WO2014112502A1 - Dispositif d'analyse de gaz par laser - Google Patents

Dispositif d'analyse de gaz par laser Download PDF

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Publication number
WO2014112502A1
WO2014112502A1 PCT/JP2014/050527 JP2014050527W WO2014112502A1 WO 2014112502 A1 WO2014112502 A1 WO 2014112502A1 JP 2014050527 W JP2014050527 W JP 2014050527W WO 2014112502 A1 WO2014112502 A1 WO 2014112502A1
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gas
wavelength
laser
absorption
light
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PCT/JP2014/050527
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English (en)
Japanese (ja)
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康彦 光本
力 矢田部
平田　隆昭
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横河電機株式会社
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • 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
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis

Definitions

  • the present invention relates to a laser gas analyzer, and more particularly to a laser gas analyzer that can efficiently measure a hydrocarbon multicomponent mixed gas.
  • Laser gas analyzers using the TDLAS (Tunable Diode Laser Absorption Spectroscopy) method only irradiate light from a wavelength tunable semiconductor laser to the measurement target components such as high temperature and corrosive gas. Even in the case of a concentration of 1, there is an advantage that the component selectivity is high without being interfered by other components, and measurement can be performed in real time at high speed without contact.
  • TDLAS Tunable Diode Laser Absorption Spectroscopy
  • FIG. 7 is a block diagram showing an example of a conventional laser gas analyzer using the TDLAS method, in which a light source unit including a semiconductor laser that irradiates a measurement laser beam into a measurement gas atmosphere, and measurement of the measurement gas atmosphere It comprises a light receiving element that detects the measurement laser beam that has passed through the space, and a detection unit that includes an arithmetic processing unit that processes the output signal of this light receiving element.
  • a light source unit including a semiconductor laser that irradiates a measurement laser beam into a measurement gas atmosphere, and measurement of the measurement gas atmosphere It comprises a light receiving element that detects the measurement laser beam that has passed through the space, and a detection unit that includes an arithmetic processing unit that processes the output signal of this light receiving element.
  • the laser gas analyzer shown in FIG. 7 uses a semiconductor laser having a very narrow oscillation wavelength spectrum line width for the light absorption spectrum inherent to the molecule due to the vibration / rotational energy transition of the molecule to be measured existing in the infrared to near infrared region. To measure.
  • the absorption spectra unique to most molecules such as O 2 , NH 3 , H 2 O, CO, CO 2 are in the infrared to near-infrared region, and are measured by measuring the amount of light absorption (absorbance) at a specific wavelength. The concentration of the component can be calculated.
  • the semiconductor laser 11 provided in the light source unit 10 irradiates and outputs a measurement laser beam in the atmosphere of the measurement gas 20.
  • the laser light output from the semiconductor laser 11 has a very narrow oscillation wavelength spectrum line width, and the oscillation wavelength can be changed by changing the laser temperature or drive current. Therefore, only one of the absorption peaks of the absorption spectrum can be measured.
  • the absorption peak that is not affected by the interference gas can be selected, the wavelength selectivity is high, and it is not affected by other interference components. Therefore, the process gas is removed without removing the interference gas in the previous stage of measurement. Can be measured directly.
  • the spectrum shape includes the measurement gas temperature, the measurement gas pressure, It changes due to the broadening phenomenon of spectrum due to coexisting gas components. For this reason, the actual process measurement accompanied by these environmental variations requires correction.
  • the apparatus shown in FIG. 7 uses a spectrum area method in which the spectrum area is obtained by scanning the oscillation wavelength of the semiconductor laser 11 and measuring the absorption spectrum, and converting the spectrum area into the component concentration.
  • the peak height method for determining the measurement component from the peak height of the absorption spectrum or the wavelength scan signal is modulated and the PP (peak-to-peak) value of the frequency modulation waveform is double that frequency.
  • the 2f method for obtaining the concentration of the measured component from the above is used, but these are easily affected by fluctuations in temperature, pressure, coexisting gas components, and the like.
  • the spectrum area is not affected by changes due to the difference in the coexisting gas components in principle (the spectrum area is almost constant regardless of the coexisting gas components), and the spectrum area is also in principle against pressure fluctuations. Shows a linear change.
  • the above three fluctuation factors (temperature, pressure, coexisting gas components) all affect nonlinearly, and when these fluctuation factors coexist, correction is difficult.
  • the linear correction for the gas pressure fluctuation and the non-linear correction for the gas temperature fluctuation can be performed, and an accurate correction can be realized.
