CN114235701B - Real-time self-calibration trace gas concentration detection device - Google Patents
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- 238000007405 data analysis Methods 0.000 claims abstract description 6
- 238000013480 data collection Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 67
- 230000001427 coherent effect Effects 0.000 claims description 9
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- 238000000180 cavity ring-down spectroscopy Methods 0.000 description 3
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention relates to the technical field of gas detection, and discloses a detection device capable of performing real-time self-calibration on detection results to trace gas concentration. The trace gas concentration detection device provided by the invention comprises a DFB laser, a beam splitting sampling plate, a laser wavelength monitoring module, a laser control circuit module, a neutral beam splitter, a collimator, a mode matching lens group, a real-time self-calibration ring-down cavity, a focusing lens, a detector and a data collection and analysis processing circuit module. The open ring-down cavity gas detection parameters are calibrated in real time by utilizing the closed ring-down cavity detection parameters, so that the problems that the detection process is complicated, the cavity parameters need to be re-measured when a light source is replaced for detecting another gas, and the cavity ring-down parameters cannot be updated in real time according to the change of the detection environment in the existing cavity ring-down spectrum gas detection technology are solved.
Description
Technical Field
The invention relates to the technical field of gas detection, in particular to a trace gas concentration detection device capable of performing self-calibration in real time.
Background
The method has wide application requirements and higher detection precision requirements for the detection of the gas concentration in the fields of industrial production, social safety, resource exploration, medical diagnosis, environmental monitoring and the like. The detection of a gas concentration that is extremely low in concentration compared to the background gas is trace gas detection. The detection method of trace gas concentration has been developed from the initial chemical reaction measurement technology to the laser absorption spectrum detection technology with highest precision at present. In the laser absorption spectrum detection technology, along with the development of the laser technology and the improvement of the device performance, a device for gas detection is also continuously upgraded in the aspects of precision, sensitivity and the like.
At present, conventional methods for gas detection mainly include electrochemical methods, mass spectrometry, gas chromatography, thermocatalytic methods, and the like. Although the traditional methods all realize the measurement of the gas to different degrees, the traditional methods all sample the gas manually, the instrument is expensive and the operation is complex, and the traditional methods are commonly used for measuring the gas in a laboratory, so that the requirement of people on quick qualitative detection of the gas is hardly met. The laser spectrum technology mainly utilizes the interaction of substances and light to achieve the aim of gas discrimination and detection. The laser spectrum gas detection technology is used for trace gas detection, has the characteristics of high measurement accuracy, high detection speed, capability of realizing real-time online monitoring and the like, and is divided into a direct detection technology and an indirect detection technology according to different detection principles. The direct detection technique is realized by utilizing the absorption characteristics of a substance to light. The indirect detection technology refers to that a substance to be detected is excited by laser according to the energy level transition theorem, so that electron absorption energy of the substance to be detected transits from a ground state to an excited state, and electrons are released along with energy release to return to a stable ground state due to instability of the excited state, and the process comprises fluorescence, internal energy conversion, vibration relaxation and the like.
The cavity ring-down spectroscopy technology is an absorption spectroscopy technology taking ring-down time as a measurement parameter, and is used for measuring through forming a ring-down curve by exponentially attenuating the transmitted light intensity of the ring-down cavity along with time, wherein the ring-down time is only related to the reflectivity of a ring-down cavity reflector and the absorption of a medium in the ring-down cavity, is irrelevant to the size of the incident light intensity, and has the advantages of high sensitivity, high signal to noise ratio and strong anti-interference capability. In existing cavity ring-down spectroscopy gas detection techniques, cavity ring-down experiments are typically performed to determine the fundamental performance of the detection device prior to gas detection. On the basis of a large amount of cavity ring-down time data, the obtained noise equivalent absorption coefficient is analyzed, and parameters such as measurement sensitivity, measurement precision or detection limit of the detection device on certain gas are obtained by utilizing the data and combining the gas absorption section. This increases the number of steps in the gas detection process, which makes the detection process cumbersome. Meanwhile, when the ambient temperature is detected to change, the cavity ring-down parameters cannot be updated in time, so that the error of the detection result is increased. When the laser light source is replaced to detect other gases, the cavity ring-down parameters need to be re-measured for calibration.
Disclosure of Invention
Aiming at the problems that the existing cavity ring-down spectroscopy gas detection technology is complicated in gas detection process, the cavity ring-down parameter needs to be re-measured when a light source is replaced to detect another gas, and the cavity ring-down parameter cannot be updated in real time according to the change of the detection environment, the invention provides a real-time self-calibration trace gas concentration detection device which is simple in gas detection process to be detected, can update the cavity ring-down parameter in real time according to the change of the detection environment, and has small error of gas concentration detection results.
