WO2019069526A1 - Spectromètre - Google Patents

Spectromètre Download PDF

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Publication number
WO2019069526A1
WO2019069526A1 PCT/JP2018/026263 JP2018026263W WO2019069526A1 WO 2019069526 A1 WO2019069526 A1 WO 2019069526A1 JP 2018026263 W JP2018026263 W JP 2018026263W WO 2019069526 A1 WO2019069526 A1 WO 2019069526A1
Authority
WO
WIPO (PCT)
Prior art keywords
slit
light
aperture
plate
spectroscope
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/JP2018/026263
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English (en)
Japanese (ja)
Inventor
小田　竜太郎
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
Original Assignee
Shimadzu Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Publication of WO2019069526A1 publication Critical patent/WO2019069526A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • G01J3/04—Slit arrangements slit adjustment
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/443—Emission spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/12—Generating the spectrum; Monochromators
    • G01J3/18—Generating the spectrum; Monochromators using diffraction elements, e.g. grating

Definitions

  • the present invention relates to a spectrometry apparatus for analyzing a sample in a sample cell by irradiating light from a light source to a sample cell, and splitting the light from the sample cell with a spectrometer and guiding the light to a light detector for detection. It is a thing.
  • FIG. 8 shows an example of a conventional spectrometer.
  • This spectrometer measures the light from the light source 2 to the sample cell 6, guides the light transmitted through the sample cell 6 to the light detector 16, and measures the absorbance of the light of a specific wavelength of the sample in the sample cell 6. It is.
  • a mirror 4 is provided as an irradiation optical system for guiding the light from the light source 2 to the sample cell 6, and a mirror 8, a slit 10a, and a measurement optical system for guiding the light transmitted through the sample cell 6 to the light detector 16.
  • a diffraction grating 14 is provided.
  • the slit 10 a is provided in the slit plate 10.
  • the slit plate 10 is disposed between the mirror 8 and the diffraction grating 14.
  • the light emitted from the light source 2 is irradiated to the sample cell 6 by the mirror 4, and the light transmitted through the sample cell 6 is reflected by the mirror 8, passes through the slit 10 a, and is dispersed by the diffraction grating 14 onto the light detector 16. It is imaged and detected.
  • the sample cell 6 is connected to, for example, the downstream side of the analysis column of the separation channel of the liquid chromatograph, and a liquid containing the sample separated for each component in the separation column flows.
  • the photodetector 16 detects a temporal change in the intensity of light transmitted through the sample cell 6, and detects the component concentration of each sample contained in the sample by the temporal change in absorbance based on the detected data. .
  • the width of a slit provided in front of a spectrometer is configured to be changeable (see, for example, Patent Document 1).
  • the slit width is narrowed, the light entering the spectrometer is limited to the light near the center of the light beam of the measurement light, and the wavelength resolution of the spectrometer is enhanced.
  • increasing the slit width increases the amount of measurement light incident on the spectrometer and increases the detection sensitivity of the measurement (signal intensity), but also takes in light at a position distant from the center of the measurement light beam. The resolution is reduced.
  • the numerical aperture of a spectroscope is the range of the spectroscope of the spectroscope used for spectroscopy. When the numerical aperture is reduced, spectroscopy is performed using a limited range on the center side of the spectral surface, and when the numerical aperture is increased, spectroscopy is performed using a wide range of the spectral surface.
  • the numerical aperture is increased, light dispersed in a wide range of the spectral surface of the spectroscope can be guided to the detector, and the detection sensitivity becomes high, but at a position of poor spectral accuracy away from the center of the spectral surface The wavelength resolution is lowered because the split light is also used. Conversely, if the numerical aperture is reduced, the wavelength resolution will be high but the detection sensitivity will be low.
  • the numerical aperture is set to a smaller value, even if the slit width is broadened to increase the detection sensitivity, only light incident on a narrow range of the spectral surface of the spectroscope can be used for measurement. Can not raise. That is, in the conventional apparatus, the high sensitivity measurement is limited in the spectrometric apparatus set to obtain high wavelength resolution, and the high wavelength resolution is set in the high sensitivity measurement possible. There was a problem that was not obtained.
