WO2021124937A1 - Dispositif d'analyse et système d'analyse - Google Patents

Dispositif d'analyse et système d'analyse Download PDF

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Publication number
WO2021124937A1
WO2021124937A1 PCT/JP2020/045320 JP2020045320W WO2021124937A1 WO 2021124937 A1 WO2021124937 A1 WO 2021124937A1 JP 2020045320 W JP2020045320 W JP 2020045320W WO 2021124937 A1 WO2021124937 A1 WO 2021124937A1
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WO
WIPO (PCT)
Prior art keywords
gas
unit
measurement target
analyzer
measurement
Prior art date
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PCT/JP2020/045320
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English (en)
Japanese (ja)
Inventor
山本　篤志
賢弥 長澤
岳 大塚
Original Assignee
株式会社堀場製作所
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Application filed by 株式会社堀場製作所 filed Critical 株式会社堀場製作所
Priority to JP2021565475A priority Critical patent/JPWO2021124937A1/ja
Priority to CN202090001011.0U priority patent/CN218524582U/zh
Publication of WO2021124937A1 publication Critical patent/WO2021124937A1/fr

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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
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/031—Multipass arrangements
    • 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

Definitions

  • the present invention relates to an analyzer and an analysis system for analyzing a measurement target gas contained in a sample gas.
  • an analyzer that irradiates a sample gas with measurement light and analyzes the measurement target gas based on the intensity of the measurement light absorbed by the measurement target gas contained in the sample gas.
  • the sample gas is filled in a predetermined cell, and the analysis is performed based on the intensity of the measurement light passing through the cell.
  • the ambient environment other than the inside of the cell is the gas to be measured and the gas that does not contain the gas that affects the measurement light (hereinafter referred to as "purge gas"). It is common to fill with.
  • the purge gas that does not contain the gas to be measured is supplied from, for example, a cylinder.
  • the reference gas is generated, for example, by passing air or the like through a substance capable of removing the gas to be measured.
  • a sample gas atmosphere
  • a carbon dioxide adsorbent such as zeolite
  • a substance that adsorbs a polar substance such as silica gel.
  • zeolite or silica gel when zeolite or silica gel is used as an adsorbent, it is necessary to provide a heating device such as a heater in order to remove the adsorbed components (carbon dioxide, moisture) from the zeolite or silica gel, and the device configuration is also complicated in this case as well.
  • a heating device such as a heater
  • An object of the present invention is to enable an analyzer that analyzes a gas to be measured to supply a gas that does not contain the gas to be measured, such as purge gas and reference gas, without increasing the burden on the user.
  • the analyzer is an apparatus for analyzing the gas to be measured.
  • the analyzer includes a filling unit, an irradiation unit, a propagation unit, and a measurement target removing unit.
  • the filling portion is filled with a sample gas containing the gas to be measured.
  • the irradiation unit irradiates the measurement light toward the filling unit.
  • the propagation portion is provided between the filling portion and the irradiation portion, and forms a propagation space in which the measurement light propagates.
  • the measurement target removing unit has a gas separation membrane that removes the measurement target gas from the gas and generates a purge gas for purging the propagation space.
  • a purge gas that purges the propagation space in which the measurement light propagates until it reaches the filling portion is generated by the measurement target removing portion having a gas separation membrane. This eliminates the need for work that increases the burden on the user, such as frequent replacement of cylinders for supplying purge gas. That is, the purge gas can be generated and supplied without increasing the burden on the user.
  • the analyzer further includes a detection unit and a first determination unit.
  • the detection unit detects the measurement light that has passed through the propagation space purged by the purge gas.
  • the first determination unit determines the deterioration of the measurement target removal unit based on the intensity of the measurement light absorbed by the measurement target gas and the gas that affects the measurement light by passing through the propagation space. Thereby, the deteriorated state of the measurement target removing portion can be easily determined by a method similar to the analysis of the measurement target gas.
  • the analyzer further comprises a second determination unit.
  • the second determination unit determines the deterioration of the measurement target removal unit based on the pressure or flow rate of the gas supplied to the measurement target removal unit. This makes it possible to determine whether or not deterioration (abnormality) has occurred due to "clogging" or the like that affects the pressure or flow rate of the gas supplied to the measurement target removing unit.
  • the analyzer is further equipped with a notification unit.
  • the notification unit notifies that the measurement target removal unit has been determined to be deteriorated. As a result, the user can be notified that the measurement target removing unit has deteriorated.
  • the analyzer is further equipped with a housing.
  • the housing houses the filling portion, the irradiation portion, and the propagation portion and isolates them from the external space.
  • the nitrogen gas separated from the gas is used as the purge gas.
  • nitrogen gas as a purge gas can be generated without increasing the burden on the user.
  • the gas to be measured is carbon dioxide (CO 2 ), carbon monoxide (CO), methane (CH 4 ), sulfur dioxide (SO 2 ), ammonia (NH 3 ), nitrogen oxide (NOx), hydrogen chloride (HCl). , Water (H 2 O), Ethan (C 2 H 6 ), Acetylene (C 2 H 2 ), Propane (C 3 H 8 ), Ethylene (C 2 H 4 ), Hexene (n-C 6 H 14 ), Propropylene (C 3 H 6 ), hydrogen sulfide (H 2 S), isobutene (i-C 4 H 8 ), methanol (CH 3 OH), phosgen (COCl 2 ), butane (n-C 4 H 10 ), chloro Ethylene (C 2 H 3 Cl), Methyl nitrite (CH 3 ONO), Cyclohexane (C 6 H 12 ), butadiene (C 4 H 6 ), Isobutan (i-C 4 H 10 ), Isopen
  • the analysis system includes the above-mentioned analysis device and a notification device for notifying information output from the analysis device. As a result, it is possible to realize a system in which the analyzer and the notification device for notifying information about the analyzer are separated.
  • the analyzer includes the intensity of the measurement light passing through the sample gas containing the measurement target gas, the intensity of the measurement light passing through the reference gas used as a reference for the analysis of the measurement target gas, and the intensity of the measurement light. It is a device that analyzes the gas to be measured based on.
  • the analyzer includes a filling unit, an irradiation unit, and a measurement target removing unit.
  • the filling portion is filled with a gas containing a sample gas or a reference gas.
  • the irradiation unit irradiates the measurement light toward the filling unit.
  • the measurement target removing unit has a gas separation membrane that separates the measurement target gas from the reference gas generation gas to generate the reference gas.
  • the measurement target removing unit has a gas separation membrane that separates the measurement target gas from the reference gas generation gas to generate the reference gas. Since this gas separation membrane can be used for a long period of time, it is not necessary to frequently replace the removal part to be measured. As a result, it is possible to prevent an increase in the burden on the user in the analysis of the gas to be measured.
  • the measurement target removing unit since the measurement target removing unit has a long life, it is not necessary for the analyzer to have a complicated configuration such as switching a plurality of gas lines to generate a reference gas, and the control of the analyzer can be simplified.
  • the analyzer is further equipped with an introduction unit.
  • the introduction section alternately introduces the sample gas and the reference gas into the filling section. This makes it possible to realize a cross-flow modulation type analyzer for the gas to be measured.
  • the reference gas generation gas is a sample gas. As a result, a more appropriate reference gas can be generated from the sample gas to be measured.
  • the reference gas generation gas is air supplied from a source different from the sample gas.
  • the condition of the reference gas generation gas supplied to the measurement target removal unit can be set to an appropriate condition that allows the performance of the measurement target removal unit to be fully exhibited.
  • the analyzer further includes a detection unit and a determination unit.
  • the detection unit detects the measurement light that has passed through the filling unit.
  • the determination unit determines the deterioration of the measurement target removal unit based on the intensity of the measurement light that has passed through the filling unit filled with the reference gas. Thereby, the deterioration state of the measurement target removing portion can be easily determined by a method similar to that of performing the measurement target gas based on the intensity of the measurement light passing through the gas filled in the filling portion.
  • the analyzer is further equipped with a notification unit.
  • the notification unit notifies that the measurement target removal unit has been determined to be deteriorated. As a result, the user can be notified that the measurement target removing unit has deteriorated.
  • the analyzer is further equipped with a scrubber that removes the measurement target gas from the gas that has passed through the measurement target removal unit. As a result, the life of the scrubber can be extended.
