CN104990887A - High-resolution infrared standard spectral measurement device and method - Google Patents
High-resolution infrared standard spectral measurement device and method Download PDFInfo
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- CN104990887A CN104990887A CN201510482902.8A CN201510482902A CN104990887A CN 104990887 A CN104990887 A CN 104990887A CN 201510482902 A CN201510482902 A CN 201510482902A CN 104990887 A CN104990887 A CN 104990887A
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Abstract
The invention discloses a high-resolution infrared standard spectral measurement device and method. According to the infrared spectroscopy absorbing features of gas components, the feature information (the absorbing wave band, the absorbing peak, the detection limit, the standard absorbance and the like) of each gas component is determined. The high-resolution infrared standard spectral measurement device and method can be used for high-resolution infrared standard spectral measurement of gas components of different concentrations and different temperatures and gas component quantitative analysis and qualitative identification in atmospheric environment detection through the Fourier transformation infrared spectroscopy technology and can meet the specific application needs of the infrared spectroscopy technology in gas detection.
Description
Technical field
The present invention relates to atmospheric environment detection technique and optical field, particularly relate to a kind of high-resolution reference infrared spectra measuring method and device.
Background technology
Infrared spectroscopy can be used for structure and the chemical bond of studying molecule, there is high characteristic, the method contrasted with the infrared spectrum of n-compound can be adopted to do Analysis and Identification, utilize the characteristic waves of chemical bond to differentiate the type of compound, and can be used for quantitative measurement, integrated use the present computer technology, the newest research results of multiple subject such as mathematical statistics and Chemical Measurement, and make it to combine together, with its exclusive feature in a lot of field, as environment, agricultural, oil, food, biochemical industry, pharmacy and medical science etc. are widely applied, in product quality analysis, the aspect such as on-line checkingi and technology controlling and process also obtains comparatively ten-strike.
Gas componant reference infrared spectra is the basis that fourier-transform infrared (FTIR) spectral technique carries out gas analysis related application, for the qualitative recognition algorithm of gas composition concentration inverting and non-principal component provides necessary spectral information.The infrared standard database that can be used for qualitative and quantitative analysis conventional at present mainly comprises three kinds: HITRAN database, NIST database and QAsoft database.HITRAN database provides the spectral line information of 30 different kinds of molecules existed in air, and NIST database provides the absorbance information of 21 kinds of atmospheric compounds molecules, and QAsoft database provides 310 kinds of atmospheric compounds molecular spectrum information altogether.The spectroscopic data kind of these databases can meet common gas and analyze demand, and spectroscopic data exists certain error, but for some gas componants not in database, before analyzing, must measure and obtain its standard spectrum information.
Summary of the invention
The object of this invention is to provide a kind of high-resolution reference infrared spectra measuring method and device, the gas componant high-resolution reference infrared spectra measurement of variable concentrations, different temperatures can be realized, thus meet the embody rule demand of infrared spectrum technology in gas detect.
The object of the invention is to be achieved through the following technical solutions:
A kind of high-resolution reference infrared spectra measurement mechanism, comprising: infrared light supply 1, first paraboloidal mirror 2, beam splitting chip 3, horizontal glass 4, index glass 5, first rotatable mirror 6, first ellipsoidal mirror 7, second paraboloidal mirror 8, gas cell directs window 9, three pieces of spherical mirrors 10 ~ 12, the infrared window 13 of gas cell outgoing, the 3rd paraboloidal mirror 14, second ellipsoidal mirror 15, second rotatable mirror 16, the 3rd rotatable mirror 17, focusing paraboloidal mirror 18, detector 19, computing machine 24 and gas sample cell 25; Wherein:
The continuous infrared waves of infrared light supply 1 radiation, by after the first paraboloidal mirror 2 reflection, reaches beam splitting chip 3; Wherein a part of light arrives index glass 5 through described beam splitting chip 3, prolongs original optical path return by index glass 5 after being reflected, and again arrives beam splitting chip 3, reflects through beam splitting chip 3; Another part light is reached horizontal glass 4 by described beam splitting chip 3 reflection, prolongs original optical path and returns, through beam splitting chip 3 transmission by horizontal glass 4 after being reflected;
Describedly to reflect through beam splitting chip 3 and light through beam splitting chip 3 transmission converges again, and produce interference when index glass 5 prolongs rectilinear motion, interference light is after the first rotatable mirror 6 reflects, the direction of propagation changes 90 degree, and reflect through the first ellipsoidal mirror 7, the direction of propagation changes 90 degree, again after the second paraboloidal mirror 8 reflects, gas sample cell 25 is entered through gas cell directs window 9, then after the reflection of piece spherical mirror 10 ~ 12 of three in gas sample cell 25 continuous several times, penetrate through the infrared window 13 of gas cell outgoing, the light of injection is the infrared interference light that have recorded gas absorption information in gas sample cell,
This infrared interference light reflects through paraboloidal mirror 14, reach the second ellipsoidal mirror 15, reflect through the second ellipsoidal mirror 15, the direction of propagation changes 90 degree, then reflects through the second rotatable mirror 16, the direction of propagation changes 90 degree, reflect through the 3rd rotatable mirror 17, the direction of propagation changes 90 degree again, arrives focusing paraboloidal mirror 18, after reflect focalization, be detected device 19 receive and record, computing machine 24 completes the sampling and processing of infrared interference signal from detector 19.
