WO2024095514A1 - フレーム式原子吸光光度計 - Google Patents

フレーム式原子吸光光度計 Download PDF

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Publication number
WO2024095514A1
WO2024095514A1 PCT/JP2023/020679 JP2023020679W WO2024095514A1 WO 2024095514 A1 WO2024095514 A1 WO 2024095514A1 JP 2023020679 W JP2023020679 W JP 2023020679W WO 2024095514 A1 WO2024095514 A1 WO 2024095514A1
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Prior art keywords
flame
light
burner
unit
atomic absorption
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
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PCT/JP2023/020679
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English (en)
French (fr)
Japanese (ja)
Inventor
信之 岩井
智光 小林
琢也 木本
央祐 小林
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Shimadzu Corp
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Shimadzu Corp
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Priority to JP2024554107A priority Critical patent/JPWO2024095514A1/ja
Priority to CN202380055923.4A priority patent/CN119604752A/zh
Priority to US19/123,205 priority patent/US20260086025A1/en
Publication of WO2024095514A1 publication Critical patent/WO2024095514A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • G01N21/35—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
    • 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
    • G01N33/0011—Sample conditioning
    • G01N33/0013—Sample conditioning by a chemical reaction
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23N—REGULATING OR CONTROLLING COMBUSTION
    • F23N5/00—Systems for controlling combustion
    • F23N5/02—Systems for controlling combustion using devices responsive to thermal changes or to thermal expansion of a medium
    • F23N5/08—Systems for controlling combustion using devices responsive to thermal changes or to thermal expansion of a medium using light-sensitive elements
    • 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
    • G01J3/02—Details
    • G01J3/027—Control of working procedures of a spectrometer; Failure detection; Bandwidth calculation
    • 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
    • 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
    • G01N21/3103—Atomic absorption analysis
    • 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
    • G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • 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
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners

Definitions

  • the present invention relates to a flame-type atomic absorption spectrophotometer.
  • a sample liquid atomized by a nebulizer is mixed with combustion gas in a chamber, and the mixed gas is then burned while being blown out of a slit opening in the burner head, forming a flame.
  • the components in the sample are atomized in this flame, and when light is shone on the flame containing the atomized sample components, only light of a specific wavelength corresponding to the type of atom (element) is absorbed. Therefore, by measuring the absorption of light by the sample atoms, the elements in the sample can be identified and quantified.
  • the combustion gas for forming the flame is usually a mixture of a fuel gas consisting of a hydrocarbon such as acetylene ( C2H2 ) and a combustion supporting gas consisting of air or nitrous oxide ( N2O ).
  • a fuel gas consisting of a hydrocarbon such as acetylene ( C2H2 )
  • a combustion supporting gas consisting of air or nitrous oxide ( N2O ).
  • some conventional flame-type atomic absorption spectrophotometers have a light sensor installed near the flame to constantly monitor the intensity of the light (flame light) emitted by the flame, and are equipped with a function that automatically extinguishes the flame and stops the supply of combustion gas when the intensity falls below the amount of light that occurs during normal combustion (see, for example, Patent Document 1).
  • soot is generated and accumulates on the burner head. This soot can cause the flame to become unstable, so it needs to be properly removed.
  • the present invention has been made in consideration of these points, and its purpose is to enable a flame type atomic absorption spectrometer to accurately detect abnormalities related to the stability of the flame combustion state. More specifically, the first purpose is to provide a flame type atomic absorption spectrometer that can reliably determine whether the flame is continuing to burn normally. The second purpose is to enable a flame type atomic absorption spectrometer to detect flashback before it occurs. The third purpose is to enable a flame type atomic absorption spectrometer to reliably detect the occurrence of incomplete combustion. The fourth purpose is to enable a user to reliably grasp the accumulation status of soot on the burner head in a flame type atomic absorption spectrometer.
  • the present invention provides a flame type atomic absorption spectrophotometer according to a first aspect thereof, which comprises: a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame; A flame light detection unit that detects light emitted from the flame; a flame extinguishing determination unit that determines that the flame has been extinguished when the intensity of the light detected by the flame light detection unit is lower than a predetermined threshold value; having The flame light detection section selectively detects light having a wavelength of 290 nm or more and 330 nm or less.
  • a flame type atomic absorption spectrophotometer comprises: a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame; A flame light detection unit that detects light emitted from the flame and selectively detects light having a wavelength of 290 nm or more and 330 nm or less; A Swan band light detection unit that selectively detects C2 Swan band light from the light emitted from the flame; a flashback symptom determination unit that determines that there is a flashback symptom when a ratio of the intensity of the light detected by the Swan band light detection unit to the intensity of the light detected by the flame light detection unit falls below a predetermined threshold; It has the following.
