CN103389283B - Turnable diode laser trace gas measurement device and method using high diffuse reflection square chamber to increase optical paths - Google Patents
Turnable diode laser trace gas measurement device and method using high diffuse reflection square chamber to increase optical paths Download PDFInfo
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
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Abstract
A turnable diode laser trace gas measurement device and method which use a high diffuse reflection square chamber to increase optical paths belong to the technical field of trace gas concentration measurement. The invention solves the problem that methods which increase gas absorption optical paths in a limited space are complex in structure and high in cost. The device comprises a diode laser and a high diffuse reflection square chamber. The device further comprises a photomultiplier tube, a sawtooth wave signal generator, a sine wave signal generator, a mixer, a temperature controller, a current controller, a data collection card, a computer, a high voltage power supply, a wedge incident quartz lens and a wedge exit quartz lens. The method demodulates an electrical signal output by the photomultiplier tube into a second harmonic signal in the computer to obtain an optical parameter OP of the concentration of a to-be-measured gas, and then compares the OP to a standard curve of a to-be-measured gas optical parameter changing with the concentration of a gas in a high diffuse reflection square chamber, to obtain the concentration of the to-be-measured gas and to achieve measurement of the content of the to-be-measured gas. The device and the method are used for trace gas measurement.
Description
Technical field
The present invention relates to the tunable diode laser trace gas detection device and the method that adopt high diffuse reflection square chamber to increase light path, belong to trace gas concentration detection technique field.
Background technology
The Sensitive Detection technology of gas concentration has important application in a lot of fields, such as in the monitoring of industrial production waste gas, medical treatment to the detection of characteristics of contaminated respiratory droplets gas componant and content, and air environmental pollution gas and the monitoring of toxic gas content etc.Utilize gas to the absorption characteristic of special wavelength light, developed multiple gases absorption spectroscopy techniques, comprise Differential Optical Absorption Spectroscopy DOAS, Fourier transform spectrometry (FTS) FTIR, associated light spectral technology COSPEC and tunable diode laser technology TDLAS etc.TDLAS technology has very high sensitivity, low detection limit, can detect gas concentration changing condition by real-time online, therefore be widely studied.In TDLAS technology, the diode laser having a very narrow emission spectrum by one is by sawtooch sweep and modulated by a high_frequency sine wave, the sweep limit of sawtooth wave is through the absorption line of gas to be measured, the second harmonic signal of demodulation sine wave, then can gas concentration be calculated according to Beer-Lambert law.There is the gas pollutant being interrupted spectral line characteristic, as all available TDLAS technology such as oxygen, methane and carbon dioxide detect.
At present, for improving the detection level of TDLAS technology to gas further, the most direct effective method increases gas absorption light path exactly in the finite space.Current light path both domestic and external increases technology and mainly contains the TDLAS technology etc. of leading to pool technology, integration chamber output spectrum technology ICOS, Research on Cavity Ring Down Spectroscopy CRDS, integrating sphere technology and scattering and strengthening more.Many logical pool technologies utilize light repeatedly to turn back to reach in the finite space effect increasing light path in sample cell, and for ensureing high reflectance and less energy loss, normal employing converges spherical mirror as reflecting element.Abroad to the research comparatively morning in many logical ponds, commercial White pond, Herriot pond and Chernin pond and various improvement pond are all widely used in the every field of trace gas/liquid body detection at present.Research on Cavity Ring Down Spectroscopy CRDS is also called cavity-type BPM laser absorption spectroscopy CavityRing-down Laser Absorption Spectroscopy, CRLAS, in sample cell, between two high reflection mirrors, propagate continuous absorbed strength retrogression back and forth by measurement light and the time measure sample concentration, Dalian Chemical Physics Research Institute utilizes cavity attenuation and vibration technique, research has been done to the general frequency spectrum of H2O, Wuhan Inst. of Physics and Mathematics, Chinese Academy of Sciences, the National University of Defense technology, Northwestern Polytechnical University, University of Electronic Science and Technology, many departments such as Photoelectric Technology Inst., Chinese Academy of Sciences have also carried out a large amount of research work to CRDS technology.Namely integrating sphere technology utilizes integrating sphere as gas cell, because integrating sphere itself makes complicated, expensive, is therefore used for greatly the gasmetry research in laboratory at present, is lessly applied to during industrial gasses detect.The advantage of TDLAS technology that scattering strengthens be highly sensitive, cost is low and volume is little, but due to the less stable of scattering medium own, the position of laser incident angle and detector all can make effective light path produce deviation, therefore need in practical application, to effective light path calibration of each scattering medium, to add measurement difficulty.In sum, the TDLAS technology of current long light path is in the complicacy of structure, and stabilization of equipment performance, portability and cost all respectively have shortcoming.
