WO2024143122A1 - 分光分析装置及び分光分析方法 - Google Patents

分光分析装置及び分光分析方法 Download PDF

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Publication number
WO2024143122A1
WO2024143122A1 PCT/JP2023/045761 JP2023045761W WO2024143122A1 WO 2024143122 A1 WO2024143122 A1 WO 2024143122A1 JP 2023045761 W JP2023045761 W JP 2023045761W WO 2024143122 A1 WO2024143122 A1 WO 2024143122A1
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Prior art keywords
unit
concentration
analysis
component
liquid sample
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PCT/JP2023/045761
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English (en)
French (fr)
Japanese (ja)
Inventor
慧 若林
美岐子 内ケ島
庸行 中
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Horiba Ltd
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Horiba Ltd
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Priority to JP2024567690A priority Critical patent/JPWO2024143122A1/ja
Priority to CN202380088677.2A priority patent/CN120418637A/zh
Priority to EP23911902.7A priority patent/EP4644873A1/en
Publication of WO2024143122A1 publication Critical patent/WO2024143122A1/ja
Anticipated expiration legal-status Critical
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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
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • 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
    • 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
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/645—Specially adapted constructive features of fluorimeters
    • 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
    • G01N2021/1738—Optionally different kinds of measurements; Method being valid for different kinds of measurement
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/12—Circuits of general importance; Signal processing
    • G01N2201/124—Sensitivity