  • a flame type atomic absorption spectrophotometer which has been made to solve the above problems, comprises: a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame; A flame light detection unit that detects light emitted from the flame and selectively detects light having a wavelength of 290 nm or more and 330 nm or less; A luminous flame detection unit that selectively detects light having a wavelength of 800 nm or more and 1100 nm or less from the light emitted from the flame; an incomplete combustion determination unit that determines that incomplete combustion is occurring when a ratio of the intensity of the light detected by the luminous flame detection unit to the intensity of the light detected by the flame light detection unit exceeds a predetermined threshold value; It has the following.
  • a flame type atomic absorption spectrophotometer which has been made to solve the above problems, comprises: a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame; A flame light detection unit that detects light emitted from the flame and selectively detects light having a wavelength of 290 nm or more and 330 nm or less; A bandpass filter that selectively transmits light having a wavelength of 800 nm or more and 1100 nm or less; an image sensor having a plurality of photodetection elements arranged two-dimensionally and configured to receive light emitted from the burner and passing through the bandpass filter; a soot accumulation determination unit that obtains a ratio of the intensity of light detected by each of the plurality of light detection elements to the intensity of light detected by the flame light detection unit, and determines that soot has accumulated on the burner when a predetermined number or more of the plurality of light detection elements have the ratio exceeding
  • the flame-type atomic absorption spectrophotometer according to the first aspect above makes it possible to reliably determine whether the flame is continuing to burn normally.
  • the flame-type atomic absorption spectrophotometer according to the second aspect above makes it possible to detect flashbacks before they occur.
  • the flame-type atomic absorption spectrophotometer according to the third aspect above makes it possible to reliably detect the occurrence of incomplete combustion.
  • the flame-type atomic absorption spectrophotometer according to the fourth aspect above makes it possible for the user to reliably grasp the soot accumulation status. Therefore, the flame-type atomic absorption spectrophotometers according to the first to fourth aspects above make it possible to accurately detect abnormalities related to the stability of the flame combustion state.
  • FIG. 1 is a diagram showing the configuration of a main part of a flame type atomic absorption photometer according to a first embodiment of the present invention
  • FIG. 5 is a diagram showing the configuration of the main parts of a flame type atomic absorption spectrometer according to a second embodiment of the present invention
  • FIG. 13 is a diagram showing the configuration of the main parts of a flame type atomic absorption spectrometer according to a third embodiment of the present invention.
  • FIG. 13 is a diagram showing the configuration of the main parts of a flame type atomic absorption photometer according to a fourth embodiment of the present invention.
  • FIG. 13 is a diagram showing the configuration of the main parts of a flame type atomic absorption photometer according to a fifth embodiment of the present invention.
  • FIG. 1 is a configuration diagram of the main parts of the flame type atomic absorption spectrometer according to this embodiment.
  • This flame type atomic absorption spectrometer includes a burner 110, a gas supply unit 120, a sample supply unit 130, a light source 140, a spectroscopic unit 150, and a control/processing unit 160.
  • the burner 110 is equipped with a nebulizer 111 that atomizes the sample liquid, a chamber 112 that mixes the atomized sample liquid with combustion gas, and a burner head 114 that forms a flame 113 by blowing the mixed gas upward and burning it.
  • the burner 110 is also provided with an ignition unit (not shown) that ignites the gas.
  • a mixed gas of acetylene as a fuel gas and air or nitrous oxide as a combustion supporting gas is supplied to the chamber 112 from a gas supply unit 120 as a combustion gas.
  • the gas supply unit 120 includes a fuel gas supply pipe 122 that guides fuel gas from a fuel gas source 121, such as a gas cylinder, to the burner 110, a fuel gas pipe opening/closing valve 123 and a fuel gas flow rate control valve 124 provided on the fuel gas supply pipe 122, a supporting gas supply pipe 126 that guides supporting gas from a supporting gas source 125, such as a gas cylinder or air compressor, to the burner 110, a supporting gas pipe opening/closing valve 127 and a supporting gas flow rate control valve 128 provided on the supporting gas supply pipe 126, and a valve drive unit 129 that drives these valves 123, 124, 127, and 128.
  • a fuel gas supply pipe 122 that guides fuel gas from a fuel gas source 121, such as a gas cylinder, to the burner 110
  • a fuel gas pipe opening/closing valve 123 and a fuel gas flow rate control valve 124 provided on the fuel gas supply pipe 122
  • a supporting gas supply pipe 126 that guides supporting
  • the light source 140 is disposed to the side of the region where the frame 113 is formed (hereinafter referred to as the frame forming region).
  • the spectroscopic unit 150 includes a spectrometer 151 and a photodetector 152, and is disposed in a position facing the light source 140 across the frame forming region.
  • the light source 140 emits light having an emission line spectrum including the resonance line of the target element, and this light passes through the atomic vapor in the frame forming region.
  • the light that passes through the atomic vapor is dispersed by the spectrometer 151, and light of a specific wavelength corresponding to the emission line (usually the resonance line) with the highest absorption by the target element is extracted.