Summary of the invention
The present invention seeks in the finite space, to increase the complex structure and expensive problem that exist in the method for gas absorption light path at present to solve, providing a kind of the tunable diode laser trace gas detection device and the method that adopt high diffuse reflection square chamber increase light path.
The high diffuse reflection square chamber of employing of the present invention increases the tunable diode laser trace gas detection device of light path, it comprises diode laser and high diffuse reflection square chamber, it also comprises photomultiplier, Saw-tooth Signal Waveform Generator, sine wave signal generator, frequency mixer, temperature controller, current controller, data collecting card, computing machine, high-voltage power supply, incident wedge shape quartz lens and outgoing wedge shape quartz lens
High diffuse reflection square chamber sidewall arranges air intake opening and exhausr port,
The sawtooth signal output terminal of Saw-tooth Signal Waveform Generator connects the sawtooth signal input end of frequency mixer, the sine wave signal output terminal of sine wave signal generator connects the sine wave signal input end of frequency mixer, the mixed frequency signal output terminal of frequency mixer connects the current controling signal input end of current controller, the current controling signal output terminal of current controller connects the current controling signal input end of diode laser, the temperature control signals input end of diode laser connects the temperature control signals output terminal of temperature controller, the laser beam that diode laser exports is in the paramount diffuse reflection square chamber of incident wedge shape quartz lens entrance that high diffuse reflection square chamber incidence hole is arranged outward, the final outgoing wedge shape quartz lens outgoing arranged outward through high diffuse reflection square chamber light hole, and received by photomultiplier, photomultiplier provides operating voltage by high-voltage power supply, the collection signal input end of the gas absorption electrical signal connection data capture card of photomultiplier, the modulation reference signals input end of data collecting card connects the modulation reference signals output terminal of sine wave signal generator, the trigger pip input end of data collecting card connects the trigger pip output terminal of Saw-tooth Signal Waveform Generator, the collection signal output terminal of data collecting card connects the collection signal input end of computing machine,
Described high diffuse reflection square chamber is square, its light hole is arranged on bottom surface, incidence hole is arranged on the sidewall adjacent with bottom surface, light hole place, air intake opening is arranged on the end face relative with described bottom surface, exhausr port is arranged on the sidewall relative with described incidence hole place sidewall, and exhausr port is positioned at the downside of place sidewall.
Described high diffuse reflection square chamber adopts black acrylic as structural framework, and the inner wall surface even application of high diffuse reflection square chamber has the Avian-D height diffuse reflection coating of Lambertian characteristics.
The temperature-controlled precision of described temperature controller is 0.1 ° of C, and temperature-control range is 8 ° of C-60 ° of C.
The high diffuse reflection square chamber of employing increasing the tunable diode laser trace gas detection device of light path based on the high diffuse reflection square chamber of above-mentioned employing increases a tunable diode laser trace gas detection method for light path,
Select the centre wavelength of diode laser outgoing laser beam according to the absorption cross section of gas to be measured, pass into gas to be measured by the air intake opening of high diffuse reflection square chamber;
By the laser beam irradiation through sine wave signal generator and Saw-tooth Signal Waveform Generator modulation in high diffuse reflection square chamber, described laser beam is constantly scattered and transmits on high diffuse reflection square cavity wall, and is died down by gas absorption to be measured; Photomultiplier receives the light signal of high diffuse reflection square chamber outgoing and converts the electric signal of amplification to, in a computer the electric signal of this amplification is demodulated into second harmonic signal, obtain the optical parameter OP of gas concentration to be measured, again the typical curve that this optical parameter OP and other optical parameter to be measured change with gas concentration in high diffuse reflection square chamber is contrasted, obtain gas concentration to be measured, realize gas content to be measured and detect.
When gas to be measured is oxygen, the centre wavelength of diode laser outgoing laser beam is chosen as 762nm.
When gas to be measured is methane, the centre wavelength of diode laser outgoing laser beam is chosen as 1310nm.
When gas to be measured is carbon dioxide, the centre wavelength of diode laser outgoing laser beam is chosen as 1578nm.