  • the gas to be measured is carbon dioxide (CO 2 ), carbon monoxide (CO), methane (CH 4 ), sulfur dioxide (SO 2 ), ammonia (NH 3 ), nitrogen oxide (NOx), hydrogen chloride (HCl). , Water (H 2 O), Ethan (C 2 H 6 ), Acetylene (C 2 H 2 ), Propane (C 3 H 8 ), Ethylene (C 2 H 4 ), Hexene (n-C 6 H 14 ), Propropylene (C 3 H 6 ), hydrogen sulfide (H 2 S), isobutene (i-C 4 H 8 ), methanol (CH 3 OH), phosgen (COCl 2 ), butane (n-C 4 H 10 ), chloro Ethylene (C 2 H 3 Cl), Methyl nitrite (CH 3 ONO), Cyclohexane (C 6 H 12 ), butadiene (C 4 H 6 ), Isobutan (i-C 4 H 10 ), Isopen
  • gas that does not contain the gas to be measured such as purge gas and reference gas, can be supplied without increasing the burden on the user.
  • FIG. 1 is a diagram showing a configuration of an analyzer according to the first embodiment.
  • the analyzer 100 is an apparatus for analyzing a gas to be measured contained in a sample gas SG such as an exhaust gas generated from a flue.
  • the measurement target gases that can be measured by the analyzer 100 are, for example, carbon dioxide (CO 2 ), carbon monoxide (CO), sulfur oxide (SOx) (for example, sulfur dioxide (SO 2 )) and ammonia (NH 3 ).
  • Nitrogen oxide (NOx) eg, nitrogen monoxide (NO), nitrogen dioxide (NO 2 ), acetylene oxide (N 2 O), etc.
  • hydrogen chloride (HCl) water (H 2 O), various hydrocarbons Hydrogen (eg, methane (CH 4 ), ethane (C 2 H 6 ), acetylene (C 2 H 2 ), propane (C 3 H 8 ), ethylene (C 2 H 4 ), hexane (n-C 6 H 14) ), Propylene (C 3 H 6 ), Isobutene (i-C 4 H 8 ), Butane (n-C 4 H 10 ), Propane (C 3 H 8 ), Cyclohexane (C 6 H 12 ), butadiene (C 4) H 6 ), isobutane (i-C 4 H 10 ), isopentan (i-C 5 H 12 ), toluene (C 6 H 5 CH 3 ), etc.), hydrogen sulfide (H 2 S),
  • the analyzer 100 has a structure in which the components for analyzing the gas to be measured can be separated from the external space, and the ambient environment of the analyzer 100 contains flammable gas. Even if there is, it is possible to measure the gas to be measured with high accuracy.
  • the analyzer 100 includes a housing 1, a filling unit 3, an irradiation unit 5, a propagation unit 7, a measurement target removal unit 9, and a control unit 20.
  • the housing 1 constitutes the main body of the analyzer 100, and houses the filling unit 3, the irradiation unit 5, and the propagation unit 7 in the internal space IS thereof. Further, an air supply line 11 is provided in the internal space IS of the housing 1. That is, in the present embodiment, the measurement target removing unit 9 generates purge gas from the air supplied from the air supply line 11.
  • the air supply line 11 is connected to the air supply unit 12, and the air AR supplied from the air supply unit 12 is introduced into the internal space IS of the housing 1.
  • the air supply unit 12 is, for example, a device provided at an installation location of the analyzer 100 and the like to supply instrumentation air to be used at the installation location.
  • the air supply unit 12 is a system including a compressor that compresses the air AR and various filters that remove dust, oil, and the like contained in the air AR. Further, the housing 1 is provided with a discharge port 13. The discharge port 13 discharges the air AR supplied from the air supply line 11 to the outside.
  • a pressure gauge PR1 may be provided at the outlet of the measurement target removing unit 9 (purge gas supply line 77 (described later)).
  • the pressure of the purge gas PG (that is, air AR) measured by the pressure gauge PR1 can be used, for example, to monitor the “clogging” of the measurement target removing unit 9.
  • a flow meter for measuring the flow rate of the purge gas PG that is, air AR
  • both the pressure gauge PR1 and the above flowmeter may be provided at the outlet of the measurement target removing unit 9.
  • At least one of the pressure gauge PR1 and the flow meter may be provided in the propagation space TS.
  • at least one of the pressure gauge PR1 and the flow meter may be provided in the air supply line 11 between the air supply unit 12 and the measurement target removal unit 9.
  • the air AR in the internal space IS is discharged while the air AR is supplied from the air supply line 11 to the internal space IS in the housing 1.
  • the internal space IS can be purged with air AR by discharging from the outlet 13.
  • the internal space IS can be made into an air atmosphere that does not contain dangerous gases such as flammable gases, and a structure can be formed in which these gases do not enter the internal space IS.
  • the filling section 3 is made of a transparent material such as quartz, calcium fluoride, or barium fluoride that hardly absorbs the measurement light L (described later), and the sample gas SG can be filled therein.
  • the space in which the sample gas SG of the filling unit 3 is filled is referred to as a “sampling space SS”.
  • the filling unit 3 is provided with an inlet 31 for introducing the sample gas SG into the sampling space SS and an outlet 32 for discharging the sample gas SG in the sampling space SS. Has been done.
  • the sample gas SG is filled in the sampling space SS from the inlet 31 and then discharged from the outlet 32.
  • the sampling space SS is provided with the first reflective member 33a and the second reflective member 33b.
  • the first reflection member 33a and the second reflection member 33b multiple-reflect the measurement light L incident on the sampling space SS and then propagate it toward the propagation space TS (described later) of the propagation unit 7.
  • the optical path length of the measurement light L passing through the sample gas SG filled in the sampling space SS can be increased.
  • the first reflection member 33a is provided at a position close to the propagation portion 7 in the sampling space SS.
  • the first reflecting member 33a reflects the measurement light L and propagates the measurement light L toward the second reflecting member 33b. Further, the multiple-reflected measurement light L is propagated toward the propagation unit 7. Therefore, the first reflecting member 33a is a member capable of reflecting light such as a half mirror and transmitting a part of the light.
  • the second reflective member 33b is provided at a position away from the propagation portion 7 in the sampling space SS.
  • the second reflecting member 33b reflects the measurement light L toward the first reflecting member 33a. Since the second reflective member 33b does not have to be able to transmit light unlike the first reflective member 33a, for example, a mirror can be used as the second reflective member 33b.
  • the irradiation unit 5 generates the measurement light L.
  • the measurement light L generated from the irradiation unit 5 is guided to the filling unit 3 by the propagation unit 7.
  • the irradiation unit 5 according to the present embodiment is composed of a plurality of light sources 51a to 51d.
  • the plurality of light sources 51a to 51d each output a plurality of elemental lights L1 to L4 having different wavelength regions.
  • the plurality of light sources 51a to 51d are, for example, laser oscillators such as semiconductor laser devices.
  • the element lights L1 to L4 generated from the plurality of light sources 51a to 51d are multiplexed in the propagation space TS of the propagation unit 7 and propagate as the measurement light L toward the filling unit 3. That is, the measurement light L is composed of a plurality of element lights L1 to L4 having different wavelength regions. Since the measurement light L is composed of a plurality of element lights L1 to L4, for example, a plurality of types of measurement target gases having absorption peaks in the wavelength regions of the element lights L1 to L4 can be measured.
  • the interference gas component refers to a component that affects the analysis result of the gas to be measured as a result of having an absorption peak at the same position as or similar to a part of the absorption peak of the gas to be measured. If the influence of the interference gas component can be measured, the influence of the interference gas component can be removed from the measurement result of the measurement light L received by the detection unit 75 (described later), and the measurement target gas can be analyzed with high accuracy.
  • the meaning of "removal" is not only to prevent the influence of the interference gas component at all, but also to reduce the degree of influence as compared with that before the removal.
  • the propagation section 7 is provided between the filling section 3 and the irradiation section 5. Specifically, as shown in FIG. 1, the propagation portion 7 has an L-shape, and is fixed in a state where a plurality of light sources 51a to 51d are partially inserted in a portion corresponding to one side of the L-shape. To. On the other hand, the filling portion 3 is fixed to the other end of the L-shape of the propagation portion 7 via the optical window W. The filling portion 3 and the propagation portion 7 can be fixed by using, for example, a flange F.
  • a plurality of mirrors are arranged in the internal space of the propagation unit 7.
  • the element lights L1 to L4 output from the irradiation unit 5 are propagated to the filling unit 3 by changing the propagation path by these mirrors. That is, the measurement light L propagates in the internal space of the propagation unit 7 while being reflected by at least one mirror.
  • the internal space of the propagation unit 7 through which the measurement light L propagates is referred to as a “propagation space TS”.
  • the first mirror 71a, the second mirror 71b, the third mirror 71c, the fourth mirror 71d, and the fifth mirror 71e are arranged in the propagation space TS. Further, in the propagation space TS, a first optical element 73a, a second optical element 73b, and a third optical element 73c are arranged.