The aim of the invention is realized by the following technical scheme:
a trace gas concentration detection apparatus capable of performing real-time self-calibration on cavity ring-down parameters, the apparatus comprising a DFB laser, a beam splitting sampling plate, a laser wavelength monitoring module, a laser control circuit module, a neutral beam splitter, a collimator, a pattern matching lens group, a real-time self-calibrating ring-down cavity, a focusing lens, a detector, and a data collection and analysis processing circuit module, wherein:
the DFB laser is connected with the laser control circuit module and used as a laser light source to output narrow linewidth laser.
The beam splitting sampling plate samples the laser beam and reflects the sampled laser beam to the laser wavelength monitoring mode.
And the laser wavelength monitoring module monitors the laser wavelength emitted by the laser after receiving the laser beam reflected by the beam splitting sampling plate, and feeds back the monitoring result to the laser control circuit module.
The laser control circuit module is used for providing a driving power supply for the DFB laser and adjusting and controlling the laser wavelength of the laser to the driving circuit of the laser according to the signal fed back by the laser wavelength monitoring module.
The neutral beam splitter splits the laser transmitted by the neutral beam splitter into two beams of coherent light, and the two beams of coherent light are respectively collimated by the collimator and irradiated to the ring-down cavity after being processed by the pattern matching lens group.
The real-time self-calibration ring-down cavity consists of a closed ring-down cavity and an open ring-down cavity which are parallel and adjacent to each other, wherein the closed ring-down cavity and the open ring-down cavity form ring-down cavities with identical parameters by using a flat concave reflector with identical indexes, and the leak rate of the closed ring-down cavity is better than 1.3x10 -10 Pa m 3 The stainless steel material of/s is made into the shell, the ring-down cavity formed by the plano-concave reflecting mirror is loaded into the shell, a gas inlet and outlet, a laser beam inlet and outlet and a vacuum gauge interface are formed in the stainless steel shell, the closed ring-down cavity is filled with nitrogen as zero gas or vacuumized when gas detection is carried out, the obtained ring-down curve is used as a benchmark of the ring-down curve obtained by the open cavity, and then an accurate gas concentration value is obtained.
The focusing lens is positioned behind the closed ring-down cavity and the open ring-down cavity respectively and is used for focusing laser beams transmitted by the closed ring-down cavity and the open ring-down cavity, and the focused laser beams are irradiated to the respective detectors.
The detector is a high-sensitivity photoelectric detector and is used for receiving laser signals transmitted by the closed ring-down cavity and the open ring-down cavity respectively.
The data collection and analysis processing circuit module is used for processing the photoelectric signals obtained by the detector to obtain the attenuation condition of the transmitted light intensity of the ring-down cavity along with time after the gas to be detected acts with the laser beam, so that the concentration of the gas to be detected is obtained.
According to the technical scheme, the cavity ring-down experiment step can be omitted in the gas detection process, the problems that in the existing cavity ring-down spectrum gas detection technology, the gas detection process is complicated, the cavity ring-down parameter needs to be re-measured when a light source is replaced to detect another gas, and the cavity ring-down parameter cannot be updated in real time according to the detection environment change are solved, and the method has the advantages of being simple in trace gas detection step, small in detection result error and capable of conducting real-time self-calibration on a test ring-down cavity.
The technical scheme provided by the invention can fulfill the aim of trace gas detection under different detection environment conditions.
According to the technical scheme provided by the invention, the trace gas concentration detection device has the advantages of simple trace gas detection steps and small detection error value, the parameters obtained by the open ring-down cavity are calibrated by using the parameters obtained by the closed ring-down cavity, the parameters obtained by the closed ring-down cavity can be calibrated in real time in various test environments, the test process is simple, and the detection result error value is small.
Drawings
In order to more clearly demonstrate the technical scheme of the real-time self-calibration trace gas concentration detection device provided by the invention, the technical scheme of the invention is intuitively displayed in the attached figure 1. It is obvious that the drawings are provided as an embodiment of the technical solution of the present invention, and that other drawings can be obtained from these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a real-time self-calibrating trace gas concentration detection apparatus of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
In the following, CO will be used in combination with the accompanying drawings 2 Or N 2 The O gas concentration detection means is described in further detail for the embodiment. FIG. 1 is a trace CO of the present invention 2 Or N 2 The structure of the O gas concentration detection device is schematically shown, and the device mainly comprises: DFB laser 1, beam splitting sampling plate 2, laser wavelength monitoring mode 3, laser control circuit module 4, neutral beam splitter 5, collimator 6, collimator 7, pattern matching lens group 8, pattern matching lens group 9, closed ring down cavity 10, open ring down cavity 11, focusing lens 12, focusing lens 13, detector 14, detector 15, data collection and analysis processing circuit module 16, wherein:
the DFB laser 1 has a linewidth of less than or equal to 2MHz, an output power of more than or equal to 10mW, a temperature tuning rate of 0.1 nm/DEG C, a current tuning rate of 0.01nm/mA, and a trace amount of CO 2 The laser wavelength of 1960nm in the gas is as follows, in trace N 2 The laser wavelength of the O gas is 2260nm, and trace CO 2 Or N 2 In the case of O gas, 1960nm and 2260nm wavelength lasers were used simultaneously.