Advantage of the present invention: the present invention using high diffuse reflection square chamber as gas cell, in conjunction with t unable filter, trace gas concentration is detected, the laser of modulation is irradiated in high diffuse reflection square chamber by it, due to the strong scattering effect of diffuse coatings on square cavity wall, laser is constantly scattered and transmits on square cavity wall; The light of the gas absorption specific wavelength to be measured in chamber, side makes it die down, and then detects the emergent light died down with photomultiplier.Adopt high diffuse reflection square chamber to make in the finite space, add gas absorption light path as gas cell, and this gas cell is easy to make, volume is little, and cost is low, can eliminate the impact of interference fringe, thus increases gas body burden detection sensitivity.
Apparatus of the present invention are by trace gas detection device miniaturization, and structure is simple, simple operation, and it has low cost and the high advantage of stability simultaneously.
Apparatus of the present invention and detection method can be used for contamination gas in industrial processes and detect, and diagnosed the illness and the field such as ambient atmosphere monitoring, can realize real time on-line monitoring gas concentration in medical treatment by human body Exhaust Gas.
Accompanying drawing explanation
Fig. 1 is the structural principle block diagram that the high diffuse reflection square chamber of employing of the present invention increases the tunable diode laser trace gas detection device of light path.
Embodiment
Embodiment one: present embodiment is described below in conjunction with Fig. 1, high diffuse reflection square chamber is adopted to increase the tunable diode laser trace gas detection device of light path described in present embodiment, it comprises diode laser 1 and high diffuse reflection square chamber 2, it also comprises photomultiplier 3, Saw-tooth Signal Waveform Generator 4, sine wave signal generator 5, frequency mixer 6, temperature controller 7, current controller 8, data collecting card 9, computing machine 10, high-voltage power supply 11, incident wedge shape quartz lens 12 and outgoing wedge shape quartz lens 13
High diffuse reflection square chamber 2 sidewall arranges air intake opening 2-1 and exhausr port 2-2,
The sawtooth signal output terminal of Saw-tooth Signal Waveform Generator 4 connects the sawtooth signal input end of frequency mixer 6, the sine wave signal output terminal of sine wave signal generator 5 connects the sine wave signal input end of frequency mixer 6, the mixed frequency signal output terminal of frequency mixer 6 connects the current controling signal input end of current controller 8, the current controling signal output terminal of current controller 8 connects the current controling signal input end of diode laser 1, the temperature control signals input end of diode laser 1 connects the temperature control signals output terminal of temperature controller 7, the laser beam that diode laser 1 exports is in the incident paramount diffuse reflection square chamber 2 of incident wedge shape quartz lens 12 that high diffuse reflection square chamber 2 incidence hole is arranged outward, final outgoing wedge shape quartz lens 13 outgoing arranged outward through high diffuse reflection square chamber 2 light hole, and received by photomultiplier 3, photomultiplier 3 provides operating voltage by high-voltage power supply 11, the collection signal input end of the gas absorption electrical signal connection data capture card 9 of photomultiplier 3, the modulation reference signals input end of data collecting card 9 connects the modulation reference signals output terminal of sine wave signal generator 5, the trigger pip input end of data collecting card 9 connects the trigger pip output terminal of Saw-tooth Signal Waveform Generator 4, the collection signal output terminal of data collecting card 9 connects the collection signal input end of computing machine 10,
Described high diffuse reflection square chamber 2 is square, its light hole is arranged on bottom surface, incidence hole is arranged on the sidewall adjacent with bottom surface, light hole place, air intake opening 2-1 is arranged on the end face relative with described bottom surface, exhausr port 2-2 is arranged on the sidewall relative with described incidence hole place sidewall, and exhausr port 2-2 is positioned at the downside of place sidewall.
In present embodiment, select photomultiplier 3 as detector, the high input voltage that high-voltage power supply 11 produces is in photomultiplier 3, convert electric signal after getting to the receiving screen of photomultiplier 3 by the light signal of high diffuse reflection square chamber 2 outgoing to and be exaggerated, then gathered by data collecting card 9, simultaneously using the TTL signal of Saw-tooth Signal Waveform Generator 4 and sine wave signal generator 5 in the trigger pip and modulation reference signals input data collecting card 9 of data acquisition.Digital signal is sent in computing machine 10 by pci interface by data collecting card 9, finally carries out demodulation by the lock-in amplify software write based on Labview to it and obtains second harmonic signal.The voltage of photomultiplier 3 is by high-voltage power supply 11 regulating and controlling.