  • the first mirror 71a reflects the element light L1 toward the first optical element 73a.
  • the first optical element 73a reflects the element light L1 and transmits the element light L2. That is, the first optical element 73a multiplexes the element light L1 and the element light L2.
  • the element light L1 and the element light L2 multiplexed by the first optical element 73a pass on the same optical path and head toward the second mirror 71b.
  • the second mirror 71b reflects the element light L1 and the element light L2 multiplexed by the first optical element 73a toward the second optical element 73b.
  • the second optical element 73b reflects the multiplexed element light L1 and the element light L2, and transmits the element light L3. That is, the second optical element 73b multiplexes the element light L1, the element light L2, and the element light L3.
  • the element lights L1 to L3 multiplexed by the second optical element 73b pass on the same optical path and head toward the third mirror 71c.
  • the third mirror 71c reflects the element lights L1 to L3 multiplexed by the second optical element 73b toward the third optical element 73c.
  • the third optical element 73c reflects the multiplexed element lights L1 to L3 and transmits the element light L4. That is, the third optical element 73c multiplexes the element light L1, the element light L2, the element light L3, and the element light L4.
  • the element lights L1 to L4 multiplexed by the third optical element 73c pass on the same optical path toward the fourth mirror 71d.
  • the fourth mirror 71d reflects the element lights L1 to L4 multiplexed by the third optical element 73c toward the fifth mirror 71e.
  • the element lights L1 to L4 multiplexed as described above become the measurement light L.
  • the fifth mirror 71e changes the propagation path of the measurement light L in which the element lights L1 to L4 are multiplexed in the arrangement direction of the filling portion 3.
  • the measurement light L whose propagation path has been changed by the fifth mirror 71e passes through the optical window W and propagates in the sampling space SS of the filling portion 3. Since these mirrors are provided in the propagation space TS, it is possible to prevent the inflow of unnecessary gas from the outside and keep the mirrors in a clean state.
  • a detection unit 75 is arranged in the propagation space TS of the propagation unit 7.
  • the detection unit 75 detects the measurement light L incident on the sampling space SS and reflected multiple times.
  • a thermal photodetector such as a thermopile, a semiconductor detector, a quantum photoelectric device, or the like can be used.
  • the purge gas flows in the propagation space TS, and the state of the detection unit 75 provided in the propagation space can be made a clean state.
  • the sixth mirror that changes the propagation path of the measurement light L that has been multiple reflected in the sampling space SS and returned to the propagation unit 7 in the arrangement direction of the detection unit 75. 71f is provided.
  • the propagation unit 7 has a purge gas supply line 77 and a purge gas discharge port 79.
  • the purge gas supply line 77 is connected to the measurement target removal unit 9, and the purge gas PG generated by the measurement target removal unit 9 is introduced into the propagation space TS.
  • the purge gas discharge port 79 discharges the purge gas PG introduced into the propagation space TS into the internal space IS of the housing 1.
  • the purge gas PG is a gas from which the gas to be measured is removed from the air AR
  • the measurement light L is measured while propagating from the irradiation unit 5 to the filling unit 3 by purging the propagation space TS with the purge gas PG. Can be suppressed from being absorbed by the gas to be measured.
  • the purge gas PG circulates in the propagation space TS, and the state of the plurality of mirrors provided in the propagation space TS can be made a clean state.
  • the measurement target removal unit 9 is provided in the purge gas supply line 77, and removes the measurement target gas from the air AR supplied from the air supply unit 12 to generate the purge gas PG.
  • the measurement target removing unit 9 is, for example, a member called an "N 2 separator" in which a polyimide hollow fiber membrane or a gas separation membrane is filled in a hollow member.
  • the N 2 separator introduces compressed air into the hollow thread film and gas separation film, and the introduced air is made into a nitrogen-rich gas (that is, a gas containing almost no components other than nitrogen gas) and an oxygen-rich gas (that is, a gas containing almost no components other than nitrogen gas). That is, it is separated into the remaining gas) obtained by removing nitrogen from the air AR.
  • the measurement target removing unit 9 which is an N 2 separator discharges nitrogen-rich gas as purge gas PG to the purge gas supply line 77, while discharging oxygen-rich gas to the outside (internal space IS of the housing 1).
  • the hollow fiber membranes include, for example, polyimide, polyamide, polysulfone, cellulose acetate and its derivatives, polyphenylene oxide, polysiloxane, itself microporous polymers, mixed matrix membranes, accelerated transport membranes, polyethylene oxide, polypropylene oxide, carbon. It is composed of membranes, zeolites, or mixtures thereof.
  • the hollow fiber membrane of N 2 separator a nitrogen-rich gas separated by the gas separation membrane, hardly it contains also a measurement target gas. That is, the N 2 separator can separate the gas to be measured from the air and generate a nitrogen-rich gas containing no gas to be measured as a purge gas PG. Further, since the N 2 separator can also separate water, it can be applied to an apparatus for analyzing a gas to be measured whose analysis result is affected by water.
  • the function of separating the nitrogen-rich gas and the oxygen-rich gas from the air does not deteriorate for a long time unless the compressed air to be introduced is contaminated. Therefore, by using the N 2 separator as the measurement target removal unit 9, it is almost unnecessary to replace the measurement target removal unit 9.
  • the measurement target removing unit 9 is arranged in the internal space IS of the housing 1.
  • the oxygen-rich gas discharged from the measurement target removing unit 9 which is an N2 separator and It is also possible to introduce the nitrogen-rich gas discharged from the purge gas discharge port 79 into the internal space IS and substantially purge the internal space IS with air AR.
  • the present invention is not limited to the above, and for example, when oxygen-rich gas is discharged to the outside of the housing 1 without causing a safety problem, the main body (hollow) of the measurement target removing unit 9 can be arranged outside the housing 1.
  • the measurement target removing portion 9 may be arranged outside the housing 1.
  • Control unit 20 is a computer system composed of a CPU, a storage device (for example, a storage device such as RAM and ROM), and various interfaces.
  • the control unit 20 may be a system in which each of the above devices is individually provided, or may be a System (System on Chip) in which each of the above devices is integrated on one chip.
  • the control unit 20 controls the components of the analyzer 100. Further, the analyzer 100 is calibrated and the measurement target gas is analyzed based on the intensity of the measurement light L detected by the detection unit 75.
  • FIG. 2 is a diagram showing a specific configuration of the control unit according to the first embodiment.
  • the control unit 20 mainly includes an analysis unit 201, a first determination unit 203, and a notification unit 205.
  • a part or all of the functions of the above-mentioned parts of the control unit 20 are realized by executing a program stored in the storage device of the computer system constituting the control unit 20.
  • some of the functions of the above parts may be realized in terms of hardware.
  • the analysis unit 201 executes the analysis of the measurement target gas contained in the sample gas SG filled in the filling unit 3. Specifically, the analysis unit 201 controls the irradiation unit 5 (light sources 51a to 51d) to irradiate the measurement light L toward the sampling space SS of the filling unit 3, and the detection unit 75 detects the measurement light L. As a result, the output signal is received.
  • the analysis unit 201 includes the intensity of the measurement light L in each wavelength region after passing through the sampling space SS filled with the reference gas (referred to as the reference gas) that does not contain the measurement target gas, and the sampling filled with the sample gas SG.
  • the gas to be measured is analyzed based on the intensity of the measurement light L after passing through the space SS in each wavelength region. For example, the analysis unit 201 calculates the concentration of the measurement target gas contained in the sample gas SG.
  • the intensity of the measurement light L after passing through the sampling space SS filled with the reference gas is acquired at the time of calibration of the analyzer 100 as the intensity of the measurement light L (referred to as the reference intensity) as the reference for analysis, and is described above. It is stored in the storage device. Alternatively, the reference strength may be acquired at the time of shipment, installation, etc. of the analyzer 100 and stored in the storage device.
  • the reference gas is, for example, nitrogen gas supplied from a cylinder or the like.
  • the first determination unit 203 determines the deterioration of the measurement target removal unit 9 based on the intensity of the measurement target gas L absorbed by the measurement target gas and the gas that affects the measurement light L by passing through the propagation space TS. .. Specifically, the first determination unit 203 has the reference intensity acquired during the calibration operation in which the detection unit 75 detects the measurement light L while filling the filling unit 3 with the reference gas, and the analyzer 100 is installed at the time of shipment. It is determined whether or not the measurement target removal unit 9 is deteriorated based on the comparison with the reference strength acquired at the time or when the measurement target removal unit 9 is replaced.
  • the purge gas PG contains almost no measurement target gas. Therefore, the intensity of the measurement light L obtained by filling the sampling space SS'of the filling unit 3 with the reference gas is substantially the same between the present and the past.
