WO2014132379A1 - フーリエ変換赤外分光光度計 - Google Patents
フーリエ変換赤外分光光度計 Download PDFInfo
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- WO2014132379A1 WO2014132379A1 PCT/JP2013/055295 JP2013055295W WO2014132379A1 WO 2014132379 A1 WO2014132379 A1 WO 2014132379A1 JP 2013055295 W JP2013055295 W JP 2013055295W WO 2014132379 A1 WO2014132379 A1 WO 2014132379A1
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- transform infrared
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 title claims abstract description 41
- 230000003287 optical effect Effects 0.000 claims abstract description 26
- 238000005259 measurement Methods 0.000 abstract description 40
- 238000009434 installation Methods 0.000 abstract 2
- 238000001228 spectrum Methods 0.000 description 33
- 239000007788 liquid Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000000691 measurement method Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
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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
- G01J3/28—Investigating the spectrum
- G01J3/45—Interferometric spectrometry
- G01J3/453—Interferometric spectrometry by correlation of the amplitudes
- G01J3/4535—Devices with moving mirror
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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
- G01J3/0264—Electrical interface; User interface
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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
- G01J3/027—Control of working procedures of a spectrometer; Failure detection; Bandwidth calculation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/02—Details
- G01J3/0275—Details making use of sensor-related data, e.g. for identification of sensor parts or optical elements
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/02—Details
- G01J3/0289—Field-of-view determination; Aiming or pointing of a spectrometer; Adjusting alignment; Encoding angular position; Size of measurement area; Position tracking
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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
- G01J3/108—Arrangements of light sources specially adapted for spectrometry or colorimetry for measurement in the infrared range
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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
- G01J3/12—Generating the spectrum; Monochromators
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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
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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
- G01J3/0205—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
- G01J3/021—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows using plane or convex mirrors, parallel phase plates, or particular reflectors
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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
- G01J3/0297—Constructional arrangements for removing other types of optical noise or for performing calibration
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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
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Definitions
- the present invention relates to a Fourier transform infrared spectrophotometer (Fourier Transform InfraRed Spectrophotometer, hereinafter referred to as “FTIR”).
- FTIR Fourier Transform InfraRed Spectrophotometer
- an infrared interference wave whose amplitude varies with time is generated by an interferometer typified by a Michelson interferometer, and the sample is irradiated with the transmitted light transmitted through the sample or reflected light reflected by the sample.
- a spectrum power spectrum
- the Michelson interferometer is a device including a beam splitter (half mirror), a fixed mirror, a moving mirror, etc., and divides the light into two by the beam splitter, one is a fixed mirror and the other is a moving mirror. After the reflection, these two reflected lights are made to interfere with each other.
- the amplitude of the obtained interference light varies with time.
- sample spectrum the power spectrum obtained from the light transmitted or reflected through the sample. Since the background is superimposed on the sample spectrum, it is necessary to subtract the background from the sample spectrum in order to obtain an absorption spectrum or a transmission spectrum.
- an operation for obtaining a background spectrum is performed by measuring without a sample before measuring a sample spectrum.
- Patent Document 1 dynamic alignment
- samples are installed according to differences in measurement methods such as total reflection measurement (ATR), specular reflection measurement, and diffuse reflection measurement, or according to differences in sample phases (gas, liquid, solid).
- ATR total reflection measurement
- specular reflection measurement specular reflection measurement
- diffuse reflection measurement or according to differences in sample phases (gas, liquid, solid).
- Attach a replaceable measurement accessory to the sample chamber For example, when measuring a liquid or gas, an accessory having a cell for accommodating them is used.
- the sample is fixed to the surface of the prism, and a moving mechanism is provided that moves the prism to change the incident angle of infrared interference light on the sample. Use the product.
- the manual mechanism there is a moving mechanism that uses a motor.
- an infrared microscope may be attached to the sample chamber as an accessory.
- the sample chamber in which these accessories are mounted is placed on the instrument housing via a suspension so that vibration is not easily transmitted, but the interference conditions are optimal with no accessories in the sample chamber. Even if it is set to, the attachment may be deviated from the optimum interference condition by attaching the accessory, and the manner of deviation differs depending on the accessory.