  • the measurement laser light that has passed through the atmosphere of the measurement gas 20 is received by the light receiving element 31 provided in the detection unit 30 and converted into an electrical signal.
  • the output signal of the light receiving element 31 is adjusted to an appropriate amplitude level via the variable gain amplifier 32, input to the A / D converter 33, and converted into a digital signal.
  • the integration is performed a predetermined number of times (for example, several hundred to several thousand times) between the integrator 34 and the memory 35, and the memory 35 is supplied. Is repeated, noise included in the measurement signal is removed and the data is smoothed, and then input to the CPU 36.
  • the CPU 36 performs arithmetic processing such as measurement gas concentration analysis based on the measurement signal from which noise has been removed, and an amplifier when the amplitude level of the output signal of the light receiving element 31 is not appropriate as the input level of the A / D converter 33. 32 gain adjustment is performed.
  • Non-Patent Document 1 describes the measurement principle, features, and specific measurement examples of a laser gas analyzer that applies wavelength-tunable semiconductor laser spectroscopy.
  • the laser gas analyzer configured as shown in FIG. 7 is limited to the measurement of a single component because the wavelength variable range of the semiconductor laser 11 is narrow.
  • hydrocarbons other than CH 4 when measuring a hydrocarbon multi-component gas mixture, hydrocarbons other than CH 4 have a complicated molecular structure and a large number of absorption lines overlap, so that broad absorption exists in the base other than sharp absorption lines. There is no wavelength. For this reason, it is impossible to correct the baseline fluctuation due to the change in the transmittance of the gas cell itself.
  • the spectrum width of aromatic hydrocarbon species having a large carbon number, alkylbenzene, etc. is several tens nm or more, whereas methane having a small carbon number has a narrow spectrum width of about 0.1 nm. Therefore, the spectrum broadening effect can be obtained by analyzing the concentration of mixed hydrocarbons of a gas with a narrow spectral width such as methane and a gas with a wide spectral width such as aromatic hydrocarbon species or alkylbenzene by the statistical method of the prior art.
  • the concentration error of a gas having no absorption peak increases due to the spectral error of a gas having a narrow spectral width due to a slight wavelength error.
  • a narrow gas spectrum such as a methane peak
  • the spectrum shape changes greatly due to the broadening effect, and the absorption error due to wavelength changes is large, so that the spectrum error due to wavelength errors is large.
  • the concentration of methane gas is sufficiently high compared to other gases
  • the spectral error due to such spectral shape change and wavelength error at the methane peak becomes so large that it cannot be ignored compared to other gas spectra. This is an error in measuring the concentration of gases other than methane.
  • the present invention solves these problems, and its purpose is to use a wavelength tunable laser having a wide wavelength tunable width as a laser light source, and remove a sharp peak portion of a mixed gas (for example, methane) for concentration detection.
  • a statistical method is used to realize a laser gas analyzer that can measure a hydrocarbon having a large spectral characteristic at the same time as a hydrocarbon having a small spectral characteristic with high accuracy. Even if the gas to be measured is a mixed gas of a gas having a small absorption spectrum characteristic and a gas having a large absorption spectrum characteristic, the concentration of the gas having a small absorption spectrum characteristic in the measurement gas can be accurately determined.
  • An object is to realize a laser gas analyzer capable of measuring.
  • a wavelength tunable laser having a wide wavelength tunable width a light irradiating means for irradiating the gas to be measured with the output light of the wavelength tunable laser as measurement light, and absorption related to the measurement light transmitted through the gas to be measured
  • a laser gas analyzer configured with a data processing unit for obtaining an absorption spectrum of the gas to be measured based on a signal and obtaining a concentration of each component based on a statistical method
  • the data processing unit determines the component concentration of a gas having no sharp absorption peak, and has a wavelength at which no sharp absorption peak of another gas component exists in an absorption spectrum obtained by sweeping a relatively wide wavelength range. The absorption spectrum of the region is used.
  • a wavelength tunable laser having a wide wavelength tunable width a light branching means for branching the output light of the wavelength tunable laser into measurement light and reference light, and irradiating the measurement light with the measurement light, and the reference light
  • a data processing unit for obtaining an absorption spectrum of the measurement gas based on the reference signal obtained and an absorption signal related to the measurement light transmitted through the measurement gas, and obtaining a concentration of each component based on a statistical method.