  • This light of the specific wavelength is introduced into the photodetector 152, which outputs a detection signal according to the amount of incident light.
  • the detection signal is amplified by an amplifier (not shown) and converted into a digital signal by an A/D converter (not shown) and input to the control/processing unit 160.
  • the analysis data processing unit 161 which is a functional block provided in the control/processing unit 160, calculates the absorbance for the specific wavelength light based on this digital signal, and performs a predetermined arithmetic processing to perform quantitative analysis.
  • the control/processing unit 160 is mainly composed of a computer including a CPU and memory, and performs various calculation processes and outputs control signals for controlling the operation of each of the above-mentioned units.
  • the control/processing unit 160 has a flame-out determination unit 162, a gas supply control unit 163, and a display control unit 164 as functional blocks.
  • an operation unit 171 such as a keyboard and a display unit 172 such as a liquid crystal display are connected to the control/processing unit 160, and instructions from the user are input to the control/processing unit 160 via the operation unit 171, and analysis results, etc. are displayed on the display unit 172.
  • an OH-derived light detection optical sensor 182 which is an optical sensor for detecting light derived from OH radicals (hereinafter simply referred to as OH) in the frame 113, is disposed near the frame forming region, and an OH-derived light transmission bandpass filter 181, which is a bandpass filter that selectively transmits light having a wavelength of around 310 nm, is disposed between the OH-derived light detection optical sensor 182 and the frame forming region (the OH-derived light transmission bandpass filter 181 and the OH-derived light detection optical sensor 182 correspond to the flame light detection section in the present invention).
  • the OH-derived light detection optical sensor 182 receives light from the entire frame 113, but it may also receive light from only a part of the frame 113.
  • the optical sensor 182 for detecting OH-derived light is disposed diagonally above the frame 113, but the position of the optical sensor 182 for detecting OH-derived light is not limited to this (the same applies to the following embodiments 2 to 5).
  • a phototransistor can be suitably used, but it is not limited thereto, and any type of sensor, such as a photodiode, a phototube, or a photomultiplier tube, can be used.
  • the combustion flame of a hydrocarbon such as acetylene contains an emission spectrum derived from OH.
  • the emission spectrum derived from OH exists in a plurality of regions in the ultraviolet range, but the band spectrum in the above-mentioned 310 nm band (3064 ⁇ System) has a high intensity, a high transmittance of an optical element, and a high detection sensitivity by a general optical sensor.
  • ambient light such as sunlight, incandescent lamp, fluorescent lamp, or white LED, which is disturbance light, all has a low intensity in the 310 nm band.
  • the OH-derived light transmission bandpass filter 181 that selectively passes light having a wavelength of about 310 nm as described above is provided in front of the OH-derived light detection optical sensor 182, thereby preventing the OH-derived light detection optical sensor 182 from being affected by disturbance light.
  • the light emitted from the frame 113 and passing through the OH-derived light transmitting bandpass filter 181 is incident on the OH-derived light detecting optical sensor 182, and a detection signal corresponding to the amount of incident light is output from the OH-derived light detecting optical sensor 182.
  • This detection signal is amplified by an amplifier (not shown) and converted into a digital signal by an A/D converter (not shown) and input to the extinction determination unit 162.
  • the extinction determination unit 162 compares the intensity of this digital signal with a predetermined threshold T1 , and determines that extinction of the frame 113 has occurred if the digital signal is below the threshold T1 .
  • the threshold T1 may be set before the device is delivered to the user or at the installation stage of the device, or may be set by the user.
  • the gas supply control unit 163 controls the valve drive unit 129 to close the fuel gas pipe opening/closing valve 123 and the auxiliary gas pipe opening/closing valve 127.
  • the display control unit 164 controls the display unit 172 to display a predetermined message on its screen, thereby notifying the user that the gas supply has been stopped due to the flame going out.
  • a message notifying the user that the flame of the frame 113 has gone out may be displayed on the screen of the display unit 172 before or at the same time as the fuel gas pipe opening/closing valve 123 and the auxiliary gas pipe opening/closing valve 127 are closed.
  • such a notification may not be given and only the fuel gas pipe opening/closing valve 123 and the auxiliary gas pipe opening/closing valve 127 may be closed.
  • a configuration may be used in which only a notification that the flame of the frame 113 has gone out is given without closing the fuel gas pipe opening/closing valve 123 and the auxiliary gas pipe opening/closing valve 127.
  • Fig. 2 is a block diagram of the main parts of the flame type atomic absorption spectrometer according to this embodiment. Note that in this embodiment, components that are the same as or correspond to those shown in Fig. 1 are given reference numerals with the same last two digits, and descriptions thereof will be omitted as appropriate.
  • the flame type atomic absorption spectrophotometer according to this embodiment has the same configuration as the flame type absorption spectrophotometer according to the first embodiment, and further includes a bandpass filter 283 for transmitting C2 origin light and an optical sensor 284 for detecting C2 origin light provided in the vicinity of the frame formation region, and a flashback symptom determination unit 265 which is a functional block provided in the control/processing unit 260.
