CN104819958A - Method and device for automatically eliminating vapor interference in Fourier transform infrared spectroscopy gas detection - Google Patents
Method and device for automatically eliminating vapor interference in Fourier transform infrared spectroscopy gas detection Download PDFInfo
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Abstract
The invention relates to a method for automatically eliminating vapor interference in Fourier transform infrared spectroscopy gas detection. The method is characterized by comprising the steps of monitoring the vapor concentration in a gas cell in real time from a specified waveband by adopting a tunable laser absorption spectrum technology, automatically introducing pure nitrogen into to-be-detected gas in the gas cell according to the vapor concentration, enabling the vapor concentration of mixed gas in the gas cell to reach a predetermined concentration value, subtracting a vapor reference spectrum under the predetermined concentration acquired in the preliminary measurement by utilizing a subtraction method, eliminating the vapor interference, calculating the concentration of each component in the to-be-detected gas diluted by nitrogen, calculating a dilution ratio of the to-be-detected gas caused by nitrogen according to the vapor concentration values of the gas in the gas cell before and after pure nitrogen is introduced, and calculating the concentration of each component in the to-be-detected gas before being diluted. By adopting the method, the capability of the Fourier transform infrared spectroscopy technology for automatically and rapidly eliminating the vapor interference in the gas detection can be realized, and the unknown polluted gas can be rapidly detected.
Description
Technical field
The invention belongs to Fourier infrared spectrograph spectral measurement field, particularly in a kind of Fourier transform infrared spectroscopy gas detect, automatically eliminate the method and apparatus of steam interference.
Background technology
Industrial development brings increasing substantially of China's other polluting emissions, constitutes very large threat to people's health.Present stage Industrial-Enterprises in China many places in value chain, downstream, limited in one's ability to the input of pollution monitoring.Testing for numerous pollution source has mainly dropped on the limited environmental monitoring unit shoulder of personnel.This can propose active demand at pollution scene to the means that variety classes industrial gaseous waste detects easily and fast to acquisition is a kind of.
Ftir Spectroscopy has the advantage that hyperchannel is measured simultaneously, view picture spectrum can be obtained fast, extremely be suitable for the fast qualitative to types of unknown pollutants, quantitative test in principle, the gas pollutant component of a large amount of kind can be detected in laboratory conditions, there is very tempting development prospect.But, the problem that the interference of water vapor absorption peak is difficult to effectively eliminate can be run into when industry spot adopts Fourier Transform Spectroscopy to detect gaseous contamination source, cause the Detection Information of a large amount of important pollutant cannot be identified by the interference at water vapor absorption peak, calculate.And the method for water vapor absorption peak interference is not only time-consuming in elimination spectrum in the past conventional in laboratory, be also difficult to carry out in the on-the-spot environment limit that is subject to of pollution.
Because steam itself belongs to strong polar molecule, have stronger absorption peak, its spectral coverage is comparatively wide, and the pollutant kind affected is a lot, up to tens kinds.If do not adopt special step to eliminate separately water vapor absorption peak, and directly use the steam reference spectrum in the International Reference spectrum storehouses such as such as HITRAN directly to carry out qualitative and quantitative analysis to it, full of prunes result can be obtained.This can there is suitable big error owing to truly being measured by spectrometer between water vapor absorption peak that the water vapor absorption peak that obtains and International Reference compose in storehouse, and be used as spectral signal by mistake and substitute in the middle of the calculating of other component to be measured.Why in the analysis carried out the spectrum containing water vapor absorption peak, be difficult to obtain steam absorptivity accurately, trace it to its cause main be by vapour molecule between hydrogen bond cause.When vapour concentration changes can there is the nonlinear change departing from Lambert-Beer law in various degree in the absorptivity of its each absorption peak, and it also can move in position spectrally.This causes great difficulty steam absorptivity being carried out to matching.Although the existing much research about matching steam absorptivity under variable concentrations, the fitting precision of result of study is up to now all unsatisfactory.When being deducted the water vapor absorption peak got by inaccurate water vapor absorption coefficient calculations from measure spectrum by Lambert-Beer law, spectrally producing "false" peak, " bearing " peak, wrong identification and the erroneous calculations of thing can be polluted.During dusty gas detects, because pollutant levels are often far below moisture concentration, must be eliminated accurately by any special measures for the interference of water vapor absorption peak, otherwise a large amount of dusty gas can be caused to be difficult to be identified and quantitative test.