  • the data processing unit determines the component concentration of a gas having no sharp absorption peak, and has a wavelength at which no sharp absorption peak of another gas component exists in an absorption spectrum obtained by sweeping a relatively wide wavelength range. The absorption spectrum of the region is used.
  • the data processing unit An absorption line wavelength data storage unit for storing absorption line wavelength data of the measured gas;
  • the reference signal and the absorption signal are input and the absorption line wavelength data storage unit is connected, and wavelength calibration means for calibrating the wavelength of the absorption spectrum based on the absorption line wavelength data, the reference signal, and the absorption signal;
  • Wavelength region selection means for selecting a wavelength region of an optical signal used for measuring the concentration of the gas to be measured;
  • a concentration detecting means for determining the concentration of the gas to be measured based on a statistical model constructed in advance.
  • the wavelength calibration means compares the absorption line of the calibration gas with a known absorption line.
  • a laser gas analyzer for determining the concentration of a component contained in a gas to be measured which is a mixed gas
  • a tunable laser that sweeps a relatively wide wavelength range
  • An optical system that transmits at least part of the output light of the wavelength tunable laser as measurement light to the gas to be measured and guides the measurement light after transmission to the light receiving element
  • a data processing unit for obtaining an absorption spectrum of the gas to be measured based on the output of the light receiving element, and obtaining a concentration of each component based on a statistical method; With The data processing unit obtains an absorption spectrum in a wavelength region in which no sharp absorption peak exists in the absorption spectrum of the measurement gas when obtaining the concentration of a gas having a small absorption spectrum characteristic among the gases contained in the measurement gas. It is characterized by using.
  • the statistical method is characterized in that the concentration of each gas is obtained from the spectrum of the gas to be measured based on a statistical model in which the relationship between the spectrum and the concentration is preliminarily constructed based on a gas spectrum having a known concentration. .
  • the statistical model includes at least one of an outside air temperature, a gas temperature, and a gas pressure as a parameter.
  • the gas to be measured is a hydrocarbon mixed gas mixture
  • the gas having a large feature in the absorption spectrum is methane
  • the gas having a small characteristic in the absorption spectrum is a hydrocarbon other than methane.
  • An optical branching unit that divides at least a part of the light emitted from the wavelength tunable laser into two of measurement light and reference light; A gas cell into which the measurement gas is introduced and the measurement light is incident; A first light receiving element on which light emitted from the gas cell is incident; A second light receiving element on which the reference light is incident,
  • the distance from the light branching means to the incident end face of the gas cell is L1, the distance from the emission end face of the gas cell to the first light receiving element is L2, and the distance from the light branching means to the second light receiving element is L3.
  • concentration of each gas contained in a multicomponent mixed gas can be measured comparatively easily using a statistical method.
  • a wavelength variable laser having a wide wavelength variable width is used as a laser light source, and an absorption spectrum in a wavelength region where there is no sharp absorption peak of the gas to be measured is used, so that the gas to be measured has small absorption spectrum characteristics. Even if it is a mixed gas of a gas and a gas having a large absorption spectrum characteristic, it is possible to realize a laser gas analyzer that can accurately measure the concentration of a gas having a small absorption spectrum characteristic in the gas to be measured.
  • FIG. 2 is a differential spectrum diagram of 1% nC 4 H 10 spectrum and CH 4 having a concentration of 80%. It is a block diagram which shows the other Example of this invention. It is a block diagram which shows an example of the conventional laser gas analyzer.
  • FIG. 1 is a block diagram showing an embodiment of a laser gas analyzer according to the present invention.
  • a wavelength tunable laser 101 generates measurement light of an absorption spectrum of a gas to be measured, and is connected to an oscillation wavelength control circuit 102 that controls the oscillation wavelength.
  • the oscillation wavelength control circuit 102 sweeps the oscillation wavelength of the wavelength tunable laser 101 within a range of 1.67 to 1.72 ⁇ m, for example.
  • the light emitted from the wavelength tunable laser 101 is converted into parallel light by the lens 103, passes through the isolator 104, and is divided into two parallel light of measurement light and reference light by the beam splitter 105.
  • One of the parallel lights divided into two by the beam splitter 105 is incident on a gas cell 106 into which a gas to be measured is introduced as measurement light, collected by a lens 107, incident on a photodiode 108, and converted into an electrical signal. And input to one input terminal of the wavelength calibration means 111.
  • the other parallel light is condensed by the lens 109 and incident on the photodiode 110 as reference light, converted into an electric signal, and input to the other input terminal of the wavelength calibration means 111.