  • an object of the present invention is to provide a spectrometry device capable of performing measurement with wavelength resolution or sensitivity according to purpose from measurement with high wavelength resolution to measurement with high sensitivity.
  • the present invention comprises a light source, a light detector, a sample cell made of a light transmitting material, for circulating or containing a sample, an irradiation optical system for guiding light from the light source to the sample cell, a sample cell And a measurement optical system having a spectroscope for separating light from the sample cell and guiding the light from the sample cell to the light detector, wherein the measurement optical systems have widths relative to one another.
  • a variable slit section for arranging a slit selected as a use slit among the slits on the optical path of light guided to the spectroscope, and a numerical aperture of the spectroscope corresponding to a width of the use slit It is characterized by having a numerical aperture adjustment part which changes into a thing.
  • the spectroscopic measurement device of the present invention can be applied to one in which the measurement optical system is configured to guide the light transmitted through the sample cell to the light detector.
  • the irradiation optical system is configured to take out the excitation component for exciting the sample contained in the sample cell among the light from the light source and guide it to the sample cell, and the measurement optical system separates the light from the sample cell
  • the present invention can also be applied to one configured to take out fluorescence components emitted from a sample by means of a light source and to guide it to a light detector.
  • the variable slit portion is composed of a light shielding slit plate disposed perpendicular to the light path of light guided to the spectroscope and provided with a plurality of slits having different widths, and a slit driving mechanism for driving the slit plate
  • the slit drive mechanism may drive the slit plate so that the slit selected as the use slit is on the optical path of the light guided to the spectroscope, in which case the numerical aperture adjustment unit It is composed of a light shielding aperture plate disposed perpendicular to the light path of light guided to the spectroscope and provided with apertures corresponding to the slits of the slit plate, and an aperture drive mechanism for driving the aperture plate.
  • the aperture drive mechanism may drive the aperture plate so that the aperture corresponding to the light is on the optical path of the light guided to the spectroscope.
  • One example of a preferred embodiment is one in which the aperture drive mechanism is configured to move the aperture plate in a direction perpendicular to the light path.
  • the aperture drive mechanism is configured to rotationally drive the aperture plate, and each aperture is provided on the same track on the aperture plate drawn by the aperture plate being rotationally driven. It is
  • the slit plate is held by the same holding member as the aperture plate, and the aperture drive mechanism drives the slit plate as the slit drive mechanism together with the aperture plate by driving the holding member.
  • the slit and the aperture can be changed by one drive mechanism, and the cost of the apparatus can be reduced and the apparatus can be miniaturized.
  • the numerical aperture of the spectroscope is disposed on the light path of the light guided to the spectroscope by the variable slit portion. Since the numerical aperture adjustment part which changes it into a thing according to the use slit is provided, the numerical aperture of a spectrometer can be made into the numerical aperture suitable for the width
  • FIG. 7 schematically shows still another embodiment of a spectrometry apparatus. It is a perspective view which shows an example of the slit variable mechanism and numerical aperture adjustment part in the Example. It is a block diagram which shows roughly an example of the conventional spectroscopy apparatus.
  • This spectrometric device irradiates the sample cell 6 with the light from the light source 2 composed of, for example, a deuterium lamp, disperses the light transmitted through the sample cell 6 with the spectroscope 14 and makes the light enter the light detector 16
  • the detection is performed to analyze the sample components flowing through the sample cell 6. For example, a sample which has passed through a separation column of liquid chromatograph flows in the sample cell 6.
  • a mirror 4 is provided as an illumination optical system for guiding light emitted from the light source 2 to the sample cell 6. Light emitted from the light source 2 is collected by the mirror 4 and guided to the sample cell 6.
  • a mirror 8, a slit plate 10, an aperture plate 12 and a spectroscope 14 are provided as a measurement optical system for guiding the light from the sample cell 6 to the light detector 16. The light transmitted through the sample cell 6 is reflected by the mirror 8, passes through the slit 10 a provided in the slit plate 10 and the aperture 12 a provided in the aperture plate 12, and enters the spectroscope 14 and is separated by the spectroscope 14 Light is directed to the light detector 16.
