WO2023112358A1 - 分光光度計 - Google Patents

分光光度計 Download PDF

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Publication number
WO2023112358A1
WO2023112358A1 PCT/JP2022/022588 JP2022022588W WO2023112358A1 WO 2023112358 A1 WO2023112358 A1 WO 2023112358A1 JP 2022022588 W JP2022022588 W JP 2022022588W WO 2023112358 A1 WO2023112358 A1 WO 2023112358A1
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WO
WIPO (PCT)
Prior art keywords
light
sample
light source
excitation wavelength
intensity
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2022/022588
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English (en)
French (fr)
Japanese (ja)
Inventor
隆宏 玉木
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
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Shimadzu Corp
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Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP2023567520A priority Critical patent/JP7837348B2/ja
Priority to CN202280059048.2A priority patent/CN117881949A/zh
Priority to US18/718,017 priority patent/US20250052613A1/en
Publication of WO2023112358A1 publication Critical patent/WO2023112358A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/10—Arrangements of light sources specially adapted for spectrometry or colorimetry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/0205—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
    • G01J3/0218—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows using optical fibers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/0205—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
    • G01J3/0254—Spectrometers, other than colorimeters, making use of an integrating sphere
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/30—Measuring the intensity of spectral lines directly on the spectrum itself
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27—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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G01J2003/421—Single beam