Described gas sample cell 25 adopts light path multiple reflections to cherish special structure, its outside is provided with glass capsulation cover 26, three pieces of spherical mirrors 10 ~ 12 of its inside are coated with infrared golden film and diaphragm, spectral range 2 ~ 14um, reflectivity > 90%, multiple reflections light path is the longest is 5 meters, and in three pieces of spherical mirrors 10 ~ 12, main spherical mirror 10 is placed in bottom gas sample cell 25, and secondary spherical mirror 11 and 12 is placed in gas sample cell 25 top;
The bottom of described gas sample cell 25 has also been opened two light holes and has been installed the infrared window 13 of gas cell directs window 9 gas cell outgoing respectively; The top of described gas sample cell 25 arranges air inlet/outlet, is connected with gas gas distributing system 21 by tracheae; Glass capsulation cover 26 is outer is also enclosed with heating tape, and in heating tape, set temperature sensor is connected with temperature control system 20.
Described gas gas distributing system 21 is connected with object gas 23 with zero gas 22 respectively, by controlling the flow of zero gas 22 and object gas 23, realizes the target gas levels preparation of variable concentrations.
A kind of high-resolution reference infrared spectra measuring method, the method realizes the infrared sampling and processing relating to light signal by aforesaid device, thus obtains high-resolution reference infrared spectra; Concrete:
The infrared interference signal that computing machine 24 collects is the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell, and have recorded the infrared interference signal of object gas absorption information in gas sample cell;
When after the above-mentioned interference signal that computing machine 24 collects, respectively the conversion of interference signal to spectrogram is carried out to above-mentioned interference signal, obtain zero gas spectrum and object gas absorption spectrum;
Object gas absorption spectrum division by 0 gas spectrum is obtained object gas Transmittance spectrum τ, gets negative logarithm operation: A=-ln τ to object gas Transmittance spectrum τ, the object gas absorbance spectrum A obtained is the reference infrared spectra of object gas.
Described interference signal comprises to the switch process of spectrogram:
Infrared interference signal is carried out Mertz phase only pupil filter;
By former bilateral interference signal zero padding to the same data length requiring frequency spectrum, then carry out truncation to interference signal, the truncation funcation of employing is rectangular function;
Again non-liner revision is carried out to interference signal, finally carry out Fourier transform, complete the conversion of interference light signal to spectrogram.
Obtain the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell, and the step of the infrared interference signal that have recorded object gas absorption information in gas sample cell comprises:
By zero gas 22 by gas gas distributing system 21 insufflation gas sample cell 25, and open temperature control system 20, the temperature of gas sample cell 25 is set to re-set target temperature, after gas temperature in gas cell is stable, gas sample cell 25 is entered by gas cell directs window 9, penetrating light by the infrared window 13 of gas cell outgoing is again the infrared interference light that have recorded zero aspiration collection of letters breath in gas sample cell, thus is collected the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell by computing machine 24;
Afterwards, the object gas 23 of concentration known is filled with by gas gas distributing system 21 insufflation gas sample cell 25, and continue to be filled with a period of time, after zero gas in gas sample cell 25 is all discharged and in gas sample cell 25, gas temperature is stablized, gas sample cell 25 is entered by gas cell directs window 9, penetrating light by the infrared window 13 of gas cell outgoing is again have recorded object gas in gas sample cell to absorb the infrared interference light of information, thus collects the infrared interference signal of the object gas absorption information in gas sample cell that have recorded by computing machine 24.