  • the ability to remove the measurement target gas from the air AR is reduced, so that the measurement target gas is included in the purge gas PG.
  • the measurement light L is absorbed by the measurement target gas contained in the purge gas PG while propagating in the propagation space TS, and the intensity of the measurement light L obtained by filling the sampling space SS'of the filling unit 3 with the reference gas is increased.
  • Present and past are different. Specifically, the current strength is smaller than the past strength.
  • the first determination unit 203 determines that the intensity of the measurement light L acquired when the reference gas is filled in the sampling space SS of the filling unit 3 is the sampling space of the filling unit 3 in the past.
  • the intensity is lower than the intensity of the measurement light L obtained by filling the SS by a predetermined intensity or more, it can be determined that the measurement target removing unit 9 has deteriorated.
  • the first determination unit 203 determines that the measurement target removal unit 9 has deteriorated, the first determination unit 203 notifies the notification unit 205 of the determination result.
  • the notification unit 205 When the first determination unit 203 receives the determination result that the measurement target removal unit 9 is deteriorated, the notification unit 205 notifies that the measurement target removal unit 9 is deteriorated. Specifically, the notification unit 205 outputs a signal for operating the notification device 30 when it is determined that the measurement target removal unit 9 is deteriorated.
  • the notification device 30 is, for example, a device (speaker) that emits sound, a warning light, a device that displays an image on a screen (display), and the like. As described above, the notification device 30 is a device that notifies the information output from the analyzer 100.
  • the notification device 30 can be used as an analysis system as a device separate from the analysis device 100. By making the notification device 30 and the analysis device 100 separate devices, for example, the notification device 30 can be installed at a place different from the installation place of the analysis device 100.
  • the control unit 20 may have a second determination unit 207.
  • the second determination unit 207 monitors the pressure measured by the pressure gauge PR1, and the measured pressure is the normal pressure (for example, the pressure when the measurement target removing unit 9 is operating normally without clogging or the like. ), It is determined that the measurement target removing unit 9 is deteriorated due to clogging or the like when the value increases by a predetermined value or more. As a result, deterioration of the measurement target removing unit 9 can be detected without measuring at least the intensity of the measurement light L that has passed through the propagation space TS.
  • the second determination unit 207 determines that the measurement target removal unit 9 has deteriorated, the second determination unit 207 notifies the notification unit 205 of the determination result.
  • FIG. 3 is a flowchart showing an analysis operation of the analyzer according to the first embodiment.
  • the operation shown below is executed by the control unit 20 controlling the analyzer 100.
  • the internal space IS of the housing 1 is purged with air AR in step S1. Specifically, while supplying the air AR from the air supply unit 12 to the air supply line 11, the gas (air AR) in the internal space IS is discharged from the discharge port 13 for a predetermined time.
  • the propagation space TS of the propagation unit 7 is purged with the purge gas PG.
  • the air AR is supplied to the measurement target removal unit 9, and the measurement target removal unit 9 is supplied. Removes the measurement target gas from the supplied air AR to generate a purge gas PG, and discharges the purge gas PG to the purge gas supply line 77.
  • the purge gas PG is supplied from the purge gas supply line 77 to the propagation space TS, and the gas in the propagation space TS (purge gas) is supplied from the purge gas discharge port 79.
  • the propagation space TS can be purged with the purge gas PG.
  • the predetermined time for supplying the air AR to the air supply line 11 is, for example, the time during which the internal space IS of the housing 1 can be replaced by the air AR supplied by the air supply line 11, or the propagation space TS of the propagation unit 7. It can be the longer of the time that can be replaced by the purge gas PG.
  • the time during which the internal space IS can be replaced by the air AR can be determined, for example, based on the capacity of the internal space IS and the flow rate of the air AR. Further, the time during which the propagation space TS can be replaced by the purge gas PG can be determined based on, for example, the capacity of the propagation space TS and the flow rate of the purge gas PG.
  • the purge gas PG can be generated using the air AR supplied from the air supply line 11 as described above. As a result, it is not necessary to prepare a gas cylinder for purging the propagation space TS and install it in the analyzer 100, so that the burden on the user can be reduced.
  • step S3 After purging the internal space IS and the propagation space TS, in step S3, it is determined whether or not the analyzer 100 needs to be calibrated. For example, when a predetermined period (for example, one week) has passed since the previous calibration, or when the analysis of the gas to be measured has been performed a predetermined number of times since the previous calibration, the analyzer 100 is calibrated. It can be determined that it is necessary.
  • a predetermined period for example, one week
  • step S3 If it is determined that the analyzer 100 is to be calibrated (“Yes” in step S3), the analyzer 100 is calibrated in step S4. The specific calibration operation in step S4 will be described in detail later. On the other hand, when it is determined that the calibration of the analyzer 100 is not executed (“No” in step S3), the analysis operation proceeds to step S5, and the analysis of the gas to be measured is executed.
  • the analysis unit 201 After performing the calibration of the analyzer 100 or determining that the calibration is unnecessary, the analysis unit 201 starts the analysis of the gas to be measured in step S5. Specifically, the analysis is performed as follows. First, the sample gas SG is supplied to the sampling space SS of the filling unit 3, and the sampling space SS is filled with the sample gas SG. While supplying the sample gas SG to the sampling space SS, the analysis unit 201 controls the light sources 51a to 51d of the irradiation unit 5 to output the measurement light L toward the sampling space SS of the filling unit 3. The analysis unit 201 receives the detection signal of the measurement light L that has passed through the sampling space SS from the detection unit 75, and based on the detection signal, in the wavelength region of each element light L1 to L4 of the detected measurement light L. Calculate the strength.
  • the analysis unit 201 determines the intensity (that is, the reference intensity) of the measurement light L before passing through the sampling space SS filled with the sample gas SG in the wavelength region, and after passing through the sampling space SS filled with the sample gas SG.
  • the concentration of the measurement target gas contained in the sample gas SG is calculated based on the ratio of the measurement light L to the intensity in the above wavelength region. For example, when the measurement target gas can absorb all of the element lights L1 to L4, the analysis unit 201 interferes with the analysis result of the measurement target gas based on the intensity in the wavelength region of each element light L1 to L4.
  • the concentration of the gas can be calculated, and the concentration of the gas to be measured can be calculated accurately in consideration of the influence of the interference gas.
  • the analysis unit 201 concerned when there are a plurality of gas to be measured, the analysis unit 201 concerned, for example, based on the intensity of any wavelength region of the element lights L1 to L4 that can be absorbed by the gas to be measured among the element lights L1 to L4. The concentration of the gas to be measured can be calculated.
  • step S5 If you want to continue the analysis of the gas to be measured after completing one analysis, repeat step S5 above. On the other hand, when it is desired to end the analysis of the gas to be measured, the generation of the measurement light L from the irradiation unit 5 is stopped, and the analysis operation is ended.
  • FIG. 4 is a flowchart showing a calibration operation of the analyzer according to the first embodiment. The operation shown below is executed by the control unit 20 controlling the analyzer 100.
  • the control unit 20 controlling the analyzer 100.
  • the analyzer 100 according to the first embodiment when the analyzer 100 is calibrated, after acquiring the intensity (that is, the reference intensity) of the measurement light L that has passed through the reference gas that does not contain the measurement target gas, the measurement target is further further measured. Deterioration of the removing unit 9 is determined. Specifically, the following steps S41 to S45 are executed as calibration operations.
  • the sampling space SS of the filling unit 3 is filled with a reference gas (a gas that does not contain the gas to be measured).
  • the reference gas is nitrogen gas.
  • the control unit 20 controls the light sources 51a to 51d of the irradiation unit 5 to output the measurement light L toward the sampling space SS filled with the reference gas.
  • the control unit 20 receives the detection signal of the measurement light L that has passed through the sampling space SS from the detection unit 75, and calculates the intensity of the detected measurement light L based on the detection signal.
  • step S43 the control unit 20 determines the intensity of the measurement light L calculated in step S42 as the intensity of the measurement light L before passing through the sampling space SS filled with the sample gas SG (that is, the reference intensity). , Stored in the storage device of the control unit 20. By executing the acquisition and storage of the reference intensity, the calibration device 100 can be calibrated.
  • the first determination unit 203 acquires the reference strength acquired by this calibration and the past (for example, at the time of shipment of the analyzer 100, at the time of installation, at the time of replacement of the previous measurement target removal unit 9, etc.).
  • the reference strength acquired this time is smaller than a predetermined value or more than the reference strength acquired in the past, it is determined that the measurement target removing unit 9 has deteriorated.