Up to now, a large amount of research work has been carried out in home and abroad in the interference of elimination steam, wherein in the detection of solid sample, report the multiple means reaching the interference of automatic steam and eliminate, but then relatively limited to the achievement in research in the steam interference elimination of gas detect.Be removed before steam enters measuring system for the most Perfected process eliminating steam interference.This not only can save the process eliminating steam interference, can also reduce the spectral energy loss that water vapor absorption causes, improve signal to noise ratio (S/N ratio).Main path solid testing sample being removed to steam in light path has: vacuum method and nitrogen sweeping method.But in dusty gas is detected, also do not have so far can under the prerequisite of not losing pollutant the method for Ex-all steam.Although this is can steam in Ex-all gas owing to there is many gas pre-treating methods, these methods generally all will use the method for condensation.And a large amount of gas pollutant belongs to water miscible, just can dissolve in wherein once touch condensate water, and discharge with water, pollute a large amount of even whole losses of thing.For avoiding the loss of pollutant, in gas preprocessing system, main employing is dewatered by the mode of solid drier or chemical reaction.Domestic gas pretreating device generally vapour concentration in gas can be dropped to be equivalent to-4 degrees Celsius dew point below, be equivalent to the intrinsic standoff ratio of 4000ppm to 5000ppm, be still much higher than in discharge of pollutant sources for the concentration (1 ~ 100ppm) of gas pollutant.Therefore after pre-treatment dewaters, also steam interference will be eliminated further by other means.
When water vapor absorption peak inevitably appears in determinand spectrum time, just must reach by deducting steam reference spectra on all four with it object eliminating steam interference.The spectrum subtraction technology be wherein often applied in solid sample detection adopts computer technology to carry out analog computation to water vapor absorption peak, subtracts for use in the difference measuring water vapor absorption peak in spectrum.For how calculate the absorption peak of variable concentrations steam is better the important research direction of field of gas detection always, but the result that existing method calculates still and between true measurement exists certain error.If have concentration difference infinitesimal steam reference spectrum storehouse in theory, the Fitting Calculation result is can steam spectrum in infinite approach experiment measuring.But in reality, because the variation range of the concentration of steam in gas to be measured is very large, carrying out the very little demarcation of spacing to it and mean extremely huge reference spectrum quantity, is unpractical.And both made to obtain such reference spectrum storehouse by an instrument by great many of experiments, due to different spectrometer and their instrument linear functions under different resolution all different, error also can be brought when transplanting on other spectrometer in this reference spectrum storehouse.The error brought in now steam spectrum simulation calculating, when solid sample detects because the light path in light path is shorter, steam error of fitting is little compared with determinand absorption intensity, can also accept.But when measuring dusty gas, because pollutant levels are often much smaller than vapour concentration, now the slight error caused calculated for water vapor absorption peak and all will have a strong impact on calculating to gas pollutant, so do not recommend this mode in the world.
Recommend in the world now to be also the removing method of steam interference in the gas detect generally adopted in laboratory be: after measuring gaseous spectrum to be measured, gas cell is purged with nitrogen clean, and passes into the nitrogen containing steam.By increasing vapour concentration in gas cell gradually, time completely the same to the water vapor absorption peak in itself and gaseous spectrum to be measured, the steam spectrum measured now is used for subtracting each other with gaseous spectrum to be measured, effectively can remove the impact of aqueous vapor interference.Because region, water vapor absorption peak in dusty gas exists the absorption peak interference of other pollutant, the mode artificially judged usually to be adopted when judging whether consistent with steam spectrum.Meanwhile, because FT-NIR spectra method does not have the ability measured in real time, carrying out each degree of regulation of the concentration of adjustments of gas pool inner water vapour by estimation and flow control can not very high (1% ~ 5%).Classic method often needs repeatedly to regulate, measure and carry out convergence target for several times, and the waste plenty of time is with artificial.This largely reducing the fast advantage of the measuring speed of Fourier transform infrared spectrometry own.So far there is no a kind of method eliminated steam automatically, fast and disturb in gas detect, this has had a strong impact on the practicality of FT-NIR spectra technology in gas detect.