  • the absorption spectrum of the gas to be measured is obtained from the measurement signal based on the measurement light of the gas and the reference signal based on the reference light of the output intensity.
  • a wavelength region selection unit 112 is connected to the wavelength calibration unit 111, and a concentration detection unit 113 is connected to the wavelength region selection unit 112.
  • FIG. 2 is a block diagram showing a specific example of a laser gas analyzer based on the present invention for measuring hydrocarbon multicomponents, and the same reference numerals are given to the parts common to FIG.
  • an absorption line wavelength data storage unit 114 is connected to the wavelength calibration unit 111
  • a use wavelength data storage unit 115 is connected to the wavelength region selection unit 112
  • a statistical model storage unit 116 is connected to the concentration detection unit 113. It is connected.
  • MEMS-VCSEL is used as the wavelength tunable laser 101 (light source) and that the laser beam output from the wavelength tunable laser 101 is three beams by the beam splitter 117 after the isolator 104. And the third light is incident on the photodiode 120 through the wavelength calibration cell 118 and the lens 119 in which the reduced pressure CH 4 is enclosed. Note that the output signal of the photodiode 120 is also input to the wavelength calibration means 111.
  • FIG. 3 is a spectrum example of a chain saturated hydrocarbon to be measured in this example.
  • A is CH 4 (methane)
  • B is C 2 H 6 (ethane)
  • C is C 3 H 8 (propane)
  • D is iC 4 H 10 (isobutane)
  • E is nC 4 H 10 (normal butane)
  • F is iC 5 H 12 (isopentane)
  • G is C 5 H 12 (normal pentane).
  • CH 4 , C 2 H 6 , C 3 H 8 , and iC 4 H 10 have sharp peaks, but there are no sharp peaks in other gas spectra. Is small. In order to perform highly accurate concentration detection from a gas spectrum having a small feature, it is effective to perform statistical processing using an absorption spectrum obtained by sweeping a wide wavelength.
  • MEMS-VCSEL is a semiconductor laser and can be swept in a relatively wide wavelength range of about 50 nm, sufficient absorption spectrum information can be obtained, and highly accurate concentration detection can be performed by a statistical method.
  • FIG. 4 is a flowchart for explaining the flow of concentration measurement operation by the apparatus according to the present invention.
  • photodiode output data and database data are first read (step S1).
  • the wavelength calibration unit 111 calibrates the wavelength of the absorption spectrum of the gas to be measured based on the position of the absorption line of CH 4 in the calibration signal and the absorption line wavelength data stored in the absorption line wavelength data storage unit 114 (step S2).
  • the absorbance is proportional to the concentration (step S3).
  • I 0 is the incident intensity to the measurement gas cell
  • I is the transmitted light intensity from the measurement gas cell.
  • S1 is a reference signal
  • S2 is a measurement signal
  • T ( ⁇ ) is an apparatus function (transmittance of the gas cell 106 to be measured, wavelength dependence of the branching ratio of the beam splitter 117).
  • the constant term includes a term corresponding to the branching ratio of the beam splitter.
  • the concentration detection means 113 Statistical methods such as multivariate analysis are used as the concentration detection means 113 (step S4).
  • the statistical method means that a statistical model of the relationship between the spectrum and the concentration is built in advance based on the gas spectrum with a known concentration, and when the spectrum of the gas to be measured is acquired, the statistical model built in advance is used. Based on this, the concentration of each gas is obtained. For example, the PLS regression method is well known. In constructing a statistical model in advance, highly accurate concentration detection is possible by measuring as uniformly as possible within the measurement target concentration range.
  • the wavelength region selection unit 112 When concentration detection is performed from a gas spectrum, it is common to use a wavelength band having a large spectral feature such as a peak. However, it may be better not to use an absorption peak when the absorption by each gas is significantly different.
  • FIG. 5 shows a 1% nC 4 H 10 spectrum and a derivative spectrum of CH 4 at a concentration of 80%.
  • the differential spectrum indicates a difference from a spectrum having a wavelength different by 1 pm, and indicates a magnitude of a spectrum error caused by a wavelength error of 1 pm.
  • the influence of the CH 4 wavelength error is large, and when a 1 pm wavelength error occurs, a spectral error larger than the nC 4 H 10 spectrum occurs in the wavelength band where the CH 4 peak exists.