  • the reference intensity is measured in a state where the sampling space SS is filled with the reference gas, that is, in a state where the measurement light L is not absorbed while passing through the sampling space SS. Therefore, the fact that the reference intensity acquired this time is smaller than the reference intensity acquired in the past means that the amount of light absorbed while the measurement light L is passing through the propagation space TS at the time of this calibration is the amount of the measurement light L in the past. It means that it is larger than the amount of light absorbed while passing through the propagation space TS.
  • the amount of light absorbed while the measurement light L passes through the propagation space TS at the time of this calibration is larger than the amount of light absorbed while the measurement light L passes through the propagation space TS in the past.
  • the amount (concentration) of the measurement target gas contained in the purge gas PG at the time of this calibration is larger than the amount (concentration) of the measurement target gas contained in the past purge gas PG, and the measurement target is removed. This means that the ability of the part 9 to remove the gas to be measured is reduced.
  • the first determination unit 203 compares the current and past reference intensities, and based on the intensity of the measurement light L that has passed through the propagation space TS, the measurement target removal unit 9 Deterioration can be determined. That is, in the analyzer 100 according to the first embodiment, the deteriorated state of the measurement target removing unit 9 can be easily determined by a method similar to the analysis of the measurement target gas.
  • the second determination unit 207 determines the pressure measured by the pressure gauge PR1 at the time of this calibration and the past (for example, at the time of shipment, installation, and previous time of the analyzer 100).
  • the pressure measured by the pressure gauge PR1 is compared with the pressure measured by the pressure gauge PR1 at the time of replacement of the measurement target removal unit 9), and the pressure measured this time is larger than a predetermined value by a predetermined value or more, the measurement target is removed. It is determined that the part 9 is deteriorated.
  • the second determination unit 207 determines whether or not the gas flow in the measurement target removal unit 9 has deteriorated based on the pressure or flow rate of the air supplied to the measurement target removal unit 9, and the gas flow is increased.
  • the second determination unit 207 can determine whether or not deterioration (abnormality) has occurred due to "clogging" or the like that affects the pressure and flow rate of the air AR supplied to the measurement target removal unit 9.
  • step S45 the first determination unit 203 and / or the second determination unit 207 determines that the measurement target removal unit 9 has deteriorated (“Yes” in step S44), in step S45, the first determination unit 203 and / or The second determination unit 207 notifies the notification unit 205 of the determination result that the measurement target removal unit 9 has deteriorated.
  • the notification unit 205 Upon receiving the determination result that the measurement target removing unit 9 has deteriorated, the notification unit 205 outputs a notification signal to the notification device 30 to operate the notification device 30.
  • a sound can be generated and / or a warning light can be turned on to notify that the measurement target removing unit 9 has deteriorated in a form that the user can visually and / or audibly recognize. ..
  • a user who recognizes that the measurement target removal unit 9 has deteriorated can take measures such as replacing the measurement target removal unit 9.
  • the deterioration of the measurement target removal unit 9 is caused by insufficient removal of the causative substances (for example, oil mist, dust, etc.) that deteriorate the measurement target removal unit 9 in the air supply unit 12. If so, the user can also replace the filter provided in the air supply unit 12 for removing causative substances such as oil mist and dust.
  • the air AR supply line for purging the internal space IS of the housing 1 and the measurement target removing unit 9 are supplied.
  • the supply line of the air AR to be used is common as the air supply line 11.
  • the present invention is not limited to this, and as shown in FIG. 5, in the modified example of the analyzer according to the first embodiment (analyzer 100'), the air AR supply line for purging the internal space IS of the housing 1 is provided.
  • the air supply line may be provided individually, with the first air supply line 11a as the first air supply line 11a and the air AR supply line supplied to the measurement target removing unit 9 as the second air supply line 11b.
  • FIG. 5 is a diagram showing a modified example of the analyzer according to the first embodiment.
  • a three-way valve 11c is provided at the confluence of the purge gas supply line 77, the first air supply line 11a, and the line from the measurement target removing unit 9.
  • the three-way valve 11c enables gas flow between the first air supply line 11a and the purge gas supply line 77.
  • the internal space IS and the propagation space TS of the housing 1 are purged with the air AR.
  • the three-way valve 11c enables gas flow between the line from the measurement target removal unit 9 and the purge gas supply line 77. As a result, the propagation space TS is purged with the purge gas PG.
  • the air AR is supplied to the measurement target removal unit 9 only when necessary to generate purge gas PG, and the replacement frequency of the measurement target removal unit 9 is reduced. it can.
  • the purge gas PG that purges the propagation space TS that is reflected by at least one mirror and propagates before the measurement light L reaches the filling portion 3 forms a gas separation membrane. It is generated by the measurement target removing unit 9 having the measurement target. This eliminates the need for work that increases the burden on the user, such as frequent replacement of cylinders for supplying purge gas. That is, the purge gas PG can be generated and supplied without increasing the burden on the user.
  • the analyzers 100 and 100' are provided with a first determination unit 203 that determines deterioration of the measurement target removal unit 9 based on the intensity of the measurement light L that has passed through the propagation space TS. Thereby, the deteriorated state of the measurement target removing unit 9 can be easily determined by a method similar to the analysis of the measurement target gas.
  • the analyzers 100 and 100' may include a second determination unit 207 that determines deterioration of the measurement target removal unit based on the pressure or flow rate of the air AR supplied to the measurement target removal unit 9. This makes it possible to determine whether or not deterioration (abnormality) has occurred due to "clogging" or the like that affects the pressure or flow rate of the air AR supplied to the measurement target removing unit 9.
  • the analyzers 100 and 100' are further provided with a notification unit 205 for notifying that the measurement target removal unit 9 has been determined to be deteriorated. As a result, the user can be notified that the measurement target removing unit 9 has deteriorated.
  • the analyzers 100 and 100'further further include a housing 1 that stores the filling unit 3, the irradiation unit 5, and the propagation unit 7 and isolates them from the external space.
  • a housing 1 that stores the filling unit 3, the irradiation unit 5, and the propagation unit 7 and isolates them from the external space.
  • the measurement target removing unit 9 has a gas separation membrane that separates nitrogen gas from air, and the nitrogen gas separated by the gas separation membrane is used as a purge gas PG. Since the ability of the gas separation membrane to separate nitrogen gas and oxygen gas from the air lasts for a long period of time, it is possible to almost eliminate the need to replace the measurement target removing unit 9. As a result, the burden on the user can be reduced.
  • the measurement target removing unit which is the N 2 separator described in the above 1st embodiment, is also used for other analyzers that analyze the measurement target gas. Applicable.
  • the measurement target removing unit can be used in the analyzer 200 according to the second embodiment described below.
  • the analyzer 200 according to the second embodiment will be specifically described.
  • the analyzer 200 according to the second embodiment is a cross-flow modulation type analyzer.
  • the reference gas RG that does not contain the measurement target gas and the sample gas SG that contains the measurement target gas are alternately introduced into the filling section 301, and the measurement light passes through the filling section 301 filled with the reference gas RG.
  • This is a method of analyzing the measurement target gas contained in the sample gas SG based on the intensity of L'and the intensity of the measurement light L'passed through the filling portion 301 filled with the sample gas SG.
  • the measurement target removing unit 302 which is the N 2 separator described in the first embodiment, is used to generate the reference gas RG.
  • the sample gas SG is, for example, the atmosphere.
  • the measurement target gas is, for example, carbon dioxide (CO 2 ) contained in the sample gas SG.
  • gases to be measured include, for example, carbon monoxide (CO), sulfur oxide (SOx) (for example, sulfur dioxide (SO 2 )), ammonia (NH 3 ), and nitrogen oxide (NOx) (for example, nitrogen monoxide).
  • the above-mentioned reference gas RG is a gas used as a reference for analysis of the gas to be measured, and is a gas that does not contain the gas to be measured at all or contains only a gas that does not affect the analysis. Therefore, the intensity of the measurement light L'passing through the filling portion 301 filled with the reference gas RG is the measurement light L'as a back grind included in the intensity of the measurement light L'passing through the filling portion 301 filled with the sample gas SG. 'Strength.
  • FIG. 6 is a diagram showing a configuration of an analyzer according to the second embodiment.
  • the analyzer 200 mainly includes a filling unit 301, a measurement target removing unit 302, and an introducing unit 303.
  • the filling section 301 has a sampling space SS'that can be filled with gas, one end of the sampling space SS'is connected to the gas outlet 303c of the introduction section 303, and the other end is connected to the discharge flow path 304.
  • the sampling space SS' can be filled with the sample gas SG or the reference gas RG.