In sum, in gas pollutant detection, steam interference is difficult to avoid and can has a strong impact on the measurement to pollutant.The method of existing elimination steam interference is difficult to the needs meeting Quick Measurement.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide the method and apparatus automatically eliminating steam interference in a kind of Fourier transform infrared spectroscopy gas detect, steam interference in gas detect can be eliminated automatically, fast in FFIR detects, reach the object precisely detected.
To achieve these goals, the technical solution used in the present invention is:
Automatically eliminate a method for steam interference in Fourier transform infrared spectroscopy gas detect, comprise the steps:
First gas to be measured is filled gas cell 2, measured by Ftir Spectroscopy and obtain its spectrum, then by vapour concentration in tunable diode laser absorption spectrometry technology Real-Time Monitoring gas cell 2;
Compare with predetermined target steam concentration value, control to pass into pure nitrogen gas in gas cell 2 internal contamination gas, the vapour concentration of mixed gas in pond is made it concentration value, the spectrum of now gas cell gas is obtained by Ftir Spectroscopy measurement, with minusing, gained spectrum and the steam reference spectrum under this predetermined concentration measuring acquisition are in advance subtracted each other again, obtain the measure spectrum after eliminating steam interference;
According to tunable diode laser absorption spectrometry technical monitoring to gas cell 2 in pass into vapour concentration before and after pure nitrogen gas, calculate the volume passing into pure nitrogen gas, and with this to by eliminate steam disturb after the concentration of test substance that obtains of measure spectrum revise, thus obtain pass into pure nitrogen gas before the concentration of each component in gas to be measured.
Describedly by the method for vapour concentration in tunable diode laser absorption spectrometry technology Real-Time Monitoring gas cell be: utilize a tunable laser 12 to send laser as light source, by beam splitter 1 by laser beam splitter, a branch of reception by infrared eye 1 after gas cell 2 measures light intensity magnitude, another bundle is by beam splitter 2 17 beam splitting again, a branch of again after beam splitting measures optical maser wavelength by wavemeter 18, another bundle again after beam splitting is received by infrared eye 2 19 and measures light intensity magnitude, the light intensity value received by comparing infrared eye 1 and infrared eye 2 19 obtain laser beam treated in gas cell side gas the absorptivity that absorbs, vapour concentration is tried to achieve again by the homologous thread of vapour concentration and absorptivity.
The wavelength chooses of described laser is be in the water vapor absorption peak that near-infrared band do not overlap with gas absorption peak to be measured.
Pass into pure nitrogen gas before in gas to be measured the concentration computing formula of each component be:
C
0＝C
1/η
Wherein, C
0for concentration of component, η is the volume ratio of pure nitrogen gas shared by gas cell passed into, C
1for the concentration of the test substance that the measure spectrum after eliminating steam interference obtains.
Present invention also offers the device automatically eliminating steam interference in a kind of Fourier transform infrared spectroscopy gas detect, comprise gas cell 2, interferometer unit 1 and the Signal reception of the catoptron in gas cell 2 and Fourier transform infrared spectrometer are connected with processing unit 3, a mouth of the gas reservoir to be measured 6 and Electrocontrolled tee valve 9 that store gas to be measured is connected, store the pure nitrogen gas storage tank 5 of pure nitrogen gas to be connected with second mouth of Electrocontrolled tee valve 9, 3rd mouth of Electrocontrolled tee valve 9 is connected with the air intake opening 10 of gas cell 2, Signal reception is connected with computing machine 4 with processing unit 3, simultaneously, also comprise tunable laser 12, the laser that tunable laser 12 exports is by beam splitter 1 beam splitting, a branch of reception by infrared eye 1 after gas cell 2 measures light intensity magnitude, another bundle is by beam splitter 2 17 beam splitting again, a branch of again after beam splitting measures optical maser wavelength by wavemeter 18, another bundle again after beam splitting is received measurement light intensity magnitude by infrared eye 19, measurement result is all sent to computing machine 4.
The wavelength of the laser that described tunable laser 12 exports controls the water vapor absorption peak being in near-infrared band and not overlapping with gas absorption peak to be measured in real time according to the measurement result of wavemeter 18.
Described beam splitter 1 according to the ratio beam splitting of light intensity energy 98:2, energy be the laser beam of 98% through gas cell 2, energy is that the laser beam of 2% is by beam splitter 2 17 beam splitting again.