The control accuracy of current controller 8 and range of control can be selected according to the type of diode laser 1, such as according to VCSEL single-mode laser then Current adjustment scope be 0mA-20mA, precision 1 μ A, general-purpose diode laser diode current range of control is 0mA-200mA, precision 0.1mA.Adopt signal generator to produce a high_frequency sine wave signal and a sawtooch sweep signal in wavelength-modulation technique, these two signals are by input current controller after frequency mixer mixing.The frequency range of Saw-tooth Signal Waveform Generator 4 is 1-100Hz, and amplitude is 100-500mV; The frequency of sine wave signal generator 5 is the 1k doubly left and right of Saw-tooth Signal Waveform Generator 4 frequency, and amplitude is 1/2 to 1/3 of Saw-tooth Signal Waveform Generator 4 amplitude.
Embodiment two: present embodiment is described below in conjunction with Fig. 1, present embodiment is described further embodiment one, described in present embodiment, high diffuse reflection square chamber 2 adopts black acrylic as structural framework, and the inner wall surface even application of high diffuse reflection square chamber 2 has the Avian-D height diffuse reflection coating of Lambertian characteristics.
Described Avian-D height diffuse reflection coating is the water base ethane coating of bi-component.
Embodiment three: present embodiment is described further embodiment one or two, the temperature-controlled precision of temperature controller 7 described in present embodiment is 0.1 ° of C, and temperature-control range is 8 ° of C-60 ° of C.
Embodiment four: present embodiment is described below in conjunction with Fig. 1, increases the tunable diode laser trace gas detection method of light path based on the high diffuse reflection square chamber of the employing of one of above-mentioned embodiment described in present embodiment,
Select the centre wavelength of diode laser 1 outgoing laser beam according to the absorption cross section of gas to be measured, pass into gas to be measured by the air intake opening 2-1 of high diffuse reflection square chamber 2;
By the laser beam irradiation modulated through sine wave signal generator 5 and Saw-tooth Signal Waveform Generator 4 in high diffuse reflection square chamber 2, described laser beam is constantly scattered and transmits on high diffuse reflection square chamber 2 inwall, and is died down by gas absorption to be measured; Photomultiplier 3 receives the light signal of high diffuse reflection square chamber 2 outgoing and converts the electric signal of amplification to, in computing machine 10, the electric signal of this amplification is demodulated into second harmonic signal, obtain the optical parameter OP of gas concentration to be measured, again the typical curve that this optical parameter OP and other optical parameter to be measured change with gas concentration in high diffuse reflection square chamber 2 is contrasted, obtain gas concentration to be measured, realize gas content to be measured and detect.
In present embodiment, can adopt lock-in amplify software that the electric signal amplified is demodulated into second harmonic signal in computing machine 10.Described typical curve is the relation curve between known gas concentration and second harmonic signal optical parameter demarcated in advance, can calculate gas concentration to be measured like this according to the size of the optical parameter OP obtained in actual measurement.
Gas to be measured passes into after in high diffuse reflection square chamber 2, can be discharged by exhausr port 2-2.
Embodiment five: present embodiment is described further embodiment four, in present embodiment, when gas to be measured is oxygen, the centre wavelength of diode laser 1 outgoing laser beam is chosen as 762nm.
In present embodiment, diode laser 1 can adopt centre wavelength at the VCSEL laser instrument of 762nm.
Embodiment six: present embodiment is described further embodiment four, in present embodiment, when gas to be measured is methane, the centre wavelength of diode laser 1 outgoing laser beam is chosen as 1310nm.
Embodiment seven: present embodiment is described further embodiment four, in present embodiment, when gas to be measured is carbon dioxide, the centre wavelength of diode laser 1 outgoing laser beam is chosen as 1578nm.