- the problem to be solved by the present invention is to provide an FTIR with high measurement accuracy without being affected by changes in interference conditions due to attachment of accessories.
- the inventor of the present application has found that the reason why the interference condition changes due to attachment of the accessory is that the base in which the sample chamber and the interferometer are installed via independent suspensions is slightly distorted by the weight of the accessory. . That is, when the base is distorted, the positional relationship between the fixed mirror and the movable mirror of the interferometer changes. Since the interference condition changes sensitively depending on this positional relationship, even a slight distortion of the base has an adverse effect. Moreover, the incident position of the infrared light to the detector may shift due to distortion of the base.
- the optical path and the optical elements such as prisms, mirrors, and slits that make up the accessory are different for each accessory, resulting in different throughput. Accordingly, the amount of infrared light incident on the detector may be reduced, thereby reducing the signal intensity.
- the present invention made to solve the above-mentioned problems is a Fourier transform infrared spectrophotometer in which a sample chamber in which accessories can be detachably attached and an interference optical system are provided on a common base.
- a) accessory information reading means for reading accessory information attached to the accessory when the accessory is mounted in the sample chamber;
- setting condition changing means for changing the setting condition of the interference optical system according to the accessory based on the accessory information read by the accessory information reading means; It is characterized by providing.
- the accessory information reading means reads accessory information attached to the accessory when the accessory is mounted in the sample chamber. Based on the accessory information read in this way, the setting condition changing means changes the setting condition of the interference optical system according to the attached accessory. Measurement is performed based on the setting condition changed in this way. Thereby, it can measure on the optimal conditions for every accessory.
- the setting conditions of the interference optical system for each accessory are obtained by conducting a background spectrum measurement experiment in advance and then recorded for each accessory in the recording means of the Fourier transform infrared spectrophotometer.
- the changing means may read the setting condition corresponding to the accessory from the recording means.
- the setting conditions of the interference optical system for each accessory may be attached to the accessory as accessory information.
- the setting condition changing means for example, in an interference optical system in which infrared light is divided into two parts, one is reflected by a fixed mirror and the other is reflected by a movable mirror, and then these two reflected lights are interfered with each other.
- the setting condition changing means may change a parameter for setting the luminance of the light source.
- the accessory information attached to the accessory may be recorded in a normal readable recording means such as an IC chip or a barcode.
- the schematic block diagram of one Example of FTIR which concerns on this invention The schematic block diagram of the sample chamber of FTIR of a present Example.
- the schematic block diagram which shows an example of the accessory with which the sample chamber of FTIR of a present Example is mounted
- the schematic block diagram which shows another example of the accessory with which the sample chamber of FTIR of a present Example is mounted
- the schematic block diagram which shows another example of the accessory with which the sample chamber of FTIR of a present Example is mounted
- the flowchart which shows a process at the time of readjusting the optimal value of the phase difference of dynamic alignment based on the power spectrum obtained by the measurement in FTIR of a present Example.
- an interferometer chamber 1 and a sample chamber 2 are provided on the upper surface of a base 3 as shown in FIG.
- a suspension (not shown) is provided between the interferometer chamber 1 and the sample chamber 2 and the base 3.
- the interferometer chamber 1 is airtight, and a main interferometer including an infrared light source 10, a condensing mirror 11, a collimator mirror 12, a beam splitter 13, a fixed mirror 14, and a moving mirror 15 is included therein. Is provided. Further, inside the interferometer chamber 1, a control interferometer including a laser light source 16 and a laser mirror 17 and a beam splitter 13, a fixed mirror 14, and a movable mirror 15 common to the main interferometer are also provided. . The main interferometer is for generating main interference light to irradiate the sample, and the control interferometer is for measuring parameters for adjusting the relative orientation of the fixed mirror 14 with respect to the movable mirror 15. is there.
- main interference light emitted from the main interferometer is introduced into the infrared light detector 6 via the parabolic mirror 4, the sample chamber 2 (described above), and the ellipsoidal mirror 5. These parts are arranged so that they are arranged.
