WO2018231065A1 - Procédé d'analyse chimique de mesure de tétrafluorométhane, cf4, à sélectivité améliorée - Google Patents

Procédé d'analyse chimique de mesure de tétrafluorométhane, cf4, à sélectivité améliorée Download PDF

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Publication number
WO2018231065A1
WO2018231065A1 PCT/NO2018/050153 NO2018050153W WO2018231065A1 WO 2018231065 A1 WO2018231065 A1 WO 2018231065A1 NO 2018050153 W NO2018050153 W NO 2018050153W WO 2018231065 A1 WO2018231065 A1 WO 2018231065A1
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concentration
gas
measurement
laser
gases
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PCT/NO2018/050153
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English (en)
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Peter Geiser
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Neo Monitors As
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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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G01J3/433—Modulation spectrometry; Derivative spectrometry
    • G01J3/4338—Frequency modulated spectrometry
    • 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
    • G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
    • G01N21/274—Calibration, base line adjustment, drift correction
    • 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
    • G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/0047—Organic compounds
    • G01N33/0049—Halogenated organic compounds
    • 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
    • G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
    • G01N2021/3148—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths using three or more wavelengths
    • 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
    • G01N2021/396—Type of laser source
    • G01N2021/399—Diode laser
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/12—Circuits of general importance; Signal processing
    • G01N2201/127—Calibration; base line adjustment; drift compensation
    • G01N2201/12746—Calibration values determination
    • G01N2201/12753—Calibration values determination and storage

Definitions

  • TDLS Spectroscopy
  • CF4 does not absorb in the near-infrared but displays a strong
  • instruments can be used on a gas cell evacuated and filled with process gas.
  • the process mass spectrometer provides a near real time measurement of both CF4 and C2F6, as well as several other gas sample components if desired. " The further description follows:
  • TDLAS is an infrared absorption technique that uses a diode laser to achieve a very narrow emission source bandwidth. As a result, the specificity of the technique is very good. The sensitivity is also excellent and the instrument is capable of direct measurement of both PFC gas components in electrolytic cell exhaust ducts. It has not been applied to fugitive gas measurements. Consequently, if fugitives are to be measured, laboratory analysis of collected time average samples, or open path methodology using FTIR techniques would provide a viable strategy.
  • the TDLAS unit as used for previous PFC measurements is relatively large. A mobile laboratory or trailer is needed to transport the instrument and ancillary sampling equipment from site to site. The equipment as used for past PFC measurements, is not broadly commercially available, is relatively expensive, is specialized and requires
  • the main objective with the current invention is to improve selectivity of a gas measurement method for the measurement of CF4 based on tuneable laser spectroscopy in presence of potential interfering gases like CH4, N20 and H20. It is an additional objective with the invention to be able to reduce the interference from these other gases also when the method is operated under normal ambient pressure as well as in-situ.
  • the at least one gas causing interference for the measurement of CF4 can be one of or any combination of methane (CH4), water vapour (H2O) and nitrous oxide (N2O).
  • the correction of the CF4 concentration can be based on subtraction of at least one absorption spectrum, the at least one absorption spectrum representing the spectrum of at least one gas causing interference for the measurement of CF4, subtracting this at least one other absorption spectrum after the detector signal has been acquired when the laser has been tuned across the spectral feature of CF4, the acquired detector signal representing an absorption spectrum of the target gas possibly comprising CF4 and other gases, subtracting the at least one absorption spectrum from the absorption spectrum of the target gas and finally determining the gas concentration of CF4 from the result of the subtraction of the spectra.
  • Figure 6 is similar to figure 5 but for wavelength modulation spectroscopy and second harmonic detection.
  • a sine wave is added to the laser current whenever the laser is on.
  • the laser current is shown.
  • the figure shows a current ramp (1000), an optional dark reference time slot (1 100) and short time slot (1 150) where the laser current is on and where the laser current is constant to allow the laser to stabilise after the dark reference.
  • Figure 6 is not to scale and is made to illustrate techniques. Description of reference signs
  • a preparatory step for determining the concentration levels of the interfering gases could be based on measurement of the levels of the concentration of the interfering gases as well as on their variations. The conclusion from such measurements could be that one or more interfering gases vary very little in concentration level and could be treated as constant possibly the year round or could be treated as constants within one season of the year where the ambient temperature and/or humidity is stable. Another conclusion could be that the concentration varies so much that the concentration of the interfering gases must be measured continuously to achieve sufficient correction of the measured CF4 concentration. The concentration of one or more of the interfering gases can be measured by the tuneable laser, the tuneable laser that scans across the CF4 spectroscopic feature (4100).
  • concentration information can be used either (1 ) to subtract predefined values proportional to the concentrations of the interfering gases (using a table as listed above), or (2) to prepare a background spectrum that is subtracted from the CF4 spectrum, or (3) is used as boundary conditions for advanced signal processing algorithms like Multivariate Analysis or similar methods.
  • the above procedure is applicable to DAS and WMS.
  • a look-up table must be generated and implemented into the signal- processing implementation prior to the actual CF4 measurements. This table includes information on the influence of the respective interference gas(es) on the CF4 concentration. These values are typically normalized to interference per 1 % or 1 ppm of the gas. Tables for different temperatures and pressures must be stored.
  • the recorded spectra during the application will be corrected for the interference by performing a point-to-point subtraction with a scaled interference spectrum.
  • the wavenumber range plotted in figure 1 is 1282-1284 cm-1 .
  • the CO2 absorption is weak in this region and the curve for the CO2 absorption (4050) overlaps the upper x-axis. This applies for figures 1 , 2, 3 and 4.
  • the figures 1 , 2, 3 and 4 covers part of the wavenumber region 1240 to1284 cm-1 .
  • the region is free of C02 interference.
  • Figure 4 shows the region where an interference free nitrous oxide (N20) line (4400) will be selected according to the first preferred embodiment. Wavenumber is shown on the X-axis and transmission is shown on the Y-axis. The wavenumber range for figure 4 is from 1273 to 1277 cm-1 . The preferred absorption line for measurement of N20 (4400) is indicated with an arrow.
  • Figure 5 shows several laser scan cycles for a gas analyser working with direct absorption technology. The laser current is shown. A current ramp (1000) scans the wavelength of the laser across at least one spectral absorption feature for a target gas to be measured. An optional dark reference (1 100) time slot follows where the laser current is off. A short time slot (1 150) where the laser current is on and where the laser current is constant to allow the laser to stabilise after the dark reference follows. Then a new laser scan ramp is performed for the next cycle. Figure 5 is not to scale.
  • the concentrations of interferents are determined applying typical DAS or WMS algorithms (including Multivariate Analysis).
  • a first preferred embodiment scans across the CF4 feature (4100) and measures the CF4 concentration, scans also across absorption features (4200, 4300, 4400) for 3 interfering gases using the tuneable laser to correct for the interference these 3 gases, CH4, H2O and N2O, impose on the measured CF4 concentration.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pathology (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
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  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Optics & Photonics (AREA)
  • Mathematical Physics (AREA)
  • Theoretical Computer Science (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne un procédé de mesure de la concentration de gaz CF4 à sensibilité réduite aux interférences provenant d'autres gaz. Le procédé consiste à pointer un laser réglable à travers un gaz cible, comprenant éventuellement du CF4 et d'autres gaz comprenant éventuellement au moins un gaz provoquant une interférence par rapport à la mesure de la concentration de gaz CF4, sur un détecteur sensible à la lumière, à acquérir et à numériser des signaux provenant du détecteur, le laser étant réglé sur une caractéristique d'absorption spectrale de CF4 (4100) autour de 1283 cm-1. Le procédé consiste en outre à corriger la concentration de gaz CF4 mesurée en fonction de données représentant une concentration desdits gaz provoquant une interférence pour la mesure de la concentration de CF4.
PCT/NO2018/050153 2017-06-16 2018-06-13 Procédé d'analyse chimique de mesure de tétrafluorométhane, cf4, à sélectivité améliorée WO2018231065A1 (fr)