Definitions

  • the present invention relates to a spectroscopic analysis device and a spectroscopic analysis method that irradiates a substance with primary light and analyzes the secondary light generated from the substance.
  • Patent Document 1 discloses an analytical device that performs Raman spectroscopy and fluorescence spectroscopy.
  • a spectroscopic analysis device includes a first analysis unit that performs fluorescence spectroscopic analysis and/or absorption spectroscopic analysis of a first component contained in a liquid sample using secondary light generated from the liquid sample irradiated with primary light, a second analysis unit that performs Raman spectroscopic analysis of a second component contained in the liquid sample using secondary light generated from the liquid sample irradiated with primary light, a concentration measurement unit that measures the concentrations of the first component and the second component contained in the liquid sample, and a control unit, and the control unit causes the first analysis unit or the second analysis unit to perform an analysis depending on the concentration measured by the concentration measurement unit.
  • the spectroscopic analysis device measures the concentrations of a first component and a second component contained in a liquid sample, and causes a first analysis unit that performs fluorescence spectroscopic analysis and/or absorption spectroscopic analysis, or a second analysis unit that performs Raman spectroscopic analysis, to perform analysis according to the measured concentrations.
  • a first analysis unit that performs fluorescence spectroscopic analysis and/or absorption spectroscopic analysis
  • Raman spectroscopic analysis the first component can be analyzed with high accuracy when the concentration of the first component is low.
  • Raman spectroscopic analysis the second component can be analyzed with high accuracy when the concentration of the second component is high.
  • the first component and the second component are different from each other, and the concentration of the first component is lower than the concentration of the second component.
  • the first component and the second component are the same.
  • the first component and the second component are the same component.
  • the spectroscopic analysis device can analyze a specific component contained in a liquid sample over a wide concentration range. When the concentration of the specific component changes over time, the change in concentration of the specific component over time can be obtained.
  • the spectroscopic analysis device performs fluorescence spectroscopic analysis or absorption spectroscopic analysis of the liquid sample when the concentration of a first component contained in the liquid sample is low, and performs Raman spectroscopic analysis of the liquid sample when the concentration of a second component contained in the liquid sample is high.
  • the spectroscopic analysis device idles the first analysis unit when the concentration of the first component is close to a value appropriate for fluorescence spectroscopy or absorption spectroscopy.
  • concentration of the first component becomes a value appropriate for fluorescence spectroscopy or absorption spectroscopy
  • analysis is immediately performed in the first analysis unit, thereby enabling fluorescence spectroscopy or absorption spectroscopy to be performed at an appropriate time.
  • the spectroscopic analysis device idles the second analysis unit when the concentration of the second component is close to a value appropriate for Raman spectroscopy.
  • the concentration of the second component becomes a value appropriate for Raman spectroscopy
  • analysis is immediately performed in the second analysis unit, thereby enabling Raman spectroscopy to be performed at an appropriate time.
  • the spectroscopic analysis device calibrates the first analysis unit when the concentration of the first component contained in the liquid sample is low, and calibrates the second analysis unit when the concentration of the second component contained in the liquid sample is high. Calibration of the first analysis unit is performed in a state appropriate for performing fluorescence spectroscopic analysis or absorption spectroscopic analysis, and the first analysis unit can be calibrated appropriately. Calibration of the second analysis unit is performed in a state appropriate for performing Raman spectroscopic analysis, and the second analysis unit can be calibrated appropriately.
  • the first threshold value and the second threshold value are the same threshold value.
  • the first threshold and the second threshold are the same. Depending on the concentration of the component contained in the liquid sample, one of the analysis methods is selectively performed.
  • a spectroscopic analysis method is characterized in that it measures the concentrations of a first component and a second component contained in a liquid sample, and when the concentration of the first component is low, performs fluorescence spectroscopic analysis and/or absorption spectroscopic analysis using secondary light generated from the liquid sample irradiated with primary light, and when the concentration of the second component is high, performs Raman spectroscopic analysis using secondary light generated from the liquid sample irradiated with primary light.
  • the concentrations of a first component and a second component contained in a liquid sample are measured, and when the concentration of the first component is low, fluorescence spectroscopy and/or absorption spectroscopy is performed on the first component, and when the concentration of the second component is high, Raman spectroscopy is performed on the second component. It is possible to analyze the liquid sample using an appropriate analytical method depending on the concentration of the component to be analyzed.
  • the present invention has excellent effects, such as being able to analyze components contained in liquid samples over a wide concentration range.
  • 1 is a block diagram showing an example of the configuration of a spectroscopic analysis device according to a first embodiment.
  • 4 is a block diagram showing an example of an internal functional configuration of a control unit;
