultraviolet laser to emit ultraviolet light with a specific wavelength.
The condensing lens 10 is arranged perpendicular to the reflected light, one side of the condensing lens 10, which is far away from the dichroic beam splitter 7, faces to the oil product, the reflected light vertically irradiates the condensing lens 10 and then irradiates to the oil product, specific molecules in the oil product are excited to generate a fluorescent reaction, fluorescent light with specific wavelength is emitted, the fluorescent light is scattered in all directions from the oil surface, and the fluorescent light parallel to the reflected light vertically enters the condensing lens 10 and is converged on the focus of the condensing lens 10. When the fluorescence transmitted through the condensing lens 10 passes through the dichroic beam splitter 7, since the transmittance of the dichroic beam splitter 7 for the fluorescence is close to 100%, the fluorescence can be transmitted through the dichroic beam splitter 7 substantially without loss.
The entrance port of the optical fiber collimator 5 is arranged at the focal point, and the fluorescence is collimated into parallel light, so that the fluorescence is gathered. The fluorescence filter 6 is arranged between the dichroic beam splitter 7 and the fiber collimator 5, and can filter out most of natural stray light in non-fluorescence bands and only leave fluorescence with narrow spectrum.
The first port of the optical circulator 3 is connected with the optical fiber collimator 5 through a first optical fiber 2.2, the optical fiber grating 4 is connected with the second port of the optical circulator 3, the optical fiber grating 4 filters fluorescence incident from the first port, wide-spectrum fluorescence is filtered into narrow-band fluorescence, the filtered fluorescence is emitted from the third port of the optical circulator 3, and the third port is connected with a second optical fiber 2.1.
The fiber grating 4 is a diffraction grating formed by periodically modulating the refractive index of the fiber core in the axial direction by a certain method, and is a passive filter device. In this embodiment, the fiber grating 4 is a tunable fiber grating, the adjustment of the fiber grating corresponds to the adjustment of the ultraviolet light source, the center wavelength of the fiber grating 4 is changed by applying different pressures to the fiber grating 4, stretching and compressing the length of the fiber grating 4, and the like, and the reflection wavelength of the fiber grating 4 is controlled, thereby playing a role in filtering. The wide spectrum fluorescence enters from the first port of the optical circulator 3 and exits from the second port to the fiber grating 4, and the fiber grating 4 converts the wide spectrum fluorescenceThe fluorescence is filtered to narrow-band fluorescence of a specific wavelength, which is reflected back from the second port and can exit the third port almost without loss and enter the second optical fiber 2.1. The ultraviolet light source and the fiber bragg grating are tunable, the peak value excitation ultraviolet wavelength and the peak value emission fluorescence wavelength of the oil product are in one-to-one correspondence, the ultraviolet light source and the fiber bragg grating can be adjusted according to the oil product to be detected, please refer to fig. 1, and lambda is obtained by adjusting the ultraviolet light source and the fiber bragg gratingk(k＝1,…,n)Is a tuned ultraviolet wavelength, λ'k(k＝1,…,n)Is the corresponding fluorescence wavelength, and can be analyzed and set through a fluorescent oil composition analysis algorithm.
The light sensing plane of the fluorescence detector is opposite to the second optical fiber 2.1, and the narrow-band fluorescence entering the second optical fiber 2.1 is emitted from the tail end of the second optical fiber 2.1 and finally vertically emitted to the light sensing plane of the fluorescence detector, so that an optical signal is converted into an electric signal. In this embodiment, the fluorescence detector is a photomultiplier tube 1. The photomultiplier 1 can convert a weak optical signal into an electric signal, the spectral response range of the photomultiplier comprises a wavelength range of 250nm-950nm, the peak response wavelength is in a blue-violet fluorescence band, and the detection efficiency of the peak wavelength is above 30%.