Definitions

  • the present invention relates to spectrophotometers.
  • photoreaction quantum yield is used to evaluate the reaction efficiency of photoreactive substances such as photocatalysts.
  • the photoreaction quantum yield is calculated as the ratio of the number of molecules produced by the photoreaction of a photoreactant to the number of photons absorbed by the photoreactant.
  • the number of photons absorbed by the photoreactant is measured with a spectrophotometer, and the number of molecules generated by the photoreaction of the photoreactant is measured with a gas chromatograph or a liquid chromatograph.
  • Patent Document 1 describes a spectrophotometer used to measure the number of photons absorbed by a photoreactive substance.
  • This device comprises a sample cell, an excitation light source for irradiating the sample cell with excitation light, a measurement light source for irradiating the sample cell with measurement light, and a spectroscopic detection section for detecting the measurement light passing through the sample cell by separating the wavelengths of the measurement light. and each part is arranged so that the optical path of the excitation light and the optical path of the measurement light are perpendicular to each other.
  • the excitation light source is a monochromatic light source, such as an LED
  • the measurement light source is a white light source, such as a xenon lamp.
  • the excitation light source the number of photons emitted from the light source and irradiated onto the sample (the number of irradiation photons) is known by preliminary measurement using an illuminometer or the like.
  • a sample cell containing a sample is irradiated only with measurement light, and the transmitted light is detected to obtain a first absorbance spectrum.
  • the sample cell is irradiated with the excitation light, the sample cell is irradiated with the measurement light in the same manner as described above, and the transmitted light is detected to obtain the second absorbance spectrum.
  • the difference between the first absorbance spectrum and the second absorbance spectrum reflects the change in light absorbance due to the reaction of the photoreactive substance in the sample.
  • the number of photons per unit time absorbed by the photoreactive substance in the sample is obtained by multiplying the number of irradiation photons irradiated in the unit time by the change in the light absorptance of the photoreactive substance.
  • Photoreactive substances are used in various products such as cosmetics and semiconductor photocatalysts, and their forms are various, such as sol, gel, and thin film.
  • a heterogeneous liquid sample such as a sol or gel or a thin film sample
  • part of the light passing through the sample is scattered (forward scattering). Correct light absorption cannot be obtained.
  • conventional spectrophotometers have the problem that the objects to be measured are limited to homogeneous liquid samples in which such light scattering does not occur.
  • the problem to be solved by the present invention is to provide a spectrophotometer capable of measuring the number of photons of light absorbed by a heterogeneous liquid sample or thin film sample.
  • a spectrophotometer which has been made to solve the above problems, a light source that emits light in a wavelength band including an excitation wavelength that causes a photoreaction in a target substance in a sample, wherein the number of photons in the light of the excitation wavelength emitted from the light source is known; an integrating sphere having a light entrance for receiving light emitted from the light source, and a light exit located at a position off the optical axis of the light incident on the light entrance; a sample placement portion provided at the light entrance; a light intensity measuring unit that measures the intensity of the light of the excitation wavelength emitted from the light exit port.
  • the spectrophotometer uses a single light source that combines the functions of a conventional excitation light source and measurement light source.
  • this spectrophotometer first, light is emitted from a light source without placing a sample in the sample placement section, and the light intensity of the excitation wavelength is measured by the light intensity measurement section. Subsequently, the sample is placed in the sample placement portion provided at the light entrance of the integrating sphere, and light is irradiated from the light source.
  • the spectrophotometer based on the intensity of the excitation wavelength light when the sample is not placed and the intensity of the excitation wavelength light when the sample is placed, the target substance contained in the sample, The absorptivity of the light of the excitation wavelength is obtained, and the product of the number of photons per unit time of the light of the excitation wavelength emitted from the light source and the absorptance of the light is the light of the excitation wavelength absorbed by the target substance. Calculate the number of photons per unit time.
  • the light intensity measurement unit measures the intensity of the light of the excitation wavelength contained in the transmitted light including the forward scattered light from the sample, and the absorbance is obtained based on the intensity. The number of photons of light absorbed by a sample or thin film sample can be measured.
  • FIG. 1 is a schematic configuration diagram of an embodiment of a spectrophotometer according to the present invention
  • FIG. FIG. 4 is a diagram for explaining a configuration for measuring total energy of light emitted from a light source
  • 4 is a flow chart of an example of a measurement procedure using the spectrophotometer of this embodiment.
  • a spectrophotometer 1 according to the present invention is used to calculate the number of photons of light absorbed by a photoreactive substance, which is necessary for calculating the photoreaction quantum yield of a photoreactive substance such as a photocatalyst.
  • FIG. 1 shows a schematic configuration of the spectrophotometer 1 of this embodiment.
  • the spectrophotometer 1 is composed of a light source 10 , an integrating sphere 20 , a spectral detection section 30 and a control/processing section 40 .
  • the light source 10 emits light in a wavelength band including an excitation wavelength that causes a photoreaction in the target substance (photoreactive substance) contained in the sample to be measured.
  • a light source called a white LED for example, a spectral total radiant flux standard LED described in Non-Patent Document 1 is used as the light source 10 .
  • the integrating sphere 20 has a light entrance opening 21 through which the light emitted from the light source 10 enters, and a light exit opening 22 through which the light exits from inside the integrating sphere 20 .
  • the integrating sphere 20 of the present embodiment is arranged so that the central axis C1 of light emitted from the light source 10 and incident on the light entrance 21 is orthogonal to the central axis C2 of light emitted from the light exit 22 to the spectral detection section 30.
  • a light entrance port 21 and a light exit port 22 are provided.
  • a sample placement portion 23 is provided at the light entrance 21 .
  • the sample placement section 23 includes a sample cell for containing a liquid sample and a mechanism for fixing a film-like sample.
  • the light exit port 22 and the entrance of the spectral detection unit 30 are connected by an optical fiber 24 .
  • the spectral detection unit 30 has a spectroscope 31 that separates the wavelength of the light emitted from the light exit port 22, and a photodetector 32 that detects the light after the wavelength separation by the spectroscope.
  • a diffraction grating is used for the spectroscope 31, for example.
  • the photodetector 32 for example, a linear sensor having a plurality of detection elements arranged in the direction in which the wavelength-separated light spreads is used.
  • the control/processing unit 40 has a storage unit 41 .
  • the storage unit 41 stores data such as the total energy of the light emitted from the light source 10, the emission spectrum, and the number of photons for each wavelength.
  • the control/processing unit 40 also includes a measurement control unit 42 and an absorption photon number calculation unit 43 as functional blocks.
  • the entity of the control/processing unit 40 is a general personal computer, and the functional blocks described above are realized by executing a pre-installed spectroscopic measurement program.
  • an input unit 48 such as a keyboard and a mouse
  • a display unit 49 such as a liquid crystal display are connected to the control/processing unit 40 .
  • the number of photons of the excitation wavelength light emitted from the light source 10 is obtained.
  • the total energy of light emitted from the light source 10 is measured (step 1). This measurement is performed by causing the light emitted from the light source 10 to enter an illuminometer (also called a power sensor) 50, as shown in FIG.