  • 5 is a flowchart illustrating an example of a procedure of a process for analyzing a first component, which is executed by the spectroscopic analysis apparatus according to the first embodiment.
  • 5 is a flowchart illustrating an example of a procedure of a process for analyzing a second component, which is executed by the spectroscopic analysis device according to the first embodiment.
  • 10 is a flowchart showing an example of a procedure of an analysis process executed by a spectroscopic analysis device according to a second embodiment.
  • 10 is a flowchart showing an example of a procedure for a calibration process executed by a spectroscopic analysis apparatus.
  • the first analysis unit 1 includes a first light source 11, a first spectroscope 12, a first detection unit 13, and an information processing unit 4.
  • the first light source 11 generates primary light, which is irradiated onto the liquid sample 61 in the optical cell 62.
  • secondary light is generated from the liquid sample 61.
  • the secondary light includes fluorescence.
  • the secondary light is incident on the first spectroscope 12.
  • the first spectroscope 12 separates the incident secondary light and emits the separated secondary light.
  • the separated secondary light is incident on the first detection unit 13.
  • the first detection unit 13 includes a photodetector and detects the incident light.
  • the first detection unit 13 includes, as the photodetector, a photodiode, an image sensor, or a photomultiplier tube, for example.
  • the first detection unit 13 may include an amplifier.
  • the concentration measurement unit 3 includes a third light source 31, a third detection unit 32, and an information processing unit 4.
  • the information processing unit 4 is shared by the first analysis unit 1, the second analysis unit 2, and the concentration measurement unit 3.
  • the third light source 31 generates light, which is irradiated onto the liquid sample 61 in the optical cell 62.
  • the third detection unit 32 detects transmitted light that has passed through the liquid sample 61, or scattered light that has been scattered by the liquid sample 61.
  • the third detection unit 32 includes a photodetector.
  • the third detection unit 32 includes, as the photodetector, for example, a photodiode, an image sensor, or a photomultiplier tube.
  • the third detection unit 32 may include an amplifier.
  • the first analysis unit 1 may be configured to perform absorption spectroscopy instead of fluorescence spectroscopy.
  • the first analysis unit 1 performs ultraviolet-visible spectroscopy as absorption spectroscopy.
  • the first analysis unit 1 may be configured to perform both fluorescence spectroscopy and absorption spectroscopy.
  • the first analysis unit 1 or the second analysis unit 2 may also have the function of the concentration measurement unit 3.
  • the spectroscopic analysis device 10 does not have a concentration measurement unit 3 separate from the first analysis unit 1 or the second analysis unit 2, and the first analysis unit 1 or the second analysis unit 2 also operates as the concentration measurement unit 3.
  • the first analysis unit 1, the second analysis unit 2, and the concentration measurement unit 3 may each have their own information processing unit, rather than sharing the information processing unit 4.
  • a common light source may be used as the first light source 11, the second light source 21, and the third light source 31.
  • the control unit 5 determines whether the concentration of the first component measured by the concentration measurement unit 3 is equal to or less than the first threshold value (S12).
  • the first threshold value is determined in advance and stored in the memory unit 54.
  • the calculation unit 51 receives the concentration input from the information processing unit 4 through the interface unit 57, and compares the received concentration with the first threshold value stored in the memory unit 54.
  • the control unit 5 causes the first analysis unit 1 to perform analysis (S13).
  • the calculation unit 51 transmits a control signal from the interface unit 57 to the first analysis unit 1 to cause the first analysis unit 1 to perform analysis.
  • the first analysis unit 1 performs fluorescence spectroscopy analysis of the first component contained in the liquid sample 61.
  • the first light source 11 emits light, and the liquid sample 61 is irradiated with primary light from the first light source 11. Secondary light from the liquid sample 61 enters the first spectroscope 12, which separates the secondary light. The separated secondary light enters the first detection unit 13.
  • the first detection unit 13 detects the separated secondary light, and inputs the intensity of the detected secondary light to the information processing unit 4.
  • the control unit 5 may perform processing to cause the first analysis unit 1 to perform analysis when the concentration of the first component is less than the first threshold.
  • the first component is a trace component contained in the liquid sample 61 in trace amounts.
  • the concentration of the first component is 0.1 mg/mL or less.
  • a first threshold is determined in advance so that a concentration of the first component of 0.1 mg/mL or less can be determined by fluorescence spectroscopy.
  • the information processing unit 4 performs a process of determining the concentration of the first component contained in the liquid sample 61 by absorption spectroscopy.
  • the first analysis unit 1 determines the concentration of the first component with higher accuracy than the concentration measurement unit 3.
  • the information processing unit 4 stores the results of the fluorescence spectroscopy or absorption spectroscopy.
  • the control unit 5 causes the first analysis unit 1 to idle (S15).
  • the calculation unit 51 sends a control signal from the interface unit 57 to the first analysis unit 1 to cause the first analysis unit 1 to idle.
  • the control unit 5 applies power to the first light source 11, the first spectrometer 12, and the first detection unit 13.
  • the first analysis unit 1 By idling the first analysis unit 1, it becomes possible for the first analysis unit 1 to immediately perform fluorescence spectroscopy or absorption spectroscopy when the concentration of the first component decreases and falls below the first threshold. This makes it possible to perform fluorescence spectroscopy or absorption spectroscopy at an appropriate time.