  • the bandpass filter 283 for transmitting C2 origin light and the optical sensor 284 for detecting C2 origin light correspond to the Swan band light detection unit in the present invention.
  • the gas supply control unit 263 corresponds to the flashback avoidance unit in the present invention.
  • the ratio of the flow rate of the supporting gas to the flow rate of the fuel gas i.e., the air-fuel ratio
  • the theoretical air-fuel ratio the air-fuel ratio when the supporting gas in the combustion gas reacts with the fuel gas in an adequate amount to maximize the combustion speed.
  • this air-fuel ratio approaches the theoretical air-fuel ratio for some reason, the combustion reaction is promoted, and the area of the outer flame in the flame 213 where the emission spectrum originating from OH is prominent expands, while the area of the inner flame including the emission spectrum originating from C 2 (diatomic carbon) in the reaction transition process decreases.
  • the flame-type atomic absorption spectrophotometer of this embodiment has the function of detecting the light from the outer flame and the light from the inner flame separately and detecting signs of flashback based on the intensity ratio between the two.
  • the band spectrum of the C2 Swan System is known.
  • the bandpass filter 283 for transmitting C2 - origin light in this embodiment selectively transmits light in the wavelength band of the band spectrum of the C2 Swan System.
  • the C2 Swan System has a plurality of spectral bands in the visible light region, and emission around 517 nm is particularly prominent. Therefore, it is preferable that the bandpass filter 283 for transmitting C2- origin light in this embodiment selectively transmits light with a wavelength of 507 nm to 527 nm (preferably 512 nm to 522 nm).
  • the transmission wavelength range of the bandpass filter 283 for transmitting C2 -origin light is not limited to this, and it may selectively transmit light in the wavelength range of other band spectra included in the C2 Swan System, that is, 464 nm to 484 nm (preferably 469 nm to 479 nm) or 554 nm to 574 nm (preferably 559 nm to 569 nm).
  • the C2 -origin light detection optical sensor 284 is a sensor that detects light emitted from the frame 213 and passed through the C2- origin light transmission bandpass filter 283.
  • a phototransistor can be suitably used, but is not limited thereto, and any other type such as a photodiode, a phototube, or a photomultiplier tube may be used.
  • the C2- origin light detection optical sensor 284 may receive light from the entire frame 213, but it is most effective to receive only light from the lower region of the frame 213 where C2 is localized.
  • the C2 -origin light detection optical sensor 284 is disposed obliquely above the frame 213 for convenience of drawing, but the position at which the C2- origin light detection optical sensor 284 is provided is not limited thereto.
  • the light emitted from the flame 213 and passing through the bandpass filter 283 for transmitting C2 origin light is incident on the optical sensor 284 for detecting C2 origin light, and a detection signal corresponding to the amount of incident light is output from the optical sensor 284 for detecting C2 origin light.
  • This detection signal is amplified by an amplifier (not shown) and converted into a digital signal by an A/D converter (not shown) and input to the flashback symptom determination unit 265 (this signal is hereinafter referred to as the " C2 origin light detection signal").
  • the detection signal from the optical sensor 282 for detecting OH origin light is amplified and digitally converted in the same manner as in the first embodiment, and then input to the control/processing unit 260 (this signal is hereinafter referred to as the "OH origin light detection signal").
  • This OH origin light detection signal is input to the flame-out determination unit 262 as in the first embodiment to determine whether or not the flame 213 has been extinguished, and is also input to the flashback symptom determination unit 265.
  • the flashback symptom determination unit 265 divides the intensity of the C2 origin light detection signal by the intensity of the OH origin light detection signal (i.e., calculates the ratio of the C2 origin light detection signal to the OH origin light detection signal) and compares the result with a predetermined threshold T2 . If the value obtained by dividing the intensity of the C2 origin light detection signal by the intensity of the OH origin light detection signal is below the threshold T2 , it is determined that there is a flashback symptom.
  • the threshold T2 may be set before the device is delivered to the user or at the installation stage of the device, or may be set by the user.
  • the gas supply control unit 263 controls the valve drive unit 229 to reduce the air-fuel ratio in the combustion gas supplied to the burner 210. Specifically, until the flashback symptom determination unit 265 determines that there is no symptom of flashback (i.e., until it determines that the ratio of the C2 origin light detection signal to the OH origin light detection signal is equal to or greater than the threshold value T2 ), the opening of the fuel gas flow rate control valve 224 is gradually increased, or the opening of the supporting gas flow rate control valve 228 is gradually decreased, or both are performed.
  • the display control unit 264 controls the display unit 272 to display a predetermined message on its screen, thereby notifying the user that the gas flow rate has been adjusted due to signs of flashback.
  • a message notifying the user that there are signs of flashback may be displayed on the screen of the display unit 272 simultaneously with or before the gas flow rate adjustment.