  • an orifice 304a and a first pump 304b are provided in the discharge flow path 304 to which the other end of the sampling space SS'of the filling portion 301 is connected.
  • the flow rate of the sample gas SG or the reference gas RG introduced into the sampling space SS' is determined by the dimensions of the orifice 304a and the flow rate of the first pump 304b.
  • the filling unit 301 includes an irradiation unit 301a that irradiates the sampling space SS'with the measurement light L', and a detection unit 301b that detects the measurement light L'that has passed through the sampling space SS'.
  • the irradiation unit 301a is, for example, a light generator such as a laser that generates measurement light L'having a wavelength (for example, infrared light) that can be absorbed by the measurement target gas.
  • the detection unit 301b is, for example, a photodetector capable of detecting the measurement light L'.
  • the measurement target removing unit 302 generates the reference gas RG to be filled in the sampling space SS'of the filling unit 301 from the reference gas generating gas. Specifically, the measurement target removing unit 302 receives the sample gas SG from the branch line 305 branched from the discharge flow path 304, and removes the measurement target gas from the supplied sample gas SG. That is, in the analyzer 200 shown in FIG. 6, the reference gas generation gas is the sample gas SG. As a result, a more appropriate reference gas RG can be generated from the sample gas SG to be measured.
  • the measurement target removing unit 302 is a member called an "N 2 separator" in which a hollow fiber membrane and a gas separation membrane are filled in a hollow member.
  • Hollow fiber membranes include, for example, polyimide, polyamide, polysulfone, cellulose acetate and its derivatives, polyphenylene oxide, polysiloxane, itself microporous polymers, mixed matrix membranes, accelerated transport membranes, polyethylene oxide, polypropylene oxide, carbon membranes. , Polyamide, or a mixture thereof.
  • the N 2 separator introduces the compressed sample gas SG into the hollow thread film and the gas separation film, so that the introduced sample gas SG is combined with a nitrogen-rich gas (that is, a gas containing almost no components other than nitrogen gas).
  • the gas is separated into an oxygen-rich gas (that is, the remaining gas obtained by removing the nitrogen gas from the sample gas SG).
  • the measurement target removing unit 302, which is an N 2 separator, supplies a nitrogen-rich gas as a reference gas RG to the reference gas supply line 306.
  • the hollow fiber membrane of the N 2 measured removal unit 302 is a separator, a nitrogen-rich gas separated by the gas separation membrane, hardly it contains also a measurement target gas. That is, the measurement target removing unit 302, which is an N 2 separator, can separate the measurement target gas from the sample gas SG and generate a nitrogen-rich gas containing no measurement target gas as the reference gas RG.
  • the branch line 305 that supplies the sample gas SG to the measurement target removal unit 302 is provided with a boosting pump 305a that boosts the sample gas SG and supplies it to the measurement target removal unit 302.
  • a regulator 305b is provided between the boosting pump 305a and the measurement target removing unit 302. The regulator 305b keeps the pressure of the sample gas SG supplied from the boosting pump 305a to the measurement target removing unit 302 constant. As a result, the life of the measurement target removing unit 302 can be extended.
  • the introduction unit 303 introduces the sample gas SG or the reference gas RG into the sampling space SS'of the filling unit 301.
  • the introduction unit 303 has a first inlet 303a, a second inlet 303b, and a gas outlet 303c, and makes the first inlet 303a and the gas outlet 303c capable of gas distribution, or It is a three-way valve that can switch between enabling gas flow between the second inlet 303b and the gas outlet 303c.
  • the sample gas SG is supplied to the first inlet 303a of the introduction unit 303.
  • the second inlet 303b is connected to the reference gas supply line 306. That is, the reference gas RG generated by the measurement target removing unit 9 is supplied to the second inlet 303b.
  • the introduction unit 303 enables gas flow between the first inlet 303a and the gas outlet 303c (that is, discharges the sample gas SG from the gas outlet 303c), and the second inlet 303b.
  • the sampling space of the filling unit 301 alternately switches between enabling the gas outlet 303c to flow through the gas (that is, discharging the reference gas RG from the gas outlet 303c) and alternately switching the sample gas SG and the reference gas RG.
  • Fill SS' By providing the introduction unit 303, it is possible to realize a cross-flow modulation type analyzer 200 that alternately fills the sampling space SS'of the filling unit 301 with the sample gas SG and the reference gas RG.
  • the analyzer 200 further includes a control unit 307.
  • the control unit 307 is a computer system composed of a CPU, a storage device (for example, a storage device such as a RAM or a ROM), and various interfaces.
  • the control unit 307 may be a system in which each of the above devices is individually provided, or may be a System (System on Chip) in which each of the above devices is integrated on one chip.
  • the control unit 307 controls the irradiation unit 301a and the introduction unit 303 of the analyzer 200.
  • the control unit 307 may be capable of controlling the operation and stop of the first pump 304b and the boosting pump 305a and / or the flow rate.
  • control unit 307 controls the irradiation unit 301a to irradiate the sampling space SS'of the filling unit 301 with the measurement light L', passes through the sampling space SS', and is detected by the detection unit 301b. Analyze the gas to be measured based on the intensity of'.
  • FIG. 7 is a flowchart showing an analysis operation of the analyzer according to the second embodiment.
  • the analyzer 200 analyzes the gas to be measured by the cross-flow modulation method.
  • the operation shown below is executed by the control unit 307 controlling the analyzer 200.
  • calibration of the analyzer 200 for example, zero calibration, span calibration is performed every predetermined period (for example, one week).
  • step S201 the control unit 307 controls the introduction unit 303 to enable gas flow between the second inlet 303b and the gas outlet 303c.
  • the reference gas RG is supplied from the reference gas supply line 306 to the introduction unit 303, and the reference gas RG is introduced from the gas outlet 303c into the sampling space SS'of the filling unit 3. That is, the reference gas RG is filled in the sampling space SS'of the filling unit 3.
  • the control unit 307 After filling the sampling space SS'of the filling unit 3 with the reference gas RG, in step S202, the control unit 307 outputs the measurement light L'from the irradiation unit 301a, and the sampling space of the filling unit 3 filled with the reference gas RG.
  • the measurement light L'that has passed through SS' is detected by the detection unit 301b.
  • the control unit 307 calculates the intensity (called the analysis reference intensity) of the measurement light L'passing through the sampling space SS'of the filling unit 3 filled with the reference gas RG based on the signal input from the detection unit 301b. ..
  • step S203 the control unit 307 controls the introduction unit 303 to enable gas flow between the first inlet 303a and the gas outlet 303c.
  • the sample gas SG is introduced from the gas outlet 303c into the sampling space SS'of the filling unit 3. That is, the sample gas SG is filled in the sampling space SS'of the filling unit 3.
  • the control unit 307 After filling the sampling space SS'of the filling unit 3 with the sample gas SG, in step S204, the control unit 307 outputs the measurement light L'from the irradiation unit 301a, and the sampling space of the filling unit 3 filled with the sample gas SG.
  • the measurement light L'that has passed through SS' is detected by the detection unit 301b.
  • the control unit 307 calculates the intensity (referred to as analysis intensity) of the measurement light L'passing through the sampling space SS'of the filling unit 3 filled with the sample gas SG based on the signal input from the detection unit 301b.
  • step S205 the control unit 307 analyzes the measurement target gas contained in the sample gas SG based on the difference between the analysis intensity calculated in step S204 and the analysis reference intensity calculated in step S202. Specifically, the concentration of the gas to be measured is calculated from the difference between the analysis intensity and the analysis reference intensity.
  • the reference gas RG is generated from the sample gas SG by using the measurement target removing unit 9. This eliminates the need to provide a gas cylinder for the reference gas RG. As a result, the burden on the user due to replacement of the gas cylinder or the like can be reduced.
  • the ability to separate nitrogen gas and oxygen gas from air lasts for a long period of time, so that it is almost unnecessary to replace the measurement target removal unit 302. Can be done. As a result, the burden on the user can be reduced.
  • the analyzer 200 shown in FIG. 6 since it is not necessary to switch and use a plurality of removing portions for removing the gas to be measured, a complicated gas path for switching and using the plurality of removing portions is provided. There is no need to form. By making the gas path of the analyzer 200 simpler in this way, the number of parts used in the analyzer 200 can be reduced.
  • a modification 1 (analyzer 200') of the analyzer according to the second embodiment further includes an air supply unit 309 for supplying the boosted air AR', and the air supply unit 309 is provided. It is connected to the measurement target removing unit 302 by the air supply line 309a.
  • FIG. 8 is a diagram showing a configuration of a modification 1 of the analyzer according to the second embodiment.