  • the information processing unit 4 performs information processing for Raman spectroscopic analysis based on the intensity and Raman shift of the Raman scattered light contained in the secondary light. More specifically, the information processing unit 4 performs processing to identify the concentration of the second component contained in the liquid sample 61 by Raman spectroscopic analysis.
  • the information processing unit 4 pre-stores the Raman shift caused by the second component, identifies the intensity of the Raman scattered light caused by the second component, and calculates the concentration of the second component based on the intensity of the Raman scattered light. For example, the information processing unit 4 pre-stores a calibration curve that represents the relationship between the intensity and concentration of the Raman scattered light caused by the second component.
  • the information processing unit 4 calculates the concentration of the second component by identifying the concentration corresponding to the intensity of the Raman scattered light based on the calibration curve.
  • the spectroscopic analysis device 10 can perform fluorescence spectroscopic analysis or absorption spectroscopic analysis with high accuracy, so that the first component contained in a trace amount in the liquid sample 61 can be analyzed with high accuracy. For example, it becomes possible to accurately determine the concentration of the first component.
  • Raman spectroscopic analysis makes it possible to analyze components with high concentrations. By performing Raman spectroscopic analysis when the concentration of the second component is high, it becomes possible to accurately analyze the second component contained in the liquid sample 61 at a high concentration. For example, it becomes possible to accurately determine the concentration of the second component. In this way, the spectroscopic analysis device 10 can analyze components in the liquid sample 61 over a wide concentration range.
  • the control unit 5 determines whether the concentration of the specific component measured by the concentration measurement unit 3 is less than the threshold value (S32).
  • the threshold value corresponds to a value where the first threshold value and the second threshold value coincide.
  • the threshold value is determined in advance and stored in the memory unit 54.
  • the calculation unit 51 compares the concentration input from the information processing unit 4 with the threshold value stored in the memory unit 54.
  • the information processing unit 4 performs information processing for fluorescence spectroscopy. More specifically, the information processing unit 4 performs processing to identify the concentration of a specific component contained in the liquid sample 61 by fluorescence spectroscopy. The information processing unit 4 pre-stores the wavelength of the fluorescence caused by the specific component, identifies the intensity of the fluorescence caused by the specific component, and calculates the concentration of the specific component based on the fluorescence intensity. In a form in which the first analysis unit 1 performs absorption spectroscopy, the information processing unit 4 performs processing to identify the concentration of a specific component contained in the liquid sample 61 by absorption spectroscopy. The information processing unit 4 stores the results of the fluorescence spectroscopy or absorption spectroscopy.
  • the control unit 5 determines whether the concentration of the specific component measured by the concentration measurement unit 3 is within a predetermined second range (S34).
  • the second range is a range of values that are less than the threshold and close to the threshold.
  • the second range is a range that exceeds a predetermined value that is less than the threshold and is less than the threshold.
  • Data indicating the second range is pre-stored in the memory unit 54.
  • the calculation unit 51 compares the concentration with the second range. If the concentration is within the second range (S34: YES), the control unit 5 causes the second analysis unit 2 to idle (S35).
  • the control unit 5 causes the second analysis unit 2 to perform an analysis (S36). At this time, the control unit 5 does not cause the first analysis unit 1 to perform an analysis.
  • the calculation unit 51 sends a control signal from the interface unit 57 to the second analysis unit 2 to cause the second analysis unit 2 to perform an analysis.
  • the second analysis unit 2 performs Raman spectroscopic analysis of the liquid sample 61. Note that the control unit 5 may perform a process to cause the second analysis unit 2 to perform an analysis if the concentration exceeds the threshold value.
  • the control unit 5 determines whether the concentration of the specific component measured by the concentration measurement unit 3 is within a predetermined first range (S37).
  • the first range is a range of values that exceed the threshold and are close to the threshold.
  • the first range is a range that is smaller than a predetermined value that exceeds the threshold and exceeds the threshold.
  • Data indicating the first range is pre-stored in the memory unit 54.
  • the calculation unit 51 compares the concentration with the first range. If the concentration is within the first range (S37: YES), the control unit 5 causes the first analysis unit 1 to idle (S38).

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  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Physics & Mathematics (AREA)
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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
PCT/JP2023/045761 2022-12-28 2023-12-20 分光分析装置及び分光分析方法 Ceased WO2024143122A1 (ja)

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JP2024567690A JPWO2024143122A1 (https=) 2022-12-28 2023-12-20
CN202380088677.2A CN120418637A (zh) 2022-12-28 2023-12-20 分光分析装置和分光分析方法
EP23911902.7A EP4644873A1 (en) 2022-12-28 2023-12-20 Spectroscopic analysis device and spectroscopic analysis method

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