  • only the gas flow rate may be adjusted without such a notification.
  • a configuration may be adopted in which only a notification that there are signs of flashback is given without adjusting the gas flow rate.
  • a mechanism may be provided that reduces the combustion rate of the flame 213 by reintroducing exhaust gas from the burner 210 into the burner 210.
  • a flame-type atomic absorption spectrophotometer equipped with such a mechanism (a flame-type atomic absorption spectrophotometer according to a third embodiment of the present invention) is described below.
  • FIG. 3 is a diagram showing the main configuration of a flame-type atomic absorption spectrophotometer according to a third embodiment of the present invention.
  • components that are the same as or correspond to those shown in the first or second embodiment are given reference numerals with the same last two digits, and the description thereof will be omitted as appropriate.
  • the flame type atomic absorption spectrophotometer according to this embodiment has the same configuration as the flame type absorption spectrophotometer according to the second embodiment, and further includes an exhaust reintroduction pipe 315 for returning a portion of the exhaust gas generated from the burner 310 to the burner 310, an opening/closing valve (hereinafter referred to as the exhaust opening/closing valve 316) and a flow rate control valve (hereinafter referred to as the exhaust flow rate control valve 317) provided on the exhaust reintroduction pipe 315, an exhaust valve drive unit 318 that drives these valves 316, 317, and an exhaust reintroduction control unit 366 which is a functional block provided in the control/processing unit 360 and controls the exhaust valve drive unit 318.
  • an exhaust reintroduction pipe 315 for returning a portion of the exhaust gas generated from the burner 310 to the burner 310
  • an opening/closing valve hereinafter referred to as the exhaust opening/closing valve 316
  • a flow rate control valve
  • the exhaust reintroduction pipe 315, the exhaust opening/closing valve 316, the exhaust flow rate control valve 317, the exhaust valve drive unit 318, and the exhaust reintroduction control unit 366 correspond to the exhaust introduction unit in this invention.
  • the exhaust reintroduction pipe 315 is a pipe branched off from an exhaust pipe 391 for discharging exhaust from the burner chamber 390 housing the burner 310 to the outside, and its tip is connected to the chamber 312 of the burner 310.
  • the burner chamber 390 and the exhaust pipe 391 are also provided in the flame-type atomic absorption spectrophotometers according to the first and second embodiments, but are not shown in these embodiments for the sake of simplicity (the same applies to the fourth and fifth embodiments described below).
  • the exhaust reintroduction control unit 366 controls the exhaust valve drive unit 318 to recirculate the exhaust gas generated in the burner 310 to the chamber 312 of the burner 310. Specifically, when it is determined that there is a symptom of flashback, first the exhaust opening/closing valve 316 is opened, and further the opening of the exhaust flow rate control valve 317 is gradually increased until the flashback symptom determination unit 365 determines that there is no longer a symptom of flashback. This reduces the burning speed of the flame 313, making it possible to avoid the occurrence of flashback.
  • the flow rate of the combustion supporting gas and/or fuel gas may be adjusted in the same manner as in embodiment 2.
  • the method of determining flashback symptoms and the method of adjusting the flow rate of the combustion supporting gas and/or fuel gas in this embodiment are the same as in embodiment 2, so a description thereof will be omitted here.
  • Fig. 4 is a configuration diagram of the main parts of the flame type atomic absorption spectrometer according to this embodiment. Note that in this embodiment, components that are the same as or correspond to those shown in the first embodiment are given reference numerals with the same last two digits, and the description thereof will be omitted as appropriate.
  • the flame type atomic absorption spectrophotometer according to this embodiment has the same configuration as the flame type absorption spectrophotometer according to the first embodiment, and further includes a luminous flame light transmitting bandpass filter 485 and a luminous flame light detecting optical sensor 486 provided near the frame forming region, and an incomplete combustion determination section 467 which is a functional block provided in the control/processing section 460.
  • the luminous flame light transmitting bandpass filter 485 and the luminous flame light detecting optical sensor 486 correspond to the luminous flame detection section in the present invention.
  • the gas supply control section 463 corresponds to the incomplete combustion elimination section in the present invention.
  • the bright flame light transmitting bandpass filter 485 is a bandpass filter that selectively transmits light (bright flame) emitted from soot in the frame 413, and specifically, selectively transmits all or part of the wavelength range of 800 nm to 1100 nm.
  • the bright flame light detecting optical sensor 486 is a sensor that detects light emitted from the frame 413 and passed through the bright flame light transmitting bandpass filter 485.
  • a phototransistor can be suitably used as the bright flame light detecting optical sensor 486, but this is not limited thereto, and any type of sensor such as a photodiode, a phototube, or a photomultiplier tube can be used.
  • the bright flame light detecting optical sensor 486 receives light from the entire frame 413, but it may also receive light from only a part of the frame 413.