  • the reference gas generation gas supplied to the measurement target removing unit 302 from the air supply unit 309, which is a supply source different from the sample gas SG, it is sufficient without providing the boosting pump 305a.
  • a regulator 309b is provided between the air supply unit 309 and the measurement target removal unit 302.
  • the regulator 309b keeps the pressure of the sample gas SG supplied from the air supply unit 309 to the measurement target removal unit 302 constant.
  • the intensity of the measurement light L'when the reference gas RG supplied from the measurement target removing unit 302 is filled in the filling unit 3, and the gas used for, for example, zero calibration (for example,).
  • the state of the ability of the measurement target removing unit 302 to remove the measurement target gas that is, the measurement target
  • the state of deterioration of the removing unit 302 can be confirmed.
  • the state of deterioration of the measurement target removing unit 302 is determined by the control unit 307'of the analyzer 200'.
  • Other configurations and functions of the analyzer 200' are the same as those of the analyzer 200 according to the second embodiment, and thus the description thereof will be omitted here.
  • FIG. 9 is a diagram showing a specific configuration of the control unit according to the first modification.
  • the control unit 307' mainly includes an analysis unit 307a, a determination unit 307b, and a notification unit 307c.
  • a part or all of the functions of the above-mentioned parts of the control unit 307' are realized by executing a program stored in the storage device of the computer system constituting the control unit 307.
  • some of the functions of the above parts may be realized in terms of hardware.
  • the analysis unit 307a analyzes the measurement target gas contained in the sample gas SG. Since the analysis operation of the measurement target gas executed by the analysis unit 307a is the same as the operation of the control unit 307 in the second embodiment described above, the description thereof will be omitted here.
  • the determination unit 307b determines the deterioration of the measurement target removal unit 302.
  • the determination unit 307b contains, for example, the intensity of the measurement light L'obtained when the reference gas RG is filled in the sampling space SS'of the filling unit 3, and the zero gas used for zero calibration of the analyzer, which contains almost no gas to be measured. Based on the comparison with the intensity of the measurement light L'obtained when the sampling space SS'is filled with (for example, nitrogen gas supplied from a gas cylinder), it is determined whether or not the measurement target removing unit 302 has deteriorated. To do.
  • the measurement target removal unit 302 If the measurement target removal unit 302 is not deteriorated, the content of the measurement target gas contained in the reference gas RG is close to the content of the measurement target gas in the above zero gas. Therefore, the intensity of the measurement light L'obtained when the reference gas RG is filled in the sampling space SS'of the filling portion 3 and the measurement light L'obtained by filling the sampling space SS'of the filling portion 3 with zero gas. The strength is almost the same.
  • the measurement target removal unit 302 when the measurement target removal unit 302 is deteriorated, the ability to remove the measurement target gas from the reference gas generation gas (air AR in this embodiment) is reduced, so that the measurement target gas is used as the reference gas RG. Will be included.
  • the measurement light L'passed through the sampling space SS'filled with the reference gas RG is absorbed by the measurement target gas contained in the reference gas RG, and the intensity of the measurement light L'acquired when the reference gas RG is filled. However, it becomes smaller than the intensity of the measurement light L'obtained by filling with zero gas.
  • the determination unit 307b has the intensity of the measurement light L'acquired when the reference gas RG is filled in the sampling space SS'of the filling unit 3, and the intensity of the measurement light L'is zero gas in the sampling space SS'of the filling unit 3. If the intensity is lower than the intensity of the measurement light L'obtained by filling in, it can be determined that the measurement target removing unit 302 has deteriorated. When the determination unit 307b determines that the measurement target removal unit 9 has deteriorated, the determination unit 307b notifies the notification unit 307c of the determination result.
  • the notification unit 307c When the determination unit 307b receives the determination result that the measurement target removal unit 302 has deteriorated, the notification unit 307c notifies that the measurement target removal unit 302 has deteriorated. Specifically, the notification unit 307c outputs a signal for operating the notification device 308 when it is determined that the measurement target removal unit 302 has deteriorated.
  • the notification device 308 is, for example, a device (speaker) that emits sound, a warning light, a device that displays an image on a screen (display), and the like. As described above, the notification device 308 is a device that notifies the information output from the analyzer 200.
  • the notification device 308 can be used as an analysis system as a device separate from the analysis device 200. By making the notification device 308 and the analyzer 200 separate devices, for example, the notification device 308 can be installed at a location different from the installation location of the analyzer 200.
  • FIG. 10 is a flowchart showing a deterioration determination operation of the measurement target removing portion in the analyzer according to the first modification of the second embodiment. The operation shown below is executed by the determination unit 307b controlling the analyzer 200.
  • the sampling space SS'of the filling unit 3 is filled with zero gas using, for example, a gas cylinder of zero gas (for example, nitrogen gas).
  • step S302 the measurement light L'is output from the irradiation unit 301a, and the measurement light L'that has passed through the sampling space SS' of the filling unit 3 filled with zero gas is detected by the detection unit 301b. Based on the signal input from the detection unit 301b, the intensity of the measurement light L'passed through the sampling space SS'of the filling unit 3 filled with zero gas is calculated.
  • step S303 the reference gas RG from which the measurement target gas has been removed by the measurement target removal unit 302 is filled in the sampling space SS'of the filling unit 3.
  • the introduction unit 303 is controlled to enable gas flow between the second inlet 303b and the gas outlet 303c, and the reference gas RG is filled in the sampling space SS'.
  • step S304 the measurement light L'is output from the irradiation unit 301a, and the measurement light L'that has passed through the sampling space SS' of the filling unit 3 filled with the reference gas RG is detected by the detection unit 301b. Based on the signal input from the detection unit 301b, the intensity of the measurement light L'passed through the sampling space SS'of the filling unit 3 filled with the reference gas RG is calculated.
  • the determination unit 307b determines the intensity of the measurement light L'that has passed through the zero gas acquired in step S302 and the measurement light L'that has passed through the reference gas RG acquired in step S304. Based on the comparison with the strength, it is determined whether or not the measurement target removing unit 302 has deteriorated. For example, the absolute value of the difference between the intensity of the measurement light L'that passed through the reference gas RG acquired in step S304 and the intensity of the measurement light L'that passed through the zero gas acquired in step S302 became equal to or greater than a predetermined value. In this case, it is determined that the reference gas RG contains a predetermined amount or more of the measurement target gas and the measurement target removal unit 302 has deteriorated.
  • step S306 the determination unit 307b determines that the measurement target removal unit 302 has deteriorated.
  • the result is notified to the notification unit 307c.
  • the notification unit 307c Upon receiving the determination result that the measurement target removing unit 302 has deteriorated, the notification unit 307c outputs a notification signal to the notification device 308 to operate the notification device 308.
  • a sound can be generated and / or a warning light can be turned on to notify that the measurement target removing unit 302 has deteriorated in a form that the user can visually and / or audibly recognize. ..
  • the user who recognizes that the measurement target removal unit 302 has deteriorated can take measures such as replacing the measurement target removal unit 302.
  • the determination unit 307b determines that the measurement target removal unit 302 has deteriorated (“No” in step S305)
  • the determination operation for deterioration of the measurement target removal unit 302 ends.
  • FIG. 11 is a diagram showing a configuration of a modification 2 of the analyzer according to the second embodiment. Since the analyzer 200 ′′ has the same configuration and function as the analyzer 200 ′ according to the first modification except that the scrubbers 310a and 310b are provided, the description thereof will be omitted here.
  • the scrubbers 310a and 310b are members in which the water adsorbent S and the gas adsorbent Z to be measured are sealed inside the refiner main body 311.
  • the water adsorbent S removes water from the gas supplied from the measurement target removing unit 302.
  • the water adsorbent S has a property that the adsorbed component is released by heating to a predetermined regeneration temperature.
  • silica gel having an adsorptive capacity that can be regenerated is used, in which water physically adsorbed by heating to a predetermined temperature is released by heating to a predetermined temperature.
  • the measurement target gas adsorbent Z further removes the measurement target gas from the gas supplied from the measurement target removal unit 302.
  • a zeolite having an adsorptive capacity that can be released by heating the physically adsorbed measurement target gas to a predetermined temperature higher than that of silica gel can be used.
  • a molecular sieve or the like can be used as the gas adsorbent Z to be measured.
  • Such an adsorbent utilizes, for example, a molecular sieving action that has a large number of micropores and selectively adsorbs only molecules having a size capable of entering the micropores. Unlike soda lime, which adsorbs molecules by chemical bonds, it has the property of being easily regenerated by heating.
  • the refiner main body 311 is formed of, for example, a cylindrical metal member, and an input port 311a into which gas flows in is provided on one end surface thereof, and an output port 311b from which gas is led out is provided on the other end surface thereof.