  • the spectroscope 14 is, for example, a diffraction grating.
  • the slit plate 10 disposed between the mirror 8 and the spectroscope 14 is provided with a plurality of slits 10 a in a light shielding plate member.
  • the slit plate 10 is disposed perpendicularly to the optical axis of the light guided from the mirror 8 to the spectroscope 14.
  • the aperture plate 12 disposed closer to the spectroscope 14 than the slit plate 10 between the mirror 8 and the spectroscope 14 has a plurality of apertures 12 a provided in a light shielding plate member. In this example, the aperture plate 12 is disposed in parallel with the slit plate 10.
  • the slit plate 10 is driven by the slit drive mechanism 11, and the slit drive mechanism 11 is controlled by the control unit 18.
  • the slit drive mechanism 11 drives the slit plate 10 based on a signal from the control unit 18 and arranges one of the plurality of slits 10 a provided in the slit plate 10 on the optical axis of the light from the mirror 8 Do.
  • the aperture plate 12 is driven by the aperture drive mechanism 13, and the aperture drive mechanism 13 is also controlled by the control unit 18.
  • the aperture drive mechanism 13 arranges the aperture 12a corresponding to the slit 10a disposed on the optical axis from the mirror 8 on the same optical axis based on the signal from the control unit 18.
  • variable slit portion An example of the configuration of the variable slit portion and the numerical aperture adjustment portion will be described with reference to FIG.
  • the slit plate 10 is formed of a flat plate-like member made of a light shielding material, and slits 10a-1, 10a-2 and 10a-3 having different widths are provided in a line in the vertical direction in the plane. ing.
  • the slit plate 10 is arranged perpendicularly to the optical axis so that the slits 10a-1, 10a-2 and 10a-3 are on a straight line perpendicular to the optical axis of the light from the mirror 8. .
  • the aperture plate 12 is also formed of a flat plate-like member made of a light shielding material like the slit plate 10, and the apertures 12a-1, 12a-2 and 12a- corresponding to the respective slits of the slit plate 10 in the plane thereof. 3 are provided in a line in the vertical direction.
  • the aperture plate 12 is disposed opposite to the slit plate 10 in parallel.
  • the aperture 12a-1 is disposed at a position corresponding to the slit 10a-1
  • the aperture 12a-2 is disposed at a position corresponding to the slit 10a-2
  • the aperture 12a-3 is disposed at a position corresponding to the slit 10a-3.
  • the corresponding position means a position where the slit of interest is disposed on the same optical path when the slit is disposed on the optical axis of the light from the mirror 8.
  • the size of each aperture 12a-1, 12a-2 and 12a-3 optimizes the numerical aperture of the spectroscope 14 when the target slit 10a-1, 10a-2 or 10a-3 is used The size is set.
  • the slit plate 10 and the aperture plate 12 are held by a spacer 20 which is a common holding member.
  • the spacer 20 is moved in the vertical direction by the vertical drive mechanism 22 to drive the slit plate 10 and the aperture plate 12 in the vertical direction.
  • the slit drive mechanism 11 and the aperture drive mechanism 13 shown in FIG. 1 are realized by the vertical drive mechanism 22.
  • Examples of the configuration of the vertical drive mechanism 22 include one that moves the spacer 20 up and down by rotating a ball screw with a motor.
  • the aperture 12a-1 is automatically disposed on the same optical axis, and when the slit 10a-2 is disposed, the automatic operation is performed. Specifically, the aperture 12a-2 is disposed on the same optical axis, and when the slit 10a-3 is disposed, the aperture 12a-3 is automatically disposed on the same optical axis.
  • the aperture 12a corresponding to the slit 10a is automatically arranged on the same optical axis, and the numerical aperture of the spectroscope 14 is used It is automatically adjusted to a suitable one for the slit 10a.
  • the slits 10 a-1, 10 a-2 and 10 a-3 and the apertures 12 a-1, 12 a-2 and 12 a-3 are respectively arranged in a line in the vertical direction.
  • 10a-2 and 10a-3 and the apertures 12a-1, 12a-2 and 12a-3 may be arranged in a line in the left-right direction.
  • the slit drive mechanism 11 and the aperture drive mechanism 13 can be realized by providing a mechanism for driving the slit plate 10 and the aperture plate 12 in the left-right direction instead of the vertical drive mechanism 22.
  • the slit 10 a and the aperture used by rotating the slit plate 10 and the aperture plate 12 by the rotation drive mechanism 26 there is one that switches 12a.
  • the slit plate 10 and the aperture plate 12 are both formed by a fan-shaped plate member and fixed to a common shaft 24.
  • the rotary drive mechanism 26 rotationally drives both the slit plate 10 and the aperture plate 12 at the same time by rotationally driving the shaft 24 to realize the slit drive mechanism 11 and the aperture drive mechanism 13 of FIG. 1.
  • the slits 10a-1, 10a-2 and 10a-3 are disposed on the path of the optical axis of the light from the mirror 8 which is drawn on the plane of the slit plate 10 as the slit plate 10 is rotationally driven.