The beam splitting sampling plate 2 reflects a laser beam with 5% of optical power to the laser wavelength monitoring module.
The laser wavelength monitoring module 3 receives the laser reflected by the beam splitting sampling plate 2, and feeds back the wavelength information of the laser to the laser circuit control module 4.
After receiving the feedback information of the wavelength monitoring module 3, the laser control circuit module 4 tunes the temperature and current of the laser according to parameters set in the experiment, and controls the output wavelength of the laser.
The neutral beam splitter 5 divides the laser transmitted by the beam splitting sampling plate into two beams of coherent light, and the light power ratio of the two beams of coherent light is 1:1.
The collimator 6 and the collimator 7 are used for respectively collimating two beams of coherent light obtained by the beam splitting mirror.
The mode matching lens group 8 and the mode matching lens group 9 respectively process the laser beams collimated by the collimator 6 and the collimator 7, and the coherent light processed by the mode matching lens group is respectively irradiated to the closed ring-down cavity 10 and the open ring-down cavity 11.
The closed ring-down cavity 10 and the open ring-down cavity 11 are formed by reflectors with reflectivity more than 99.99% to form a ring-down cavity, the parameters of the ring-down cavity are the same, the parameters of the reflectors are the same, wherein the closed ring-down cavity 10 uses a stainless steel shell with low leakage rate as the shell of the ring-down cavity, a gas inlet and a gas outlet, a laser beam inlet and a laser beam outlet and a vacuum gauge interface are arranged on the shell, the closed ring-down cavity is filled with nitrogen as zero gas or the closed ring-down cavity is vacuumized, and the ring-down curve obtained by the closed ring-down cavity is used for calibrating the ring-down curve obtained by the open ring-down cavity in real time.
The focusing lenses 12 and 13 are convex lenses, and focus the laser beams transmitted by the closed ring-down cavity 10 and the open ring-down cavity 11 to the detector 14 and the detector 15, respectively.
The detectors 14 and 15 are gain-adjustable InGaAs detectors, ring-down time measurement is performed under low gain, adjustment process optimization is performed under high gain, the detectors 14 and 15 transmit laser signals transmitted by the ring-down cavity to the data collecting and analyzing and processing circuit module 16, and the data collecting and analyzing and processing circuit module analyzes and processes the laser signals transmitted by the ring-down cavity to obtain laser beams and CO 2 Or N 2 The attenuation condition of the laser intensity transmitted by the ring-down cavity along with time after the O gas acts, and the CO is obtained through the obtained ring-down curve 2 Or N 2 Concentration value of O gas.
While the invention has been described with reference to preferred embodiments, it will be understood by those skilled in the art that the present invention is not limited thereto, and that various modifications and changes can be made without departing from the spirit of the invention, and it is intended that such modifications and changes be considered as the scope of the present invention.