Described beam splitter 2 17 is according to the ratio beam splitting of light intensity energy 1:1.
Described tunable laser 12 is Near-infrared Tunable laser instrument.
Compared with prior art, the invention has the beneficial effects as follows:
1, because Ftir Spectroscopy itself is not suitable for measuring the determinand concentration change from principle, present invention employs the tunable diode laser absorption spectrometry technology that is suitable for measuring in real time from specific band gas-monitoring pool inner water vapour concentration.Obtaining the judgement signal for automatically controlling with this, therefore automatically can pass into nitrogen adjustments of gas pool gas concentration to required particular value, eliminating the work that all people's work regulates, and greatly reduce regulating time, improve degree of regulation.
2, in the present invention because Ftir Spectroscopy and tunable diode laser absorption spectrometry technology can share same gas cell, therefore the cost of system volume that is low, instrument is little, also makes two kinds of light paths measured altogether road, reduces the error of measurement result.
The absorption peak kind of the gas 3, existing for near-infrared band is less, therefore can obtain vapour concentration value more accurately by measuring the water vapor absorption peak do not coincided with the absorption peak of other gas compositions in gas to be measured.Extremely be conducive to the automatic control to gas concentration in gas cell.
In sum, compact conformation of the present invention, accurately effectively can measure, regulate vapour concentration in gas to be measured, and eliminates the impact of water vapor absorption peak interference in Fourier transform infrared spectroscopy accurately and rapidly with this.The pollutant measurement kind of Fourier transform infrared spectroscopy can be increased, significantly expand its application scenario.
Accompanying drawing explanation
Fig. 1 is the principle schematic of existing FTIR spectrum gas detecting system.
Fig. 2 is the principle schematic in a kind of Fourier transform infrared spectroscopy gas detect of the present invention with the system automatically eliminating steam interference performance.
Fig. 3 is the schematic flow sheet automatically eliminating steam interference in a kind of Fourier transform infrared spectroscopy gas detect according to an embodiment of the invention.
Embodiment
Embodiments of the present invention are described in detail below in conjunction with drawings and Examples.
Existing Fourier transform infrared spectroscopy gas detecting system is general as shown in Figure 1.Mainly comprise the Fourier transform infrared spectrometer with interferometer unit 1 and Signal reception and processing unit 3, gas cell 2, computing machine 4, pure nitrogen gas storage tank 5, gas reservoir 6 to be measured, reduction valve 1 and reduction valve 28, Electrocontrolled tee valve 9 etc., catoptron wherein in gas cell 2 is connected with processing unit 3 with interferometer unit 1 and Signal reception, gas reservoir 6 to be measured is connected with a mouth of Electrocontrolled tee valve 9 and connecting line has reduction valve 28, pure nitrogen gas storage tank 5 is connected with second mouth of Electrocontrolled tee valve 9 and connecting line has reduction valve 1, 3rd mouth of Electrocontrolled tee valve 9 is connected with the air intake opening 10 of gas cell 2, gas cell 2 is also with gas outlet, Signal reception is connected with computing machine 4 with processing unit 3.
Its principle of work is: the infrared beam sent by interferometer unit 1, by being received by Signal reception and processing unit 3 and processed after gas cell 2, imports into measuring the spectral results obtained in computing machine 4.When measuring the component of certain gas to be measured, respectively by Electrocontrolled tee valve 9, post-decompression gas to be measured and pure nitrogen gas are filled gas cell 2 respectively, and measure their respective spectrum, obtain the absorption spectrum of infrared beam by gas to be measured by the spectrum of both contrasts, and constituent analysis can be carried out by it to gas to be measured.But the existence of water vapor absorption peak interference will have a strong impact on the analysis precision of multiple important dusty gas.
Thus, the invention provides the Fourier transform infrared spectroscopy gas detecting system automatically eliminating steam interference, its schematic diagram as shown in Figure 2.Except comprising in Fig. 1 and common Fourier transform infrared spectroscopy gas measurement system except all component, separately comprise tunable laser 12, beam splitter 1, catoptron 1 and catoptron 2 15, infrared eye 1, beam splitter 2 17, wavemeter 18 and infrared eye 2 19.