As seen from the above technical solution provided by the invention, it is according to gas componant Infrared spectra adsorption characteristic, determine the characteristic information (absorption bands, absorption peak, detectability and standard absorbance etc.) of each gas componant, be applicable to the gas componant high-resolution reference infrared spectra measurement of variable concentrations, different temperatures, can be used for Ftir Spectroscopy atmospheric environment detect in gas componant quantitative test and qualitative recognition, the embody rule demand of infrared spectrum technology in gas detect can be met.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
The structural representation of a kind of high-resolution reference infrared spectra measurement mechanism that Fig. 1 provides for the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
The embodiment of the present invention provides a kind of high-resolution reference infrared spectra measurement mechanism, its structural representation as shown in Figure 1, mainly comprise: infrared light supply 1, first paraboloidal mirror 2, beam splitting chip 3, horizontal glass 4, index glass 5, first rotatable mirror 6, first ellipsoidal mirror 7, second paraboloidal mirror 8, gas cell directs window 9, three pieces of spherical mirrors 10 ~ 12, the infrared window 13 of gas cell outgoing, 3rd paraboloidal mirror 14, second ellipsoidal mirror 15, second rotatable mirror 16, 3rd rotatable mirror 17, focusing paraboloidal mirror 18, detector 19, computing machine 24 and gas sample cell 25, wherein:
The continuous infrared waves of infrared light supply 1 radiation, by after the first paraboloidal mirror 2 reflection, reaches beam splitting chip 3; Wherein a part of light arrives index glass 5 through described beam splitting chip 3, prolongs original optical path return by index glass 5 after being reflected, and again arrives beam splitting chip 3, reflects through beam splitting chip 3; Another part light is reached horizontal glass 4 by described beam splitting chip 3 reflection, prolongs original optical path and returns, through beam splitting chip 3 transmission by horizontal glass 4 after being reflected;
Describedly to reflect through beam splitting chip 3 and light through beam splitting chip 3 transmission converges again, and produce interference when index glass 5 prolongs rectilinear motion, interference light is after the first rotatable mirror 6 reflects, the direction of propagation changes 90 degree, and reflect through the first ellipsoidal mirror 7, the direction of propagation changes 90 degree, again after the second paraboloidal mirror 8 reflects, gas sample cell 25 is entered through gas cell directs window 9, then after the reflection of piece spherical mirror 10 ~ 12 of three in gas sample cell 25 continuous several times, penetrate through the infrared window 13 of gas cell outgoing, the light of injection is the infrared interference light that have recorded gas absorption information in gas sample cell,
This infrared interference light reflects through paraboloidal mirror 14, reach the second ellipsoidal mirror 15, reflect through the second ellipsoidal mirror 15, the direction of propagation changes 90 degree, then reflects through the second rotatable mirror 16, the direction of propagation changes 90 degree, reflect through the 3rd rotatable mirror 17, the direction of propagation changes 90 degree again, arrives focusing paraboloidal mirror 18, after reflect focalization, be detected device 19 receive and record, computing machine 24 completes the sampling and processing of infrared interference signal from detector 19.
Described gas sample cell 25 adopts light path multiple reflections to cherish special structure, its outside is provided with glass capsulation cover 26, three pieces of spherical mirrors 10 ~ 12 of its inside are coated with infrared golden film and diaphragm, spectral range 2 ~ 14um, reflectivity > 90%, multiple reflections light path is the longest is 5 meters, and in three pieces of spherical mirrors 10 ~ 12, main spherical mirror 11 is placed in bottom gas sample cell 25, and secondary spherical mirror 10 and 12 is placed in gas sample cell 25 top;
The bottom of described gas sample cell 25 has also been opened two light holes and has been installed the infrared window 13 of gas cell directs window 9 gas cell outgoing respectively; The top of described gas sample cell 25 arranges air inlet/outlet, is connected with gas gas distributing system 21 by tracheae; Glass capsulation cover 26 is outer is also enclosed with heating tape, and in heating tape, set temperature sensor is connected with temperature control system 20.
Described gas gas distributing system 21 is respectively the gas flow controller of 5L/min and 50mL/min, stainless-steel tube, mixer, retaining valve, cabinet and control software design composition primarily of two flows, it is connected with object gas 23 with zero gas 22 respectively, by controlling the flow of zero gas 22 and object gas 23, realize the target gas levels preparation of variable concentrations.
The embodiment of the present invention also provides a kind of high-resolution reference infrared spectra measuring method, and the method realizes the infrared sampling and processing relating to light signal by aforesaid device, thus obtains high-resolution reference infrared spectra; Concrete:
The infrared interference signal that computing machine 24 collects is the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell, and have recorded the infrared interference signal of object gas absorption information in gas sample cell;
When after the above-mentioned interference signal that computing machine 24 collects, respectively the conversion of interference signal to spectrogram is carried out to above-mentioned interference signal, obtain zero gas spectrum and object gas absorption spectrum;
Object gas absorption spectrum division by 0 gas spectrum is obtained object gas Transmittance spectrum τ, gets negative logarithm operation: A=-ln τ to object gas Transmittance spectrum τ, the object gas absorbance spectrum A obtained is the reference infrared spectra of object gas.