  • the bright flame detection optical sensor 486 is placed diagonally above the frame 413, but the location of the bright flame detection optical sensor 486 is not limited to this.
  • the luminous flame which is light emitted from soot heated to high temperatures, is a continuous spectrum that is highly luminous and thermally balanced.
  • the continuous spectrum generated from soot at the temperature of the flame 413 (up to 3000K) has almost no energy in the 310 nm band where the above-mentioned OH emits light.
  • the OH-derived light detection optical sensor 482 which is equipped with an OH-derived light transmission bandpass filter 481 that selectively transmits the 310 nm band, is not affected by the luminous flame and can monitor whether the flame 413 is continuing to burn.
  • the light emitted from the flame 413 and passing through the luminous flame light transmission bandpass filter 485 is incident on the luminous flame light detection optical sensor 486, and a detection signal corresponding to the amount of incident light is output from the luminous flame light detection optical sensor 486.
  • This detection signal is amplified by an amplifier (not shown) and converted into a digital signal by an A/D converter (not shown) and input to the incomplete combustion determination unit 467 (this signal is hereinafter referred to as the "luminous flame detection signal").
  • the detection signal from the OH-derived light detection optical sensor 482 is amplified and digitally converted as in the first embodiment, and then input to the control/processing unit 460 (this signal is hereinafter referred to as the "OH-derived light detection signal").
  • This OH-derived light detection signal is input to the extinction determination unit 462 as in the first embodiment to determine whether or not the flame 413 has been extinguished, and is also input to the incomplete combustion determination unit 467.
  • the incomplete combustion determination unit 467 divides the intensity of the luminous flame detection signal by the intensity of the OH-derived light detection signal (i.e., calculates the ratio of the luminous flame detection signal to the OH-derived light detection signal) and compares the value with a predetermined threshold T4 . If the value obtained by dividing the intensity of the luminous flame detection signal by the intensity of the OH-derived light detection signal exceeds the threshold T4 , it is determined that incomplete combustion is occurring in the burner 410.
  • the threshold T4 may be set before the device is delivered to the user or at the installation stage of the device, or may be set by the user. In this way, by determining whether incomplete combustion is occurring based on the ratio of the luminous flame detection signal to the OH-derived light detection signal, it is possible to cancel the change in the intensity of the luminous flame light due to the fluctuation of the flame 413 and perform an accurate determination.
  • the gas supply control unit 463 controls the valve drive unit 429 to increase the air-fuel ratio in the combustion gas supplied to the burner 410. Specifically, the opening of the fuel gas flow rate control valve 424 is gradually decreased, the opening of the supporting gas flow rate control valve 428 is gradually increased, or both are performed, until the incomplete combustion determination unit 467 determines that incomplete combustion is not occurring (i.e., until it is determined that the ratio of the luminous flame detection signal to the OH-derived light detection signal is equal to or less than the threshold value).
  • the display control unit 464 controls the display unit 472 to display a predetermined message on its screen, thereby notifying the user that the gas flow rate has been adjusted due to the occurrence of incomplete combustion.
  • a message notifying the user that incomplete combustion has occurred may be displayed on the screen of the display unit 472 simultaneously with or before the gas flow rate adjustment.
  • only the gas flow rate may be adjusted without such a notification.
  • a configuration may be adopted in which only a notification that incomplete combustion has occurred is given without adjusting the gas flow rate.
  • FIG. 5 is a block diagram of the main parts of the flame type atomic absorption spectrometer according to this embodiment. Note that in this embodiment, components that are the same as or correspond to those shown in the first embodiment are given reference numerals with the same last two digits, and the description thereof will be omitted as appropriate.
  • the flame-type atomic absorption spectrophotometer according to this embodiment has the same configuration as the flame-type absorption spectrophotometer according to the first embodiment, and further includes a burner head imaging unit 588 that images the burner head 514, a bandpass filter 587 for transmitting luminous flame light that is disposed between the burner head imaging unit 588 and the burner head 514, and a soot accumulation determination unit 568, which is a functional block provided in the control/processing unit 560.
  • the flame-type atomic absorption spectrophotometer has the function of monitoring the soot accumulation state on the burner head 514.
  • the burner head photographing unit 588 is an image sensor equipped with a plurality of photodetection elements arranged in a two-dimensional matrix.
  • the burner head photographing unit 588 is preferably arranged so that it can photograph the entire burner head 514, but it is not limited to this, and it may be arranged so that it can photograph only the periphery of the slit opening where soot is likely to accumulate. Note that in FIG. 5, the burner head photographing unit 588 is arranged diagonally above the frame 513 for convenience of drawing, but the position of the burner head photographing unit 588 is not limited to this.
  • the luminous flame light transmitting bandpass filter 587 is a bandpass filter that selectively transmits light (luminous flame) emitted from soot heated to a high temperature, and selectively transmits light in the same wavelength range as the luminous flame light transmitting bandpass filter 485 in embodiment 4.