Tunable laser 12 sends the laser of required wavelength, light intensity energy is divided into be two bundles of 98:2 by beam splitter 1, wherein energy be 98% laser beam reflected by catoptron 1, enter to inject in gas cell 2, gas cell 2 is penetrated again after gas absorption, and reflect through catoptron 2 15, received by infrared eye 1 and measure light intensity magnitude; Energy be 2% laser beam enter to inject beam splitter 2 17, be divided into by beam splitter 2 17 laser beam that two-beam is equal by force; Wherein a branch of incidence enters in wavemeter 18, measures the wavelength value obtaining laser, and controls the wavelength output of tunable laser 12 according to this value; Beam of laser bundle is received by infrared eye 2 19 and measures light intensity magnitude in addition.
Measuring by infrared eye 1 and infrared eye 2 19 light intensity magnitude obtained by contrast, laser is subject to gas absorption decay in pond light intensity magnitude when entering to inject gas cell 2 can being obtained.Measure the laser wave long value now obtained again in conjunction with wavemeter 18, the attenuation by absorption of the laser light intensity in gas cell 2 for specific wavelength can be obtained.
Afterwards by regulating the optical maser wavelength that sends of tunable laser 12 in the absorption peak sector scanning of water vapor absorption spectrum, the absorption intensity at water vapor absorption peak in gas to be measured in gas cell 2 can be obtained, and calculated with this vapour concentration obtained in now gas cell by computing machine 4.Reach the monitoring to vapour concentration in gas cell.
When carrying out steam interference to gas to be measured and eliminating, its process flow diagram as shown in Figure 3.
First gas to be measured is filled gas cell 2, and measure its spectrogram of acquisition by Ftir Spectroscopy, and by the vapour concentration in gas to be measured in tunable diode laser absorption spectrometry technology Real-Time Monitoring gas cell.
On this basis, by computing machine 4 by comparing with predetermined target steam concentration value (wherein predetermined target steam concentration value should lower than the lower limit that dewaters of gas pretreating device), control the switch of Electrocontrolled tee valve 9, in gas cell 2, pass into appropriate pure nitrogen gas in gas to be measured, the vapour concentration of mixed gas in pond is made it concentration value.
The spectrogram of now gas cell gas is obtained by Ftir Spectroscopy measurement, because this spectrogram is that after passing into nitrogen dilution, its vapour concentration is adjusted to the spectrogram of predetermined value, therefore can be subtracted each other by the computing machine 4 pure water vapour reference spectrum of minusing with this predetermined concentration value measuring acquisition in advance, obtain the spectrogram after eliminating the interference of water vapor absorption peak.In order to calculate other gas composition concentration information separately in the rear gas to be measured of dilution according to Classical Least-Squares or pivotal methods [Liang Yizeng, Chemical Measurement, Beijing, Higher Education Publishing House, 2009.118.].
Finally by tunable diode laser absorption spectrometry technical monitoring to gas cell in pass into the forward and backward steam of nitrogen concentration value calculate the ratio of the total gas of gas cell shared by the nitrogen that passes into, and calculate with this dilution ratio η obtaining dilution, to the concentration value C of component to be measured in gas after the dilution obtained
1revise, obtain the concentration C that before passing into nitrogen dilution, in gas to be measured, each component is original
0.Its computing formula is:
C
0＝C
1/η
Should be understood that, just illustrate in the above description described and carry out the present invention in illustrating but not
Determinate, and do not depart from as appended claims under the prerequisite of the present invention that limits, can various change, distortion be carried out to above-described embodiment and/or revise.
Claims (9)
1. automatically eliminate a method for steam interference in Fourier transform infrared spectroscopy gas detect, it is characterized in that, comprise the steps:
First gas to be measured is filled gas cell (2), measured by Ftir Spectroscopy and obtain its spectrum, then by tunable diode laser absorption spectrometry technology Real-Time Monitoring gas cell (2) interior vapour concentration;
Compare with predetermined target steam concentration value, control to pass into pure nitrogen gas in gas cell (2) internal contamination gas, the vapour concentration of mixed gas in pond is made it concentration value, the spectrum of now gas cell gas is obtained by Ftir Spectroscopy measurement, with minusing, gained spectrum and the steam reference spectrum under this predetermined concentration measuring acquisition are in advance subtracted each other again, obtain the measure spectrum after eliminating steam interference;
According to tunable diode laser absorption spectrometry technical monitoring to gas cell (2) in pass into vapour concentration before and after pure nitrogen gas, calculate the volume passing into pure nitrogen gas, and with this to by eliminate steam disturb after the concentration of test substance that obtains of measure spectrum revise, thus obtain pass into pure nitrogen gas before the concentration of each component in gas to be measured.