- a piezoelectric element 14 a for adjusting the posture (orientation) of the fixed mirror 14 is provided on the back surface of the fixed mirror 14.
- FIG. 2 is a schematic configuration diagram of the sample chamber 2. Inside this, an accessory 20 as shown in FIGS. 3 to 5 is mounted.
- the accessory 20 used in the FTIR of this embodiment is provided with an IC chip 21 in which accessory information (for example, product number) is recorded.
- an accessory information reading unit 22 is provided inside the sample chamber 2 so as to read the accessory information of the IC chip 21 when the accessory 20 is mounted in the sample chamber 2.
- the FTIR of this embodiment is provided with a control unit 30 (setting condition changing means), and the control unit 30 includes a calculation unit 31, a parameter storage unit 32, and a data processing unit 33.
- the function of the control unit 30 will be described in the description of the operation of the FTIR of this embodiment described later.
- Examples of the accessory 20 mounted in the sample chamber 2 include the following.
- (a) Accessories according to the measurement method (a-1) Accessories for ATR measurement ATR measurement is performed by pressing the sample against the prism and infra-redly reflecting the sample while slightly entering the sample at the boundary between the prism and sample. An absorption spectrum of a sample is obtained from light.
- the ATR measurement accessory has a prism that is pressed against the sample, and an optical system that allows infrared light to enter the sample at a predetermined angle and introduces reflected light into a detector (for example, stocks). Made by Shimadzu Corporation, ATR-8200H).
- an ATR measurement accessory provided with a mechanism for moving the prism and the sample in order to change the incident angle of the infrared light to the sample (for example, ATR-8000A manufactured by Shimadzu Corporation).
- ATR-8000A manufactured by Shimadzu Corporation.
- a-2 Accessories for specular reflection measurement
- the specular reflection measurement is a method for measuring the reflection spectrum of a sample without using a prism, and has been performed for a long time than the ATR measurement.
- an absorption spectrum can also be obtained by analyzing the reflection spectrum by Kramers-Kronig analysis. As shown in FIG.
- the specular reflection measurement accessory has an optical system that allows infrared light to enter a sample at a predetermined angle and introduces reflected light into a detector (for example, SRM manufactured by Shimadzu Corporation). -8000A). Some specular reflection accessories also have a mechanism for changing the incident angle of infrared light on the sample (for example, VeeMAX II A manufactured by Shimadzu Corporation). (a-3) Accessories for transmission measurement Transmission measurement is a method of measuring the spectrum of infrared light that literally passes through a sample.
- the specular reflection measurement accessory transmits a sample holder with a hole and a window made of a material that transmits the infrared light, and the infrared light through the sample so as not to block the infrared light transmitted through the sample. And having an optical system introduced into the detector.
- (b) Accessories according to the phase of the sample
- (b-1) Liquid cell Used when measuring a liquid sample.
- a liquid cell with higher airtightness is used for the volatile liquid sample.
- a reflecting mirror is provided so that the infrared light is repeatedly reflected in the cell. Use a gas cell.
- FTIR Infrared microscope
- An infrared microscope as an accessory of FTIR is generally an optical system as a microscope that passes through an objective lens facing the sample, and infrared light is incident on the sample from the side of the sample, and from the opposite side of the sample. It has an optical system as an FTIR that extracts reflected light.
- laser light is emitted from the laser light source 16 of the control interferometer.
- This laser beam is split into two by being irradiated onto the beam splitter 13 via the laser mirror 17, one laser beam is reflected by the fixed mirror 14 and returns to the beam splitter 13, and the other laser beam is It is reflected by the movable mirror 15 and returns to the beam splitter 13.
- laser interference light in which these two lights interfere with each other is generated and sent to the exit of the interferometer chamber 1, that is, toward the parabolic mirror 4. Since this laser interference light travels as a light beam having a very small diameter, it is reflected by the laser mirror 18 inserted in the optical path and introduced into the laser detector 19.
- the laser detector 19 is a four-divided photodiode in which the light receiving surface is divided into four by two axes orthogonal to each other, and signals obtained by the four light receiving units are output in parallel. Signals obtained by each of the four light receiving units are input to the calculation unit 31, and the calculation unit 31 obtains a reference signal Sr and a reference signal Sr obtained from a certain one of the four light receiving units.