Wherein, described interference signal comprises to the switch process of spectrogram:
Infrared interference signal is carried out Mertz phase only pupil filter;
By former bilateral interference signal zero padding to the same data length requiring frequency spectrum, then carry out truncation to interference signal, the truncation funcation of employing is rectangular function;
Again non-liner revision is carried out to interference signal, finally carry out Fourier transform, complete the conversion of interference light signal to spectrogram.
Wherein, obtain the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell, and the step of the infrared interference signal that have recorded object gas absorption information in gas sample cell comprises:
By zero gas 22 by gas gas distributing system 21 insufflation gas sample cell 25, and open temperature control system 20, the temperature of gas sample cell 25 is set to re-set target temperature, after gas temperature in gas cell is stable, the continuous infrared waves of infrared light supply 1 radiation, according to the structure shown in Fig. 1, via the first paraboloidal mirror 2, beam splitting chip 3, horizontal glass 4, index glass 5, first rotatable mirror 6, first ellipsoidal mirror 7, after second paraboloidal mirror 8 processes, gas sample cell 25 is entered by gas cell directs window 9, penetrating light by the infrared window 13 of gas cell outgoing is again the infrared interference light that have recorded zero aspiration collection of letters breath in gas sample cell, infrared interference light is now again according to the structure shown in Fig. 1, via the second ellipsoidal mirror 15, second rotatable mirror 16, 3rd rotatable mirror 17, focusing paraboloidal mirror 18, after detector 19 processes, the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell is collected by computing machine 24,
Afterwards, the object gas 23 of concentration known is filled with by gas gas distributing system 21 insufflation gas sample cell 25, and continue to be filled with a period of time, after zero gas in gas sample cell 25 all discharges (discharging by the vent port above secondary spherical mirror 10) and in gas sample cell 25, gas temperature is stablized, gas sample cell 25 is entered by gas cell directs window 9, penetrating light by the infrared window 13 of gas cell outgoing is again have recorded object gas in gas sample cell to absorb the infrared interference light of information, thus the infrared interference signal of the object gas absorption information in gas sample cell that have recorded is collected by computing machine 24, paths process and the preceding paragraph content similar.
It should be noted that, the method realizes based on aforementioned means, and the detailed process that therefore computing machine 24 gathers infrared interference signal see the description in previous embodiment, can repeat no more herein.
Embodiment of the present invention such scheme is according to gas componant Infrared spectra adsorption characteristic, determine the characteristic information (absorption bands, absorption peak, detectability and standard absorbance etc.) of each gas componant, be applicable to the gas componant high-resolution reference infrared spectra measurement of variable concentrations, different temperatures, can be used for Ftir Spectroscopy atmospheric environment detect in gas componant quantitative test and qualitative recognition, the embody rule demand of infrared spectrum technology in gas detect can be met.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. a high-resolution reference infrared spectra measurement mechanism, it is characterized in that, comprise: infrared light supply (1), first paraboloidal mirror (2), beam splitting chip (3), horizontal glass (4), index glass (5), first rotatable mirror (6), first ellipsoidal mirror (7), second paraboloidal mirror (8), gas cell directs window (9), three pieces of spherical mirror (10) ~ (12), the infrared window of gas cell outgoing (13), 3rd paraboloidal mirror (14), second ellipsoidal mirror (15), second rotatable mirror (16), 3rd rotatable mirror (17), focusing paraboloidal mirror (18), detector (19), computing machine (24) and gas sample cell (25), wherein:
The continuous infrared waves of infrared light supply (1) radiation, by after the first paraboloidal mirror (2) reflection, reaches beam splitting chip (3); Wherein a part of light arrives index glass (5) through described beam splitting chip (3), and being prolonged original optical path after index glass (5) reflection returns, and again arrives beam splitting chip (3), reflects through beam splitting chip (3); Another part light is reached horizontal glass (4) by described beam splitting chip (3) reflection, and being prolonged original optical path after horizontal glass (4) reflection returns, through beam splitting chip (3) transmission;
Describedly again to converge through beam splitting chip (3) reflection and light through beam splitting chip (3) transmission, and produce interference when index glass (5) prolongs rectilinear motion, interference light is after the first rotatable mirror (6) reflection, the direction of propagation changes 90 degree, and reflect through the first ellipsoidal mirror (7), the direction of propagation changes 90 degree, again after the second paraboloidal mirror (8) reflection, gas sample cell (25) is entered through gas cell directs window (9), then after three pieces of spherical mirrors (10) in gas sample cell (25) ~ (12) continuous several times reflection, penetrate through the infrared window of gas cell outgoing (13), the light of injection is the infrared interference light that have recorded gas absorption information in gas sample cell,
This infrared interference light reflects through paraboloidal mirror (14), reach the second ellipsoidal mirror (15), reflect through the second ellipsoidal mirror (15), the direction of propagation changes 90 degree, then reflect through the second rotatable mirror (16), the direction of propagation changes 90 degree, again through the 3rd rotatable mirror (17) reflection, the direction of propagation changes 90 degree, arrive focusing paraboloidal mirror (18), after reflect focalization, be detected device (19) receive and record, computing machine (24) completes the sampling and processing of infrared interference signal from detector (19).