  • the apertures 12a-1, 12a-2 and 12a-3 have corresponding slits 10a on the path of the optical axis of the light from the mirror 8 which is drawn on the plane of the aperture plate 12 when the aperture plate 12 is rotationally driven. It is disposed at a position facing -1, 10a-2 and 10a-3.
  • the aperture 12a corresponding to the slit 10a is automatically arranged on the same optical axis.
  • the numerical aperture of the spectroscope 14 is automatically adjusted to one suitable for the slit 10a used.
  • the slit drive mechanism 11 and the aperture drive mechanism 13 in FIG. 1 are commonly used by the vertical drive mechanism 22 or the rotary drive mechanism 26.
  • the slit drive mechanism 11 and the aperture drive mechanism 13 are separately provided. It may be an independent drive mechanism.
  • the numerical aperture adjustment unit is not limited to one that switches the aperture (aperture 12a) disposed on the optical axis of the light from the mirror 8 as in the example of FIG. 2 or FIG.
  • the incident area of the spectroscope 14 may be limited by the aperture plate 12.
  • the aperture plate 12 is composed of a pair of L-shaped plates 12-1 and 12-2, as shown in FIG.
  • the aperture drive mechanism 13 is provided independently of the slit drive mechanism 11, and the inner opening region (in the in-plane direction by moving the pair of L-shaped plates 12-1 and 12-2) Adjust the size of the aperture 12a.
  • the controller 18 controls the plates 12-1 and 12-2 through the aperture drive mechanism 13 so as to form an opening area 12a having a size corresponding to the size of the slit 10a disposed on the optical axis of the light from the mirror 8. Drive.
  • the slit plate 10 may be the same as the example of FIG. 2 or FIG. 3
  • FIG. 6 shows another embodiment of the spectrometer.
  • the spectrometer of this embodiment extracts a wavelength component (excitation light) corresponding to excitation light from the light emitted from the light source 30 and guides it to the sample cell 38, and detects the fluorescence emitted from the excited sample.
  • concentration of the specific component in the sample is measured by guiding it to 44 and measuring its fluorescence intensity.
  • a mirror 31, an entrance slit 32, a spectroscope 34, and an exit slit 36 are provided as an irradiation optical system for extracting excitation light from light from the light source 30 and guiding it to the sample cell 38.
  • a mirror 40, an entrance slit 10a, an aperture 12a, a spectroscope 42, and an exit slit 10b are provided as a measurement optical system for guiding the fluorescence emitted from the excited sample to the photodetector 44.
  • the inlet slit 10 a and the outlet slit 10 b are provided in one slit plate 10 as a variable slit portion.
  • the aperture 12 a is provided on the aperture plate 12 as a numerical aperture adjustment unit disposed closer to the spectroscope 42 than the slit plate 10.
  • the light emitted from the light source 30 is guided by the mirror 31 to the spectroscope 34 through the entrance slit 32 and dispersed, and only the wavelength component corresponding to the excitation light among the light dispersed by the spectroscope 34 is the exit slit 36.
  • the sample cell 38 is irradiated through.
  • the fluorescence emitted from the excited sample is reflected by the mirror 40 and guided to the spectroscope 42 through the entrance slit 10a and the aperture 12a. Of the light separated by the spectroscope 42, only the wavelength component corresponding to the fluorescence is guided to the light detector 44 through the exit slit 10b, and the intensity is detected.
  • the slit plate 10 in this example is formed of a disk-shaped plate-like member, and the inlet slits 10a-1, 10a-2 and 10a-3 arranged in the circumferential direction in the plane and the outlet slits corresponding to them. 10b-1, 10b-2 and 10b-3 are provided.
  • the center of the slit plate 10 is fixed to the rotation shaft 24.
  • the aperture plate 12 is also fixed to the rotating shaft 24, and is configured to be rotationally driven together with the slit plate 10 by a common drive mechanism.
  • the aperture plate 12 is provided with apertures 12a-1, 12a-2 and 12a-3 at positions corresponding to the inlet slits 10a-1, 10a-2 and 10a-3, respectively.
  • the exit slits 10b-1, 10b-2 and 10b-3 lead from the spectroscope 42 to the light detector 44 also when the corresponding entrance slits 10a-1, 10a-2 or 10a-3 respectively are used. It is provided in the position which can be arrange
  • corresponding inlet and outlet slits are arranged in symmetrical positions about the axis of rotation 24.
  • the rotation shaft 24 is driven by a rotation drive mechanism.
  • the inlet slit 10a is switched to any of 10a-1, 10a-2 and 10a-3, and at the same time the outlet slit 10b and the aperture 12a correspond to the inlet slit It is automatically switched to things.
  • slits 10a and apertures 12a are provided and switched, but two types or four or more types of slits 10a and apertures 12a may be used.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Spectrometry And Color Measurement (AREA)