  • the detection signals from the light detection elements of the burner head imaging unit 588 are amplified by an amplifier (not shown) and converted into digital signals by an A/D converter (not shown), and then input to the soot deposition determination unit 568 of the control/processing unit 560.
  • the detection signal from the OH-derived light detection optical sensor 582 is amplified and digitally converted as in the first embodiment, and then input to the control/processing unit 560 (this signal is hereinafter referred to as the "OH-derived light detection signal").
  • this OH-derived light detection signal is input to the extinction determination unit 562 to determine whether or not the frame 513 has been extinguished, and is also input to the soot deposition determination unit 568.
  • the soot deposition determination unit 568 divides the intensity of the detection signal from each of the light detection elements by the intensity of the OH-derived light detection signal (i.e., obtains the ratio of the detection signal from each light detection element to the intensity of the OH-derived light detection signal), and compares the value with a predetermined threshold T5 .
  • the threshold value T5 and the predetermined number N may be set before the device is delivered to the user or at the installation stage of the device, or may be set by the user.
  • the soot accumulation determining unit 568 determines that soot is accumulated on the burner head 514. In this way, by determining the accumulation of soot based on the ratio of the detection signal from each light detection element to the intensity of the OH-origin light detection signal, it is possible to cancel the change in the intensity of the luminous flame light due to the fluctuation of the flame 513 and perform an accurate determination.
  • the display control unit 564 controls the display unit 572 to display a predetermined message on the screen, thereby notifying the user that soot has accumulated on the burner head 514.
  • the display control unit 564 and the display unit 572 correspond to the notification unit in the present invention.
  • an image showing the area where soot has accumulated on the burner head 514 may be displayed on the screen of the display unit 572.
  • the soot accumulation determination unit 568 identifies one or more photodetection elements among the multiple photodetection elements whose detection signal divided by the OH-derived light detection signal exceeds the threshold value T5 , and identifies the radiation position of the luminous flame on the burner head 514 (i.e., the position where soot has accumulated) based on the position of the photodetection element on the burner head imaging unit 588.
  • the soot accumulation determination unit 568, the display control unit 564, and the display unit 572 correspond to the soot accumulation area presentation unit in the present invention.
  • the flame-type atomic absorption spectrophotometer after lighting the flame 113, always monitors whether there is any abnormality related to the stability of the combustion state of the flame, such as the flame 113 going out, signs of flashback, incomplete combustion, or soot accumulation, and notifies the user when it determines that there is an abnormality.
  • it may be configured to determine whether the abnormality has occurred at a timing specified by the user or a preset timing, and notify the user of the determination result regardless of the result.
  • a bandpass filter i.e., the bandpass filter 181, 281, 381, 481 for transmitting OH-derived light, the bandpass filter 283, 383 for transmitting C2- derived light, or the bandpass filter 485 for transmitting luminous flame light
  • an optical sensor for detecting light passing through the bandpass filter i.e., the optical sensor 182, 282, 382, 482 for detecting OH-derived light, and the optical sensor 284, 384 for detecting C2- derived light, or the optical sensor 486 for detecting luminous flame light
  • the spectroscopes 151, 251, 351, 451 and the optical detectors 152, 252, 352, 452 provided in the spectroscopic units 150, 250, 350, 450 may be made to serve the roles of the bandpass filter and the optical sensor.
  • a wavelength similar to the wavelength that passes through the above-mentioned OH-derived light transmitting bandpass filter 181, 281, 381, 481 is selected by the spectrometer 151, 251, 351, 451 and guided to the photodetector 152, 252, 352, 452, and the detection signal (OH-derived light detection signal) of the photodetector 152, 252, 352, 452 at that time is input to the flame-out determination unit 162, 262, 362, 462, thereby making it possible to determine whether combustion of the flame 113, 213, 313, 413 is being maintained (i.e., whether flame-out has occurred).
  • the spectrometers 251 and 351 select wavelengths similar to those transmitted through the bandpass filters 283 and 383 for transmitting C2 -derived light, and guide them to the photodetectors 252 and 352.
  • the detection signals ( C2- derived light detection signals) of the photodetectors 252 and 352 at this time and the OH-derived light detection signals are input to the flashback symptom determination units 265 and 365, so that it is possible to determine whether or not there is a flashback symptom.
  • the spectrometer 451 selects wavelengths similar to those transmitted through the bandpass filter 485 for transmitting luminous flame light, and guides them to the photodetector 452.
  • the detection signals (luminous flame detection signals) of the photodetector 452 at this time and the OH-derived light detection signals are input to the incomplete combustion determination unit 467, so that it is possible to determine whether or not incomplete combustion has occurred.
  • the light detection for determining the presence or absence of an abnormality as described above is performed at a timing different from that of the light detection for the sample analysis.
  • the flame-type atomic absorption spectrophotometers according to the second to fifth embodiments may not include the flame-out determination unit 162, 262, 362, 462, and may use the OH-derived light detection signal only to determine whether there are flashback symptoms, whether incomplete combustion has occurred, or whether soot has accumulated.