- the phase difference ⁇ RH between the reference signal Sr and the horizontal signal Sh and the reference signal Sr are perpendicular to each other based on the horizontal signal Sh and the vertical signal Sv obtained from the light receiving units adjacent to the light receiving unit in the horizontal direction and the vertical direction, respectively.
- a phase difference ⁇ RV with respect to the signal Sv is obtained.
- the phase differences ⁇ RH and ⁇ RV obtained here are set as temporary parameters ⁇ RH0 and ⁇ RV0, respectively.
- infrared light is emitted from the infrared light source 10.
- Infrared light is introduced into the beam splitter 13 via the condenser mirror 11 and the collimator mirror 12 and divided into two.
- One infrared light is reflected by the fixed mirror 14 and returns to the beam splitter 13, and the other infrared light is reflected by the movable mirror 15 and returns to the beam splitter 13.
- main interference light in which these two lights interfere is generated.
- This main interference light is detected by the infrared light detector 6 via the parabolic mirror 4, the sample chamber 2, and the ellipsoidal mirror 5.
- the control unit 30 acquires an interferogram, and Fourier transforms the interferogram, so that the horizontal axis is the wave number, the vertical axis. Get the power spectrum with intensity on the axis. Further, the control unit 30 obtains the phase differences ⁇ RH and ⁇ RV based on the signal of the laser detector 19 over the entire length of movement of the movable mirror 15, and these phase differences ⁇ RH and ⁇ RV are maintained at the temporary parameters ⁇ RH0 and ⁇ RV0, respectively. As described above, the tilt of the fixed mirror 14 is adjusted by feedback control of the voltage applied to the piezoelectric element 14a.
- the control unit 30 performs a Fourier transform on the interferogram thus obtained, thereby acquiring a power spectrum having the horizontal axis as the wave number and the vertical axis as the intensity.
- the intensity at an arbitrary wave number for example, three points of 1000 cm ⁇ 1 , 2000 cm ⁇ 1 , and 3000 cm ⁇ 1 ) is obtained. If the intensity is equal to or greater than a predetermined value, the temporary parameters ⁇ RH0 and ⁇ RV0 are set as parameters ⁇ RHa and ⁇ RVa for adjusting the inclination of the fixed mirror 14 in the dynamic alignment.
- the operation of obtaining the power spectrum as described above after changing the temporary parameters ⁇ RH0 and / or ⁇ RV0 is repeated until the intensity of the power spectrum becomes equal to or higher than the predetermined value.
- Temporary parameters ⁇ RH0 and ⁇ RH0 when the intensity exceeds a predetermined value are set as the parameters ⁇ RHa and ⁇ RVa.
- the parameters ⁇ RHa and ⁇ RVa thus obtained are stored in the parameter storage unit 32 as a parameter table in association with information on accessories attached to the sample chamber 2. These numerical values become information used when changing the setting conditions of the interference optical system during the measurement of the sample, as will be described below.
- an interferogram is acquired by the same method as in the preliminary measurement, and a power spectrum is obtained by Fourier transforming the interferogram.
- the power spectrum obtained here is a sample spectrum including information on the sample because the main interference light passes through the sample chamber 2 or is reflected by the sample when passing through the sample chamber 2.
- the inclination of the fixed mirror 14 is adjusted based on the parameters ⁇ RHa and ⁇ RVa. Since these parameters ⁇ RHa and ⁇ RVa are set for each accessory 20, even if the distortion of the base 3 is different due to the difference of the accessory 20, a strong sample spectrum can be obtained without being affected by the distortion.
- Parameter setting change The optimum value of the parameter may change due to factors other than the weight of the accessory, such as equipment aging, changes in the measurement environment and optical axis deviation.
- the user of the apparatus or a supplier who performs regular maintenance of the apparatus may readjust the parameter settings as described below.
- FIG. 6 is a flowchart showing steps when the control unit 30 readjusts the parameters ⁇ RHa and ⁇ RVa based on the power spectrum obtained by the measurement.