  • the light source 10 is returned to the position shown in FIG.
  • the light emitted from the is introduced into the spectral detection section 30 .
  • the introduced light is wavelength-separated by the spectroscope 31, and the intensity of each wavelength is measured by the photodetector 32.
  • FIG. 1 the emission spectrum of the light source 10 (light intensity for each wavelength per unit time) is obtained (step 2).
  • the total energy of the light emitted from the light source 10 obtained in step 1, the emission spectrum of the light source 10 obtained in step 2, and the energy of one photon at each wavelength (hc/ ⁇ , where h is Planck's constant, c is the light (where ⁇ is the wavelength)
  • the number of photons for each wavelength of the light emitted from the light source 10 is calculated (step 3) and stored in the storage unit 41 .
  • steps 1 to 3 should be performed once when the light source 10 is installed, and the data on the number of photons for each wavelength should be stored in the storage unit 41. , need not be performed each time a sample is measured.
  • the measurement control unit 42 irradiates the sample with light from the light source 10 .
  • the light that has passed through the sample enters the integrating sphere 20 through the light entrance 21 and is reflected once or several times.
  • Light incident on the spectral detection unit 30 is wavelength-separated by the spectroscope 31 and detected by the photodetector 32 .
  • the photodetector 32 outputs a signal representing the intensity of light of each wavelength incident on each detection element of the photodetector 32 .
  • the measurement control unit 42 reads the output signal from the photodetector 32 (data on the intensity of light detected by each detection element) and stores it in the storage unit 41 .
  • the absorbed photon number calculation unit 43 creates transmitted light spectrum data from the data (step 5).
  • the absorbed photon number calculation unit 43 After creating the transmitted light spectrum data, the absorbed photon number calculation unit 43 further creates absorbance spectrum data from the emission spectrum data acquired in step 2 and the transmitted light spectrum data acquired in step 5 (step 6), and displays the data on the display unit. 49 displays the absorbance spectrum.
  • the absorbed photon number calculator 43 calculates the number of absorbed photons according to the following equation (step 7).
  • Ei is the amount of irradiation light per unit time
  • T is the transmittance of the sample
  • t is the time.
  • the wavelength range to be integrated in the above equation (1) is about the same as the peak in the absorbance spectrum (for example, ⁇ 10 nm centered on the excitation wavelength of the target substance).
  • the value is displayed on the screen of the display unit 49 together with the absorbance spectrum data.
  • the measurement control unit 42 determines whether or not the elapsed time from the start of measurement has reached the time set in advance by the user. If the elapsed time from the start of measurement has not yet reached the set time (NO in step 8), the process returns to step 5 and the same processing as above is performed. If the elapsed time from the start of measurement has reached the set time (YES at step 8), the measurement is terminated.
  • a sample sealed in a sample cell is irradiated with light from a measurement light source, and the intensity of the light that passes through the sample cell is measured by a spectrophotometer. It has not been possible to measure samples that scatter the measurement light passing through the cell (for example, inhomogeneous liquid samples or film-like samples).
  • the spectrophotometer 1 of this embodiment uses a single light source 10 that functions both as a measurement light source and as an excitation light source in a conventional spectrophotometer.
  • an integrating sphere 20 is used, and a sample placement portion 23 is provided at the light entrance 21 thereof, and a sample is placed there.
  • the light is made to enter the integrating sphere 20, and is reflected inside it one or more times, The light is made incident on the spectral detection unit 30 . Therefore, it is possible to calculate the number of absorbed photons during the photoreaction of the target substance contained in non-homogeneous liquid samples and film samples, which could not be measured by conventional spectrophotometers. can.
  • a white LED is used as the light source 10 in the above embodiment, other types of white light sources may be used.
  • a monochromatic light source can also be used as the light source 10 .
  • the light emitted from the integrating sphere 20 is also monochromatic light, so there is no need to use a spectroscopic element. can be used.
  • a monochromatic light source is used as the light source 10
  • light is emitted from the monochromatic light source from the light source 10 in a state in which no sample is placed on the sample placing portion 23 and a state in which a sample is placed, respectively.
  • the absorptance of the light at that wavelength is obtained.
  • the light entrance 21 and the light exit are arranged so that the central axis of the light entering the light entrance 21 from the light source 10 is perpendicular to the central axis of the light taken into the optical fiber 24 from the light exit 22 . 22 is used, but the light entrance 21 and the light exit 22 can be placed at appropriate positions as long as the light exit 22 is not positioned on the central axis of the light entering the light entrance 21 from the light source 10. should be set to
  • a spectrophotometer comprises a light source that emits light in a wavelength band including an excitation wavelength that causes a photoreaction in a target substance in a sample, wherein the number of photons in the light of the excitation wavelength emitted from the light source is known; an integrating sphere having a light entrance for receiving light emitted from the light source, and a light exit located at a position off the optical axis of the light incident on the light entrance; a sample placement portion provided at the light entrance; a light intensity measuring unit that measures the intensity of the light of the excitation wavelength emitted from the light exit port.
  • the spectrophotometer according to item 1 uses a single light source that combines the functions of a conventional excitation light source and measurement light source.
  • this spectrophotometer first, light is emitted from a light source without placing a sample in the sample placement section, and the light intensity of the excitation wavelength is measured by the light intensity measurement section. Subsequently, the sample is placed in the sample placement portion provided at the light entrance of the integrating sphere, and light is irradiated from the light source.
  • the target substance contained in the sample is determined.
  • the absorptivity of the light of the excitation wavelength is obtained, and the number of photons of the light of the excitation wavelength absorbed by the target substance is obtained by multiplying the number of photons of the light of the excitation wavelength emitted from the light source by the absorptance of the light.
  • the light intensity measurement unit measures the intensity of the light of the excitation wavelength contained in the transmitted light including the forward scattered light by the sample, and the absorbance is obtained based on the intensity. The number of photons of light absorbed by a liquid sample or thin film sample can be measured.
  • the arithmetic processing unit further calculates the number of photons of light absorbed by the target substance based on the number of photons of light of the excitation wavelength and the absorptivity.
  • the spectrophotometer according to the second term simply obtains the absorptance of the excitation wavelength light by the target substance
  • the spectrophotometer according to the third term simply obtains the number of photons of the excitation wavelength light absorbed by the target substance. be able to.
  • the light source is a white LED light source
  • the light intensity measuring unit includes a spectroscope for wavelength-separating the light emitted from the light exit port, and a photodetector for detecting the light wavelength-separated by the spectroscope.
  • the absorbance spectrum of the wavelength band including the excitation wavelength is obtained, and the number of photons of light absorbed by the target substance is calculated based on the absorbance peak centering on the wavelength band.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Mathematical Physics (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Investigating Or Analysing Materials By Optical Means (AREA)
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PCT/JP2022/022588 2021-12-14 2022-06-03 分光光度計 Ceased WO2023112358A1 (ja)