  • the flame type atomic absorption spectrophotometer according to the present invention may have two or more of a function for determining whether or not there are signs of flashback, a function for determining whether or not incomplete combustion is occurring, and a function for determining whether or not soot has accumulated.
  • the flame type atomic absorption photometer is a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame; A flame light detection unit that detects light emitted from the flame; a flame extinguishing determination unit that determines that the flame has been extinguished when the intensity of the light detected by the flame light detection unit is lower than a predetermined threshold value; having The flame light detection section selectively detects light having a wavelength of 290 nm or more and 330 nm or less.
  • the flame-type atomic absorption spectrophotometer according to paragraph 1 makes it possible to reliably determine whether a flame is continuing to burn normally without being affected by external light disturbances.
  • the flame type atomic absorption photometer is a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame;
  • a flame light detection unit that detects light emitted from the flame and selectively detects light having a wavelength of 290 nm or more and 330 nm or less;
  • a Swan band light detection unit that selectively detects C2 Swan band light from the light emitted from the flame;
  • a flashback symptom determination unit that determines that there is a flashback symptom when a ratio of the intensity of the light detected by the Swan band light detection unit to the intensity of the light detected by the flame light detection unit falls below a predetermined threshold; It has the following.
  • the flame-type atomic absorption spectrophotometer described in paragraph 2 makes it possible to detect flashback before it occurs.
  • the flame atomic absorption spectrophotometer according to the third aspect of the present invention is the flame atomic absorption spectrophotometer according to the second aspect of the present invention, further comprising: a gas supply unit that supplies the fuel gas and the combustion supporting gas to the burner; a flashback avoidance unit that controls the gas supply unit to reduce a ratio of a flow rate of the combustion supporting gas to a flow rate of the fuel gas when the flashback symptom determination unit determines that there is a flashback symptom; It has the following.
  • the flame atomic absorption spectrophotometer according to paragraph 4 is the flame atomic absorption spectrophotometer according to paragraph 2 or 3, further comprising: an exhaust gas introduction section that introduces a portion of exhaust gas generated from the burner into the burner when the flashback symptom determination section determines that there is a flashback symptom; It has the following.
  • the flame type atomic absorption photometer is a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame;
  • a flame light detection unit that detects light emitted from the flame and selectively detects light having a wavelength of 290 nm or more and 330 nm or less;
  • a luminous flame detection unit that selectively detects light having a wavelength of 800 nm or more and 1100 nm or less from the light emitted from the flame;
  • an incomplete combustion determination unit that determines that incomplete combustion is occurring when a ratio of the intensity of the light detected by the luminous flame detection unit to the intensity of the light detected by the flame light detection unit exceeds a predetermined threshold value; It has the following.
  • the flame atomic absorption spectrophotometer described in paragraph 5 makes it possible to reliably detect the occurrence of incomplete combustion.
  • the flame atomic absorption spectrophotometer according to the sixth aspect of the present invention is the flame atomic absorption spectrophotometer according to the fifth aspect of the present invention, further comprising: a gas supply unit that supplies the fuel gas and the combustion supporting gas to the burner; an incomplete combustion elimination unit that controls the gas supply unit so as to increase a ratio of a flow rate of the combustion supporting gas to a flow rate of the fuel gas when the incomplete combustion determination unit determines that incomplete combustion is occurring; It has the following.
  • the flame type atomic absorption photometer according to Clause 7 is a burner for burning a mixture of a fuel gas and a combustion supporting gas with the atomized sample liquid to form a flame;
  • a flame light detection unit that detects light emitted from the flame and selectively detects light having a wavelength of 290 nm or more and 330 nm or less;
  • a bandpass filter that selectively transmits light having a wavelength of 800 nm or more and 1100 nm or less; an image sensor having a plurality of photodetection elements arranged two-dimensionally and configured to receive light emitted from the burner and passing through the bandpass filter;
  • a soot accumulation determination unit that obtains a ratio of the intensity of light detected by each of the plurality of light detection elements to the intensity of light detected by the flame light detection unit, and determines that soot has accumulated on the burner when a predetermined number or more of the plurality of light detection elements have the ratio exceeding a predetermined threshold value;
  • a notification unit
  • the flame-type atomic absorption spectrophotometer described in paragraph 7 allows the user to reliably grasp the soot accumulation condition in the burner.
  • the flame atomic absorption spectrophotometer according to item 8 is the flame atomic absorption spectrophotometer according to item 7, further comprising: a soot accumulation region presenting unit that presents to a user, as a region where soot is accumulated, a region on the burner corresponding to one of the plurality of photodetection elements in which the ratio exceeds a predetermined threshold value; It has the following.
  • the flame-type atomic absorption spectrophotometer described in paragraph 8 allows the user to easily identify the area on the burner where soot has accumulated.

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