2. device according to claim 1, it is characterized in that, described gas sample cell (25) adopts light path multiple reflections bosom special structure, its outside is provided with glass capsulation cover (26), three pieces of spherical mirror (10) ~ (12) of its inside are coated with infrared golden film and diaphragm, spectral range 2 ~ 14um, reflectivity > 90%, multiple reflections light path is the longest is 5 meters, in three pieces of spherical mirror (10) ~ (12), main spherical mirror (10) is placed in gas sample cell (25) bottom, secondary spherical mirror (11) is placed in gas sample cell (25) top with (12),
The bottom of described gas sample cell (25) has also been opened two light holes and has been installed the infrared window of gas cell directs window (9) gas cell outgoing (13) respectively; The top of described gas sample cell (25) arranges air inlet/outlet, is connected with gas gas distributing system (21) by tracheae; Glass capsulation cover (26) is also enclosed with heating tape outward, and in heating tape, set temperature sensor is connected with temperature control system (20).
3. device according to claim 2, it is characterized in that, described gas gas distributing system (21) is connected with object gas (23) with zero gas (22) respectively, by controlling the flow of zero gas (22) and object gas (23), realize the target gas levels preparation of variable concentrations.
4. a high-resolution reference infrared spectra measuring method, is characterized in that, the method realizes the infrared sampling and processing relating to light signal by the device described in any one of claim 1-3, thus obtains high-resolution reference infrared spectra; Concrete:
The infrared interference signal that computing machine (24) collects is the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell, and have recorded the infrared interference signal of object gas absorption information in gas sample cell;
When after the above-mentioned interference signal that computing machine (24) collects, respectively the conversion of interference signal to spectrogram is carried out to above-mentioned interference signal, obtain zero gas spectrum and object gas absorption spectrum;
Object gas absorption spectrum division by 0 gas spectrum is obtained object gas Transmittance spectrum τ, gets negative logarithm operation: A=-ln τ to object gas Transmittance spectrum τ, the object gas absorbance spectrum A obtained is the reference infrared spectra of object gas.
5. method according to claim 4, is characterized in that, described interference signal comprises to the switch process of spectrogram:
Infrared interference signal is carried out Mertz phase only pupil filter;
By former bilateral interference signal zero padding to the same data length requiring frequency spectrum, then carry out truncation to interference signal, the truncation funcation of employing is rectangular function;
Again non-liner revision is carried out to interference signal, finally carry out Fourier transform, complete the conversion of interference light signal to spectrogram.
6. method according to claim 4, is characterized in that, obtain the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell, and the step of the infrared interference signal that have recorded object gas absorption information in gas sample cell comprises:
By zero gas (22) by gas gas distributing system (21) insufflation gas sample cell (25), and open temperature control system (20), the temperature of gas sample cell (25) is set to re-set target temperature, after gas temperature in gas cell is stable, gas sample cell (25) is entered by gas cell directs window (9), be the infrared interference light that have recorded zero aspiration collection of letters breath in gas sample cell again by the infrared window of gas cell outgoing (13) injection light, thus the infrared interference signal that have recorded zero aspiration collection of letters breath in gas sample cell is collected by computing machine (24),
Afterwards, the object gas (23) of concentration known is filled with by gas gas distributing system (21) insufflation gas sample cell (25), and continue to be filled with a period of time, after zero gas in gas sample cell (25) is all discharged and in gas sample cell (25), gas temperature is stablized, gas sample cell (25) is entered by gas cell directs window (9), be the infrared interference light that have recorded object gas absorption information in gas sample cell again by the infrared window of gas cell outgoing (13) injection light, thus the infrared interference signal of the object gas absorption information in gas sample cell that have recorded is collected by computing machine (24).
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