- the control part 30 acquires the intensity
- the intensity of the power spectrum is increased to a predetermined value or more by repeating the operation of acquiring the power spectrum as described above after changing the parameters, as in the previous measurement.
- the parameter is again measured to obtain the following parameter (step S6). If such a parameter is obtained, the process proceeds from step S7 to step S8, and the obtained parameter is stored in association with the corresponding accessory information (step S8).
- the accessory 20 itself (for example, the optical axis in the accessory 20 determined by the mirror included in the accessory 20). Proceeding from step S7 to step S9, a message indicating that the accessory 20 needs to be adjusted or the like is displayed.
- the phase difference is described as an example of the parameter.
- the luminance of the infrared light source 10 can be used as the parameter. Since the throughput differs for each accessory, the amount of infrared light received by the detector changes by mounting the accessory. This is because the resulting power spectrum intensity changes. Therefore, the brightness of the infrared light source 10 is changed depending on the type of the accessory 20 so that the same power spectrum intensity as when the accessory is not attached can be obtained. Since the luminance of the infrared light source 10 is proportional to the power supplied to the infrared light source 10, the power value may be stored for each accessory as a parameter.
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Abstract
Description
a) 前記付属品が前記試料室内に装着された際に、該付属品に付された付属品情報を読み取る付属品情報読取手段と、
b) 前記付属品情報読取手段で読み取られた前記付属品情報に基づいて、前記干渉光学系の設定条件を、該付属品に応じて変更する設定条件変更手段と、
を備えることを特徴とする。
本実施例のFTIRでは、図1に示すように、干渉計室1及び試料室2がベース3の上面に設けられている。干渉計室1及び試料室2とベース3の間にはサスペンション(図示せず)が設けられている。
(a) 測定方法に応じた付属品
(a-1) ATR測定用付属品
ATR測定は、プリズムに試料を押しつけ、プリズムと試料の境界においてわずかに試料内に侵入しつつ全反射される赤外光から、試料の吸収スペクトルを得るものである。ATR測定用付属品は、図3に示すように、試料に押しつけられるプリズムと、試料に所定の角度で赤外光を入射させると共に反射光を検出器に導入する光学系を有する(例えば、株式会社島津製作所製・ATR-8200H)。また、試料への赤外光の入射角度を変更するために、プリズム及び試料を移動させる機構が設けられたATR測定用付属品もある(例えば、株式会社島津製作所製・ATR-8000A)。
(a-2) 正反射測定用付属品
正反射測定は、プリズムを使用することなく試料の反射スペクトルを測定する方法であり、ATR測定よりも古くから行われているものである。また、正反射測定法では、反射スペクトルをクラマース・クローニッヒ解析することにより、吸収スペクトルを得ることもできる。正反射測定用付属品は、図4に示すように、試料に所定の角度で赤外光を入射させると共に反射光を検出器に導入する光学系を有する(例えば、株式会社島津製作所製・SRM-8000A)。正反射測定用付属品においても、試料への赤外光の入射角度を変更する機構が設けられたものがある(例えば、株式会社島津製作所製・VeeMAX II A)。