  • MEMS-VCSEL has sufficient reliability as an industrial instrument that combines a MEMS movable mirror without mechanical moving parts and a semiconductor laser that has been proven to be highly reliable in optical communications, and has a wide wavelength tunable range.
  • a wavelength tunable laser and performing wavelength sweeping within a wavelength range of 1.67 to 1.72 ⁇ m where absorption lines of various hydrocarbons exist, an absorption spectrum of a hydrocarbon multicomponent mixed gas can be measured.
  • An accurate absorption spectrum can be obtained by performing wavelength calibration of the absorption spectrum of the hydrocarbon multi-component mixed gas obtained using the CH 4 absorption line and wavelength table.
  • TDLAS that can be measured in real time has a narrow wavelength variable width of the light source, and is mainly limited to measurement of a single component.
  • the absorption spectrum of multi-component mixed gas is achieved by using MEMS-VCSEL, which has no mechanical moving parts and has high reliability required as an industrial instrument and can change the wavelength in a wide wavelength range as a light source.
  • Industrial TDLAS can be realized.
  • a TDLAS capable of analyzing a hydrocarbon multi-component gas mixture can be realized.
  • real-time measurement can be realized by using TDLAS.
  • the moisture spectrum in the air may become an obstacle to concentration detection, but by appropriately selecting the optical path lengths L1 to L3 of each part as shown in FIG. The influence of moisture in the air can be eliminated.
  • FIG. 6 is a block diagram showing another embodiment of the present invention, and the same reference numerals are given to portions common to FIG.
  • the distance from the center of the beam splitter 105 to the incident end face of the gas cell 106 is L1
  • the distance from the exit end face of the gas cell 106 to the incident face of the photodiode 108 is L2
  • the center of the beam splitter 105 is connected to the photodiode 110.
  • the distance to the incident surface is L3
  • the optical system as shown in FIG. 6 may be housed in the casing and purged with a gas that does not absorb in the infrared wavelength region such as nitrogen.
  • the light source a fiber output, it is possible to prevent the optical axis alignment from shifting due to the mounting or replacement of the wavelength tunable laser 101 which is the light source.
  • the CH 4 concentration is detected using the CH 4 peak, but the concentration detection method at this time is not limited to a statistical method, and an area method may be used.
  • a light branching means for branching the output light of the wavelength tunable laser into measurement light and reference light and irradiating the measurement gas with the measurement light, so that the data processing unit and reference signal related to the reference light
  • the reference signal is not used. Simple measurement is possible.
  • a tunable laser having a wide wavelength tunable width is used as a laser light source, and a statistical method is used for concentration detection by removing a sharp peak portion of a gas having a narrow spectral width such as methane. Therefore, it is possible to realize a laser gas analyzer that can measure hydrocarbons having large spectral characteristics and hydrocarbons having small spectral characteristics with high accuracy, and is effective for direct measurement of various process gases.

Abstract

La présente invention met en œuvre un dispositif d'analyse de gaz par laser capable de mesurer, avec une précision élevée, même un hydrocarbure ayant une caractéristique spectrale petite simultanément à un hydrocarbure ayant une caractéristique spectrale grande à l'aide d'un laser à longueur d'onde variable ayant une largeur de longueur d'onde variable large en tant que source de lumière laser et utilisant un procédé statistique dans lequel une partie pic élevée de méthane est éliminée dans une détection de concentration. Un dispositif d'analyse de gaz par laser est équipé de : un laser à longueur d'onde variable qui a une largeur de longueur d'onde variable large ; un moyen d'irradiation de lumière qui irradie un gaz à mesurer avec une lumière de sortie provenant du laser à longueur d'onde variable en tant que lumière de mesure ; et une unité de traitement de données qui, sur la base d'un signal d'absorption associé à la lumière de mesure émise à travers le gaz à mesurer, trouve le spectre d'absorption du gaz à mesurer et trouve la concentration de chaque composant par un procédé statistique. Le dispositif d'analyse de gaz par laser est caractérisé par le fait que l'unité de traitement de données utilise, parmi des spectres d'absorption obtenus par balayage d'une plage de longueur d'onde relativement large, un spectre d'absorption dans une région de longueur d'onde dans laquelle les pics d'absorption élevée d'autres composants de gaz ne sont pas présents lorsqu'une concentration de composant de gaz qui n'a pas de pic d'absorption élevée est trouvée.
PCT/JP2014/050527 2013-01-16 2014-01-15 Dispositif d'analyse de gaz par laser WO2014112502A1 (fr)

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