The photomultiplier 1 is composed of an avalanche diode array working in a Geiger mode, and when the photomultiplier normally works, the reverse working voltage of the photomultiplier is larger than the directional breakdown voltage of the avalanche diode, and when a single photon is incident to a light receiving area of the avalanche diode, avalanche pulse current can be generated. The current generated by the weak light signal on the photomultiplier tube 1 is very small, the photomultiplier tube 1 is connected with an amplifying circuit, and the weak current signal is converted into a voltage signal and amplified through the amplifying circuit. Because the avalanche diode array in the photomultiplier 1 needs reverse bias, the voltage signal obtained by the amplifying circuit is a negative voltage signal, the photomultiplier 1 is connected with a voltage conversion circuit, and the voltage is inverted by the voltage conversion circuit to obtain a positive voltage signal. The photomultiplier 1 is connected with a filter circuit, the photomultiplier 1 is connected with an analog-to-digital conversion circuit, the inverted voltage signal enters the analog-to-digital conversion circuit after high-frequency noise is filtered by the filter circuit, digital signals are obtained through analog-to-digital conversion, and the digital signals are analyzed through a fluorescent oil product analysis algorithm to determine whether the detected leaked oil product contains certain aromatic hydrocarbons and the components of certain substances in the oil product.
The outgoing light path and the incoming light path of a general optical device are structurally separated, a detection target can only be located at the intersection point of the two light paths, the detection range is limited, and the detection precision is reduced due to the fact that the oil surface light incoming surface and the oil surface light outgoing surface are not on the same plane. The technical scheme provided by the invention is that two light paths of an ultraviolet light emergent light path in front of a dichroic spectroscope 7 and a fluorescence incident light path in front of the dichroic spectroscope 7 are independent from each other, the ultraviolet light emergent light path in back of the dichroic spectroscope 7 and the fluorescence incident light path in front of the dichroic spectroscope 7 are multiplexed to a coaxial light path due to the reflection of the dichroic spectroscope 7 to ultraviolet light and the transmission of fluorescence, the coaxial light path enables a detection target to be positioned at any point of the coaxial light path outside equipment, the detection target is excited to fluorescence by the ultraviolet light, the fluorescence is focused on an optical collimator 5 at the focus of the detection target through a condensing lens 10 through the coaxial light path, the fluorescence is filtered through an optical circulator 3 and an optical fiber grating 4 and enters the light receiving surface of a photomultiplier 1, and because the wavelengths of the excited ultraviolet light and the emitted fluorescence of different components of leaked oil are, by adopting the corresponding relation, the determination of the leaked oil components can be realized by adopting a fluorescent oil component analysis algorithm.
The coaxial light path can make the fluorescence detector absorb fluorescence energy as far as possible while simplifying the light path structure, the distance between the target to be detected and the device can be changed within a certain range, the application scene is more flexible and changeable, the device user can complete the detection of the target to be detected quickly, the operation difficulty and complexity of the device are reduced, and the detection precision is improved simultaneously.
The ultraviolet light source 9 has tunable property, can emit ultraviolet light with various wavelengths in an ultraviolet band, selects excitation ultraviolet light with specific wavelength according to the characteristics of different leaked oil components to be detected, excites the oil to generate emission fluorescence with corresponding wavelength, and thus accurate fluorescence spectrum detection data is obtained.
The fluorescence receiving end adopts the fiber grating 4 to complete the filtering of fluorescence with different wavelengths, the wavelength of reflected light of the fiber grating 4 can be accurately set by adjusting the stress, the length and the like of the fiber grating 4, the fluorescence with wider spectrum only reflects narrow-band fluorescence near a certain central wavelength after entering the fiber grating 4, and the tunable narrow-band filtering effect of the fiber grating 4 is realized.
The fluorescence with specific wavelength is coupled into the sensitive light receiving surface of the photomultiplier 1 through the optical circulator 3, thereby realizing the real-time detection and effective identification of the components of the leaked oil product. The photomultiplier 1 is used as a photoelectric sensor, weak fluorescence signals can be converted into electric signals through the single photon detection capability of the photomultiplier 1, and the electric signals are processed through a subsequent circuit to obtain fluorescence spectrum detection data. The method comprises the steps of designing a transmitting-receiving coaxial light path by adopting optical devices such as a tunable ultraviolet light source and a tunable fiber grating, carrying out accurate adaptation on the wavelength of the tunable device, carrying out wavelength scanning on the fluorescence response of the oil product component to be detected, obtaining the fluorescence response curve of the oil product component, and comparing the fluorescence response curve with the fluorescence response curve of a standard oil product by an oil product component analysis algorithm to obtain the oil product component content information.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
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