Claims (7)
1. the tunable diode laser trace gas detection device adopting high diffuse reflection square chamber to increase light path, it comprises diode laser (1) and high diffuse reflection square chamber (2), it is characterized in that, it also comprises photomultiplier (3), Saw-tooth Signal Waveform Generator (4), sine wave signal generator (5), frequency mixer (6), temperature controller (7), current controller (8), data collecting card (9), computing machine (10), high-voltage power supply (11), incident wedge shape quartz lens (12) and outgoing wedge shape quartz lens (13),
High diffuse reflection square chamber (2) sidewall is arranged air intake opening (2-1) and exhausr port (2-2),
The sawtooth signal output terminal of Saw-tooth Signal Waveform Generator (4) connects the sawtooth signal input end of frequency mixer (6), the sine wave signal output terminal of sine wave signal generator (5) connects the sine wave signal input end of frequency mixer (6), the mixed frequency signal output terminal of frequency mixer (6) connects the current controling signal input end of current controller (8), the current controling signal output terminal of current controller (8) connects the current controling signal input end of diode laser (1), the temperature control signals input end of diode laser (1) connects the temperature control signals output terminal of temperature controller (7), the laser beam that diode laser (1) exports is in the incident paramount diffuse reflection square chamber (2) of incident wedge shape quartz lens (12) that high diffuse reflection square chamber (2) incidence hole is arranged outward, final outgoing wedge shape quartz lens (13) outgoing arranged outward through high diffuse reflection square chamber (2) light hole, and received by photomultiplier (3), photomultiplier (3) provides operating voltage by high-voltage power supply (11), the collection signal input end of gas absorption electrical signal connection data capture card (9) of photomultiplier (3), the modulation reference signals input end of data collecting card (9) connects the modulation reference signals output terminal of sine wave signal generator (5), the trigger pip input end of data collecting card (9) connects the trigger pip output terminal of Saw-tooth Signal Waveform Generator (4), the collection signal output terminal of data collecting card (9) connects the collection signal input end of computing machine (10),
Described high diffuse reflection square chamber (2) is square, its light hole is arranged on bottom surface, incidence hole is arranged on the sidewall adjacent with bottom surface, light hole place, air intake opening (2-1) is arranged on the end face relative with described bottom surface, exhausr port (2-2) is arranged on the sidewall relative with described incidence hole place sidewall, and exhausr port (2-2) is positioned at the downside of place sidewall.
2. the high diffuse reflection square chamber of employing according to claim 1 increases the tunable diode laser trace gas detection device of light path, it is characterized in that, described high diffuse reflection square chamber (2) adopts black acrylic as structural framework, and the inner wall surface even application of high diffuse reflection square chamber (2) has the Avian-D height diffuse reflection coating of Lambertian characteristics.
3. the high diffuse reflection square chamber of employing according to claim 1 increases the tunable diode laser trace gas detection device of light path, and it is characterized in that, the temperature-controlled precision of described temperature controller (7) is 0.1 DEG C, and temperature-control range is 8 DEG C-60 DEG C.
4. increase a tunable diode laser trace gas detection method for light path based on the high diffuse reflection square chamber of employing adopting high diffuse reflection square chamber to increase the tunable diode laser trace gas detection device of light path described in claim 1, it is characterized in that,
Select the centre wavelength of diode laser (1) outgoing laser beam according to the absorption cross section of gas to be measured, pass into gas to be measured by the air intake opening (2-1) of high diffuse reflection square chamber (2);
The laser beam irradiation will modulated through sine wave signal generator (5) and Saw-tooth Signal Waveform Generator (4) is in high diffuse reflection square chamber (2), described laser beam is constantly scattered and transmits on high diffuse reflection square chamber (2) inwall, and is died down by gas absorption to be measured; Photomultiplier (3) receives the light signal of high diffuse reflection square chamber (2) outgoing and converts the electric signal of amplification to, in computing machine (10), the electric signal of this amplification is demodulated into second harmonic signal, obtain the optical parameter of gas concentration to be measured, again the typical curve that this optical parameter and other optical parameter to be measured change with high diffuse reflection square chamber (2) interior gas concentration is contrasted, obtain gas concentration to be measured, realize gas content to be measured and detect.
5. the high diffuse reflection square chamber of employing according to claim 4 increases the tunable diode laser trace gas detection method of light path, it is characterized in that, when gas to be measured is oxygen, the centre wavelength of diode laser (1) outgoing laser beam is chosen as 762nm.
6. the high diffuse reflection square chamber of employing according to claim 4 increases the tunable diode laser trace gas detection method of light path, it is characterized in that, when gas to be measured is methane, the centre wavelength of diode laser (1) outgoing laser beam is chosen as 1310nm.
7. the high diffuse reflection square chamber of employing according to claim 4 increases the tunable diode laser trace gas detection method of light path, it is characterized in that, when gas to be measured is carbon dioxide, the centre wavelength of diode laser (1) outgoing laser beam is chosen as 1578nm.
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| ITUB20169954A1 (en) * | 2016-01-13 | 2017-07-13 | L Pro S R L | GROUP AND METHOD OF MEASURING THE CONTENT OF GAS IN CLOSED CONTAINERS AND FILLING AND / OR AUTOMATIC PACKAGING LINE USING THIS GROUP |
| EP3193159A1 (en) * | 2016-01-13 | 2017-07-19 | L PRO S.r.l. | Group and method for measuring the gas content in closed containers and an automatic filling and/or packaging plant using such a group |
| EP3413032A1 (en) * | 2016-01-13 | 2018-12-12 | L PRO S.r.l. | An arrangement and method for measuring the gas content in the head space of a closed container and an automatic filling and/or packaging plant using such an arrangement |
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