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NO20170996A NO345903B1 (en) 2017-06-16 2017-06-16 Chemical analysis method for measurement of tetrafluoromethane, cf4, with improved selectivity
NO20170996 2017-06-16

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Cited By (4)

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CN112229818A (zh) * 2019-07-15 2021-01-15 光谱传感器公司 具有宽扫描可调谐二极管激光器的光谱仪
EP3957979A4 (fr) * 2019-05-15 2023-01-11 HORIBA, Ltd. Appareil d'analyse d'échantillon
CN117368424A (zh) * 2023-12-08 2024-01-09 广东立腾医疗科技有限公司 气体浓度检测补偿方法、装置、气体检测设备及存储介质
CN117740731A (zh) * 2024-02-08 2024-03-22 清华大学合肥公共安全研究院 甲烷气体浓度检测方法、存储介质和电子设备

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Publication number Priority date Publication date Assignee Title
EP3957979A4 (fr) * 2019-05-15 2023-01-11 HORIBA, Ltd. Appareil d'analyse d'échantillon
CN112229818A (zh) * 2019-07-15 2021-01-15 光谱传感器公司 具有宽扫描可调谐二极管激光器的光谱仪
EP3767278A1 (fr) * 2019-07-15 2021-01-20 SpectraSensors, Inc. Spectromètre à diode laser accordable à large balayage
CN117368424A (zh) * 2023-12-08 2024-01-09 广东立腾医疗科技有限公司 气体浓度检测补偿方法、装置、气体检测设备及存储介质
CN117368424B (zh) * 2023-12-08 2024-02-27 广东立腾医疗科技有限公司 气体浓度检测补偿方法、装置、气体检测设备及存储介质
CN117740731A (zh) * 2024-02-08 2024-03-22 清华大学合肥公共安全研究院 甲烷气体浓度检测方法、存储介质和电子设备

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