(a-3) 透過測定用付属品
透過測定は、文字通り試料を透過する赤外光のスペクトルを測定する方法である。正反射測定用付属品は、試料を透過した赤外光を遮らないように、孔や該赤外光を透過する材料から成る窓が設けられた試料ホルダと、赤外光を、試料を透過させて検出器に導入する光学系を有する。
(b-1) 液体セル
液体試料を測定する場合に使用する。また、不揮発性の液体試料に用いる液体セルとは別に、揮発性の液体試料では、より気密性の高い液体セルを用いる。
(b-2) ガスセル(気体セル)
気体試料を測定する場合に使用する。また、希薄な気体試料を測定する場合には、試料による赤外光の吸収量を多くするために、図5に示すように、セル内で赤外光が繰り返し反射するように反射鏡を設けたガスセルを使用する。
FTIRでは、赤外顕微鏡と組み合わせることで、試料の拡大画像とサンプルスペクトルを同時に得ることができる。FTIRの付属品としての赤外顕微鏡は一般的に、試料に相対する対物レンズを通る顕微鏡としての光学系と、試料の側方から赤外光を試料に入射させ、反対側の試料側方から反射光を取り出すFTIRとしての光学系を有する。
(2-1) 事前測定
FTIRでは通常、出荷時やメンテナンス時に、試料室に付属品を装着していない状態で最適になるよう、干渉光学系が設定される。本実施例においてもその点は同様である。ここで、試料室2に装着する付属品はそれぞれ重量が異なるため、干渉計室1及び試料室2を支持するベース3に生じる歪みも付属品によって異なる。このベース3の歪みの相違によって、ダイナミックアライメントにおける固定鏡14の傾きを調整するためのパラメータが、付属品毎に相違することとなる。そこで予め、試料室に付属品を装着せずに干渉光学系が最適に設定された状態において、付属品毎に、試料室に装着したうえで当該パラメータを求める事前測定を行う。この事前測定は、工場出荷時に行ってもよいし、新しい付属品を初めて装着する際に使用者が行うようにしてもよい。以下、事前測定の方法を説明する。
まず、使用者は、測定の目的に応じた付属品20を試料室2に装着する。これにより、付属品20のICチップ21に記録された付属品情報が、試料室2の内部に配設された付属品情報読取部22により読み取られ、制御部30に送られる。制御部30は、付属品情報読取部22から付属品情報を取得すると、パラメータ記憶部32内のパラメータテーブルを参照して、試料室2内に装着された付属品に対応するパラメータΔRHa及びΔRVaを取得する。次に、使用者は試料室2に試料を装着し、FTIRの装置に測定を開始させるための操作を行う。
装置の経年劣化、測定環境の変化や光軸のずれ等、付属品の重量以外の要因により、パラメータの最適値が変わってしまう場合がある。それに対応するため、装置の使用者や、装置の定期メンテナンスを行う業者が、以下に述べるようにパラメータの設定を再調整してもよい。
11…集光鏡
12…コリメータ鏡
13…ビームスプリッタ
13…試料室
14…固定鏡
14a…圧電素子
15…移動鏡
16…レーザ光源
17、18…レーザ用ミラー
19…レーザ検出器
2…試料室
20…付属品
21…ICチップ
22…付属品情報読取部
3…ベース
30…制御部
31…演算部
32…パラメータ記憶部
33…データ処理部
4…放物面鏡
5…楕円面鏡
6…赤外光検出器
Claims (3)
- 付属品を着脱自在に装着可能な試料室と干渉光学系が共通のベース上に設けられたフーリエ変換赤外分光光度計であって、
a) 前記付属品が前記試料室内に装着された際に、該付属品に付された付属品情報を読み取る付属品情報読取手段と、
b) 前記付属品情報読取手段で読み取られた前記付属品情報に基づいて、前記干渉光学系の設定条件を、該付属品に応じて変更する設定条件変更手段と、
を備えることを特徴とするフーリエ変換赤外分光光度計。 - 前記設定条件が、赤外光を2つに分割して一方を固定鏡で、他方を移動鏡で反射させた後にこれら2つの反射光を干渉させる干渉光学系において、移動鏡に対する固定鏡の相対的な向きを調整するためのパラメータであることを特徴とする請求項1に記載のフーリエ変換赤外分光光度計。
- 前記設定条件が、前記試料に照射される赤外光の光源の輝度を設定するためのパラメータであることを特徴とする請求項1又は2に記載のフーリエ変換赤外分光光度計。
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US14/770,849 US9459150B2 (en) | 2013-02-28 | 2013-02-28 | Fourier transform infrared spectrophotometer |
PCT/JP2013/055295 WO2014132379A1 (ja) | 2013-02-28 | 2013-02-28 | フーリエ変換赤外分光光度計 |
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WO2019092772A1 (ja) * | 2017-11-07 | 2019-05-16 | 株式会社島津製作所 | 赤外分光光度計用付属品 |
WO2020174665A1 (ja) * | 2019-02-28 | 2020-09-03 | 株式会社島津製作所 | マイケルソン干渉計およびそれを備えるフーリエ変換赤外分光装置 |
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