Abstract

Selon l'invention, une plaque fendue 10 constituant une partie à fente variable et une plaque à ouverture 12 constituant une partie de réglage d'ouverture numérique sont agencées entre un miroir 8 et un spectroscope 14. Un mécanisme d'entraînement de fente 11 entraîne la plaque fendue 10 sur la base d'un signal provenant d'une unité de commande 18 et agence, sur l'axe optique de la lumière provenant du miroir 8, l'une d'une pluralité de fentes 10a formées dans la plaque fendue 10. Un mécanisme d'entraînement d'ouverture 13 agence une ouverture 12a correspondant à la fente 10a agencée sur l'axe optique de la lumière provenant du miroir 8, sur le même axe optique sur la base d'un signal provenant de l'unité de commande 18.
PCT/JP2018/026263 2017-10-04 2018-07-12 Spectromètre Ceased WO2019069526A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2017194574 2017-10-04
JP2017-194574 2017-10-04

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WO2019069526A1 true WO2019069526A1 (fr) 2019-04-11

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PCT/JP2018/026263 Ceased WO2019069526A1 (fr) 2017-10-04 2018-07-12 Spectromètre

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110196100A (zh) * 2019-05-21 2019-09-03 中国科学院上海技术物理研究所 一种成像光谱仪快速装调方法
JP2021507224A (ja) * 2017-12-15 2021-02-22 ホリバ インスツルメンツ インコーポレイテッドＨｏｒｉｂａ Ｉｎｓｔｒｕｍｅｎｔｓ Ｉｎｃｏｒｐｏｒａｔｅｄ 凹面回折格子分光器の選択的分解能のためのシステム及び方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57138026U (fr) * 1981-02-23 1982-08-28
JPH10160569A (ja) * 1996-12-03 1998-06-19 Yokogawa Electric Corp 分光装置
JPH11241948A (ja) * 1998-02-26 1999-09-07 Hitachi Ltd 分光測定装置
JP2003166878A (ja) * 2001-12-04 2003-06-13 Shimadzu Corp 分光光度計

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57138026U (fr) * 1981-02-23 1982-08-28
JPH10160569A (ja) * 1996-12-03 1998-06-19 Yokogawa Electric Corp 分光装置
JPH11241948A (ja) * 1998-02-26 1999-09-07 Hitachi Ltd 分光測定装置
JP2003166878A (ja) * 2001-12-04 2003-06-13 Shimadzu Corp 分光光度計

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021507224A (ja) * 2017-12-15 2021-02-22 ホリバ インスツルメンツ インコーポレイテッドＨｏｒｉｂａ Ｉｎｓｔｒｕｍｅｎｔｓ Ｉｎｃｏｒｐｏｒａｔｅｄ 凹面回折格子分光器の選択的分解能のためのシステム及び方法
JP7421478B2 (ja) 2017-12-15 2024-01-24 ホリバ インスツルメンツ インコーポレイテッド 凹面回折格子分光器の選択的分解能のためのシステム及び方法
CN110196100A (zh) * 2019-05-21 2019-09-03 中国科学院上海技术物理研究所 一种成像光谱仪快速装调方法
CN110196100B (zh) * 2019-05-21 2021-04-09 中国科学院上海技术物理研究所 一种成像光谱仪快速装调方法

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