Claims (3)
1. The real-time self-calibration trace gas concentration detection device comprises a DFB laser, a beam splitting sampling plate, a laser wavelength monitoring module, a laser control circuit module, a neutral beam splitting mirror, a collimator, a mode matching lens group, a real-time self-calibration ring-down cavity, a focusing lens, a detector and a data collection and analysis processing circuit module, and is characterized in that the real-time self-calibration ring-down cavity consists of a closed ring-down cavity and an open ring-down cavity which are parallel and adjacent to each other, the closed ring-down cavity and the open ring-down cavity are formed by ring-down reflectors with the same index, the ring-down cavities are made of stainless steel materials with the leak rate being better than 1.3X10-10 Pam3/s, the ring-down cavities formed by the flat-down reflectors are loaded into the shell, a gas inlet and outlet, a laser beam inlet and outlet and a vacuum gauge interface are formed in the stainless steel shell, the closed ring-down cavity is filled with nitrogen as zero gas or the closed ring-down cavity is vacuumized when the closed ring-down cavity is subjected to gas detection, the obtained ring-down cavity is subjected to ring-down curve vacuum pumping down, the obtained ring-down cavity has the ring-down curve with the same parameters, the ring-down curve is subjected to the real-down gas concentration detection, the ring-down curve is accurately detected in the real-time, and the real-time concentration detection is carried out, the ring-down curve is detected, and the concentration is accurate, and the real-time concentration detection is detected when the gas concentration is detected, and the real-time concentration detection test condition is detected, and the test concentration is detected;
the DFB laser is connected with the laser control circuit module and used as a laser light source to output laser with narrow linewidth;
the beam splitting sampling plate samples the laser beam and reflects the sampled laser beam to a laser wavelength monitoring mode;
the laser wavelength monitoring module monitors the laser wavelength emitted by the laser after receiving the laser beam reflected by the beam splitting sampling plate, and feeds back the monitoring result to the laser control circuit module;
the laser control circuit module is used for providing a driving power supply for the DFB laser and adjusting and controlling the laser wavelength of the laser for the driving circuit of the laser according to the signal fed back by the laser wavelength monitoring module;
the neutral beam splitter splits the laser transmitted by the neutral beam splitter into two coherent light beams, and the two coherent light beams are respectively collimated by the collimator and irradiated to the ring-down cavity after being processed by the pattern matching lens group;
the focusing lens is positioned behind the closed ring-down cavity and the open ring-down cavity respectively and is used for focusing laser beams transmitted by the closed ring-down cavity and the open ring-down cavity, and the focused laser beams are irradiated to the respective detectors;
the detector is a high-sensitivity photoelectric detector and is used for receiving laser signals transmitted by the closed ring-down cavity and the open ring-down cavity respectively;
the data collection and analysis processing circuit module is used for processing the photoelectric signals obtained by the detector to obtain the attenuation condition of the transmitted light intensity of the ring-down cavity along with time after the gas to be detected acts with the laser beam, so that the concentration of the gas to be detected is obtained.
2. The device for detecting the concentration of trace gas by real-time self-calibration according to claim 1, wherein the closed ring-down cavity and the open ring-down cavity are respectively formed by 2 flat concave high reflectors with reflectivity of more than or equal to 99.99%, the parameters of the reflecting lenses are the same, the parameters of the formed closed ring-down cavity and the parameters of the open ring-down cavity are the same, and the closed ring-down cavity is formed by loading the ring-down cavity formed by the high-reflecting lenses into a shell made of a low-leakage-rate stainless steel material.
3. The device for detecting the concentration of the trace gas by real-time self-calibration according to claim 1, wherein the neutral beam splitter splits a narrow linewidth laser beam into two coherent beams with optical power of 1:1, and the two beams of laser beams with the same parameters are respectively irradiated to the closed ring-down cavity and the open ring-down cavity for detecting the trace gas.
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|---|---|---|---|---|
| US5528040A (en) * | 1994-11-07 | 1996-06-18 | Trustees Of Princeton University | Ring-down cavity spectroscopy cell using continuous wave excitation for trace species detection |
| WO2021007782A1 (en) * | 2019-07-16 | 2021-01-21 | 深圳先进技术研究院 | Cavity ring-down spectrometer system |
| CN112903628A (en) * | 2021-01-25 | 2021-06-04 | 内蒙古光能科技有限公司 | Trace gas detection device in negative pressure state and detection method thereof |
| CN113092412A (en) * | 2021-04-13 | 2021-07-09 | 内蒙古光能科技有限公司 | Multi-component trace gas online detection device and method under negative pressure state |
| CN113659220A (en) * | 2021-08-05 | 2021-11-16 | 中国民航大学 | Lithium battery thermal runaway early warning system and method based on cavity ring-down spectroscopy technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7569823B2 (en) * | 2006-11-10 | 2009-08-04 | The George Washington University | Compact near-IR and mid-IR cavity ring down spectroscopy device |
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|---|---|---|---|---|
| US5528040A (en) * | 1994-11-07 | 1996-06-18 | Trustees Of Princeton University | Ring-down cavity spectroscopy cell using continuous wave excitation for trace species detection |
| WO2021007782A1 (en) * | 2019-07-16 | 2021-01-21 | 深圳先进技术研究院 | Cavity ring-down spectrometer system |
| CN112903628A (en) * | 2021-01-25 | 2021-06-04 | 内蒙古光能科技有限公司 | Trace gas detection device in negative pressure state and detection method thereof |
| CN113092412A (en) * | 2021-04-13 | 2021-07-09 | 内蒙古光能科技有限公司 | Multi-component trace gas online detection device and method under negative pressure state |
| CN113659220A (en) * | 2021-08-05 | 2021-11-16 | 中国民航大学 | Lithium battery thermal runaway early warning system and method based on cavity ring-down spectroscopy technology |
Non-Patent Citations (1)
| Title |
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| 光腔衰荡光谱技术及其应用综述;宓云;王晓萍;詹舒越;;光学仪器(第05期);全文 * |
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