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Application Number Priority Date Filing Date Title
JP2023567520A JP7837348B2 (ja) 2021-12-14 2022-06-03 分光光度計
CN202280059048.2A CN117881949A (zh) 2021-12-14 2022-06-03 分光光度计
US18/718,017 US20250052613A1 (en) 2021-12-14 2022-06-03 Spectrophotometer

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JP2021-202853 2021-12-14
JP2021202853 2021-12-14

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US20250052613A1 (en) 2021-12-14 2025-02-13 Shimadzu Corporation Spectrophotometer

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009051222A1 (ja) * 2007-10-18 2009-04-23 Shiseido Company, Ltd. 紫外線防御効果の評価方法、評価装置、評価プログラム、及び該プログラムが記録された記録媒体
JP2018109674A (ja) * 2016-12-28 2018-07-12 堺化学工業株式会社 蛍光体含有多層膜シート、並びに発光装置
WO2020022339A1 (ja) * 2018-07-26 2020-01-30 住友化学株式会社 樹脂組成物
JP2020159867A (ja) * 2019-03-27 2020-10-01 国立研究開発法人物質・材料研究機構 分光測定装置、および、分光測定プログラム

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EP3211462A4 (en) * 2014-10-24 2018-07-11 Denka Company Limited Wavelength converter, light-emitting device using same, and production method for wavelength converter
EP3708902B1 (en) * 2015-06-24 2023-05-24 Seoul Semiconductor Co., Ltd. White light source system
JP7358985B2 (ja) * 2017-06-01 2023-10-11 コニカミノルタ株式会社 分光測色計
CN113178437B (zh) * 2017-12-21 2023-08-11 厦门市三安光电科技有限公司 一种白光led封装结构以及白光源系统
WO2021166310A1 (ja) * 2020-02-20 2021-08-26 株式会社島津製作所 光反応評価装置およびフォトン数算出方法
US20250052613A1 (en) 2021-12-14 2025-02-13 Shimadzu Corporation Spectrophotometer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009051222A1 (ja) * 2007-10-18 2009-04-23 Shiseido Company, Ltd. 紫外線防御効果の評価方法、評価装置、評価プログラム、及び該プログラムが記録された記録媒体
JP2018109674A (ja) * 2016-12-28 2018-07-12 堺化学工業株式会社 蛍光体含有多層膜シート、並びに発光装置
WO2020022339A1 (ja) * 2018-07-26 2020-01-30 住友化学株式会社 樹脂組成物
JP2020159867A (ja) * 2019-03-27 2020-10-01 国立研究開発法人物質・材料研究機構 分光測定装置、および、分光測定プログラム

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CN117881949A (zh) 2024-04-12
US20250052613A1 (en) 2025-02-13
JP7837348B2 (ja) 2026-03-30
JPWO2023112358A1 (https=) 2023-06-22

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