  • the half portion of the refiner main body 311 on the input port 311a side is filled with the water adsorbent S, and the half portion on the output port 311b side is filled with the gas adsorbent Z to be measured.
  • a filter mesh M is arranged as a partition at the boundary between the water adsorbent S and the gas adsorbent Z to be measured.
  • the scrubbers 310a and 310b further have a heating mechanism 312.
  • the heating mechanism 312 is provided with a winding heater that can be turned ON / OFF by an external operation, for example, and is wound around a half portion of the refiner main body 311 on the output port 311b side to measure the gas adsorbent Z. Directly heat.
  • the water adsorbent S is indirectly heated by heat transfer or the like from the refiner main body 311.
  • the heating temperature by the heating mechanism 312 is set to be equal to or higher than the minimum reproducible temperature of the gas adsorbent Z to be measured, and the temperature of the water adsorbent S is set to be equal to or higher than the reproducible temperature and lower than the decomposition temperature.
  • the heating temperature by the heating mechanism 312 is, for example, 130 ° C to 180 ° C.
  • the analyzer 200 ′′ according to the second modification includes two scrubbers 310a and 310b in parallel.
  • the two scrubbers 310a and 310b can be used by switching between them.
  • the gas line GL1 connected to the outlet of the measurement target removing unit 302 is bifurcated in the middle to form two gas lines GL2 and GL3.
  • the gas line GL2 is connected to the input port 311a of the scrubber 310a
  • the gas line GL3 is connected to the input port 311a of the 310b.
  • a switching valve V1 (for example, a three-way valve) is provided at the branch point of the gas line.
  • the switching valve V1 switches between connecting the gas line GL1 and the gas line GL2 or connecting the gas line GL1 and the gas line GL2, so that one of the two scrubbers 310a and 310b can be removed from the measurement target. Connect to 302.
  • the gas line not connected to the gas line GL1 is connected to the purge gas discharge line GL4 by the switching valve V2 (for example, a three-way valve). ..
  • the switching valve V1 connects the gas line GL1 and the gas line GL3, and the switching valve V2 connects the gas line GL2 and the purge gas discharge line GL4.
  • the gas to be measured is removed by the scrubber 310b connected to the gas line GL3.
  • the switching valve V1 connects the gas line GL1 and the gas line GL2, and the switching valve V2 connects the gas line GL3 and the purge gas discharge line GL4.
  • the gas to be measured is removed by the unused or regenerated scrubber 310a.
  • the scrubber 310a is used in the above example, in the scrubber 310b whose removal capacity is reduced, the moisture adsorbent S and the gas adsorbent Z to be measured are regenerated by heating by the heating mechanism 312. This allows regeneration of the other scrubber while using one scrubber.
  • the above analyzer 200'' further includes scrubbers 310a and 310b for removing the measurement target gas from the gas that has passed through the measurement target removal unit 302, whereby a reference gas RG having a lower measurement target gas content can be generated. At the same time, the life of the scrubbers 310a and 310b can be extended.
  • the measurement target removing unit 302 separates the measurement target gas from the reference gas generation gas (sample gas SG or air AR') and separates the measurement target gas from the reference gas RG.
  • the reference gas generation gas sample gas SG or air AR'
  • the measurement target removing unit 302 since the measurement target removing unit 302 has a long life, it is not necessary to configure the analyzers 200, 200', 200'' in a complicated configuration such as switching a plurality of gas lines to generate a reference gas RG. , The analyzers 200, 200', 200'' can be easily controlled.
  • the deteriorated state of the measurement target removing unit 302 can be easily determined by a method similar to analyzing the measurement target gas based on the intensity of the measurement light L'passed through the gas filled in the filling unit 3. Can be judged.
  • the analyzers 200, 200', 200'' are provided with a notification unit 307c for notifying that the measurement target removal unit 302 has been determined to be deteriorated, thereby notifying the user that the measurement target removal unit 302 has deteriorated. it can.
  • the analyzers 200, 200', and 200'' are provided with an introduction unit 303 for alternately introducing the sample gas SG and the reference gas RG into the sampling space SS'of the filling unit 3, so that the measurement target gas of the cross flow modulation method is provided.
  • An analyzer can be realized.
  • the reference gas generation gas is supplied to the measurement target removing unit 302 by using the air AR'supplied from a supply source (air supply unit 309) different from the sample gas.
  • the condition of the reference gas generation gas can be set to an appropriate condition that can easily fully exhibit the performance of the measurement target removing unit 302.
  • the analyzer 200'' can generate a reference gas RG having a lower measurement target gas content, and can also generate the reference gas RG.
  • the life of the scrubbers 310a and 310b can be extended.
  • the propagation space TS includes the first mirror 71a, the second mirror 71b, the third mirror 71c, and the fourth mirror 71d. It was explained that the fifth mirror 71e and the sixth mirror 71f are arranged. The arrangement of these mirrors may be changed according to the positional relationship between the light sources 51a to 51d and the filling portion 3 inside the housing 1.
  • the distance between the light sources 51a to 51d and the filling portion 3 becomes shorter, the distance from the light sources 51a to 51d in which the measurement light L propagates in the propagation space TS to the filling portion 3 becomes shorter, in the propagation space TS.
  • the number of mirrors may be reduced, or the mirrors may not be provided in the propagation space TS.
  • the purge gas PG generated from the measurement target removal unit 9 is filled in the sampling space SS of the filling unit 3.
  • Deterioration of the measurement target removing unit 9 may be determined based on the intensity of the measurement light L that has passed through the purge gas PG in the sampling space SS.
  • the optical path length of the measurement light L in the sampling space SS is long due to multiple reflections. Therefore, based on the intensity of the measurement light L that has passed through the purge gas PG in the sampling space SS, the purge gas PG It is possible to accurately measure the low-concentration measurement target gas contained in.
  • the intensity of the measurement light L in a state including the influence thereof can be measured.
  • the content of the measurement target gas contained in the purge gas PG can be measured more accurately.
  • a gas-filled cell having the same configuration as the filling portion 3 and not containing a measurement target gas such as nitrogen gas is individually provided, and a measurement target removal unit is provided.
  • the measurement light L may be passed through the cell.
  • the amount of absorbed light L by the measurement target gas contained in the purge gas PG in the propagation space TS can be accurately measured without being affected by the contamination of the filling portion 3.
  • porous water is used to remove the measurement target gas contained in the gas.
  • a disposable removing agent using calcium oxide, a coloring agent, and silver nitrate may be used. This makes it possible to realize stable measurement at low cost.
  • the measurement target removing unit 9 generated purge gas from the air supplied from the air supply line 11.
  • the present invention is not limited to this, and instead of the air supply line 11, for example, a cylinder filled with a gas containing oxygen and nitrogen is connected to the measurement target removal unit 9, and the measurement target removal unit 9 is supplied from the cylinder. Nitrogen may be extracted from the gas to generate purge gas.
  • the present invention can be widely applied to an analyzer that analyzes a gas to be measured contained in a sample gas.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
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Abstract

La présente invention permet de fournir, entre autres, un gaz de purge qui est nécessaire pour l'analyse d'un gaz à mesurer, sans augmenter la charge pesant sur un utilisateur. Un dispositif d'analyse (100, 100') comprend une partie de remplissage (3), une partie de rayonnement (5), une partie de transmission (7) et une partie d'élimination de cible de mesure (9). La partie de remplissage (3) est remplie d'un gaz échantillon (SG) contenant un gaz à mesurer. La partie de rayonnement (5) irradie la partie de remplissage (3) avec une lumière de mesure (L). La partie de transmission (7) forme un espace de transmission (TS) à travers lequel la lumière de mesure (L) est transmise, l'espace de transmission (TS) étant prévu entre la partie de remplissage (3) et la partie de rayonnement (5). La partie d'élimination de cible de mesure (9) a une membrane de séparation de gaz qui génère un gaz de purge (PG) pour éliminer le gaz à mesurer de l'air pour purger l'espace de transmission (TS).
PCT/JP2020/045320 2019-12-17 2020-12-04 Dispositif d'analyse et système d'analyse WO2021124937A1 (fr)

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WO2023063136A1 (fr) * 2021-10-12 2023-04-20 株式会社堀場製作所 Dispositif d'analyse de gaz, procédé d'analyse de gaz et programme pour dispositif d'analyse de gaz

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DE202023101770U1 (de) 2023-04-06 2023-05-11 CS INSTRUMENTS GmbH & Co. KG Probenentnahme

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CN114577793A (zh) * 2022-05-07 2022-06-03 北京大学 一种多场景硫化氢气体含量在线监测方法及监测装置

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