2. automatically eliminate the method for steam interference according to claim 1 in Fourier transform infrared spectroscopy gas detect, it is characterized in that, describedly by the method for vapour concentration in tunable diode laser absorption spectrometry technology Real-Time Monitoring gas cell be: utilize a tunable laser (12) to send laser as light source, by beam splitter one (13) by laser beam splitter, a branch of reception by infrared eye one (16) after gas cell (2) measures light intensity magnitude, another bundle is by beam splitter two (17) beam splitting again, again after beam splitting a branch of by wavemeter (18) measure optical maser wavelength, another bundle again after beam splitting is received by infrared eye two (19) and measures light intensity magnitude, the light intensity value received by comparing infrared eye one (16) and infrared eye two (19) obtain laser beam treated in gas cell side gas the absorptivity that absorbs, vapour concentration is tried to achieve again by the homologous thread of vapour concentration and absorptivity.
3. automatically eliminate the method for steam interference according to claim 2 in Fourier transform infrared spectroscopy gas detect, it is characterized in that, the wavelength chooses of described laser is be in the water vapor absorption peak that near-infrared band do not overlap with gas absorption peak to be measured.
4. automatically eliminate the method for steam interference according to claim 1 in Fourier transform infrared spectroscopy gas detect, it is characterized in that, pass into pure nitrogen gas before in gas to be measured the concentration computing formula of each component be:
C
0＝C
1/η
Wherein, C
0for concentration of component, η is the volume ratio of pure nitrogen gas shared by gas cell passed into, C
1for the concentration of the test substance that the measure spectrum after eliminating steam interference obtains.
5. in Fourier transform infrared spectroscopy gas detect, automatically eliminate the device of steam interference, comprise gas cell (2), interferometer unit (1) and the Signal reception of the catoptron in gas cell (2) and Fourier transform infrared spectrometer are connected with processing unit (3), a mouth of the gas reservoir to be measured (6) and Electrocontrolled tee valve (9) that store gas to be measured is connected, store the pure nitrogen gas storage tank (5) of pure nitrogen gas to be connected with second mouth of Electrocontrolled tee valve (9), 3rd mouth of Electrocontrolled tee valve (9) is connected with the air intake opening (10) of gas cell (2), Signal reception is connected with computing machine (4) with processing unit (3),
It is characterized in that:
Also comprise tunable laser (12), the laser that tunable laser (12) exports is by beam splitter one (13) beam splitting, a branch of reception by infrared eye one (16) after gas cell (2) measures light intensity magnitude, another bundle is by beam splitter two (17) beam splitting again, again after beam splitting a branch of by wavemeter (18) measure optical maser wavelength, another bundle again after beam splitting is received by infrared eye (19) and measures light intensity magnitude, and measurement result is all sent to computing machine (4).
6. automatically eliminate the device of steam interference according to claim 5 in Fourier transform infrared spectroscopy gas detect, it is characterized in that, the wavelength of the laser that described tunable laser (12) exports controls the water vapor absorption peak being in near-infrared band and not overlapping with gas absorption peak to be measured in real time according to the measurement result of wavemeter (18).
7. automatically eliminate the device of steam interference according to claim 5 in Fourier transform infrared spectroscopy gas detect, it is characterized in that, described beam splitter one (13) is according to the ratio beam splitting of light intensity energy 98:2, energy be the laser beam of 98% through gas cell (2), energy is that the laser beam of 2% is by beam splitter two (17) beam splitting again.
8. automatically eliminate the device of steam interference in Fourier transform infrared spectroscopy gas detect according to claim 5 or 7, it is characterized in that, described beam splitter two (17) is according to the ratio beam splitting of light intensity energy 1:1.
9. automatically eliminate the device of steam interference according to claim 5 in Fourier transform infrared spectroscopy gas detect, it is characterized in that, described tunable laser (12) is Near-infrared Tunable laser instrument.
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