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WO2017046913A1 - Détecteur d'indice de réfraction différentiel - Google Patents

Détecteur d'indice de réfraction différentiel Download PDF

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Publication number
WO2017046913A1
WO2017046913A1 PCT/JP2015/076450 JP2015076450W WO2017046913A1 WO 2017046913 A1 WO2017046913 A1 WO 2017046913A1 JP 2015076450 W JP2015076450 W JP 2015076450W WO 2017046913 A1 WO2017046913 A1 WO 2017046913A1
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WO
WIPO (PCT)
Prior art keywords
refractive index
flow cell
cell
measurement light
differential refractive
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/JP2015/076450
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English (en)
Japanese (ja)
Inventor
亨 山口
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
Priority to PCT/JP2015/076450 priority Critical patent/WO2017046913A1/fr
Publication of WO2017046913A1 publication Critical patent/WO2017046913A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors

Definitions

  • the present invention relates to a differential refractive index detector used as a detector in an analyzer such as a liquid chromatograph.
  • the differential refractive index detector detects the refractive index of the sample solution and the concentration of the components contained in the sample solution using the difference in refractive index between the sample solution and the reference solution.
  • a flow cell comprising: an optical system that guides light from a light source to the flow cell through a slit; and an optical system that guides light that has passed through the flow cell to a light receiving element and forms a slit image on the light receiving element. Yes.
  • a reference solution flows through one cell of the flow cell, and a sample solution flows through the other cell. Light from the light source sequentially passes through the two cells of the flow cell and then enters the light receiving element.
  • the path of light passing through the flow cell changes according to the difference in refractive index between the reference solution and the sample solution, and the slit image formed on the light receiving element is displaced.
  • the component concentration of the sample solution can be obtained (Patent Documents 1 and 2).
  • the differential refractive index detector is usually configured such that a mirror 560 is disposed behind the flow cell 550, and light from the light source 510 passes through the flow cell 550 twice. That is, the light incident on the flow cell 550 is refracted by an angle ⁇ corresponding to the difference in refractive index between the reference solution and the sample solution, is emitted from the flow cell 550, is reflected by the mirror 560, and passes through the two cells again. Then, the light is further refracted by an angle ⁇ and emitted from the flow cell 550 (FIG. 9). Thereby, the displacement amount of the slit image is increased.
  • the differential refractive index detector can accurately measure the refractive index and concentration of the sample because the slit image is greatly displaced if the difference in refractive index between the reference solution and the sample solution is large.
  • the concentration of the sample in the sample solution is low or when the refractive index of the component contained in the sample is close to the refractive index of the reference solution, the refractive index difference is small and the slit image is hardly displaced. It becomes difficult to accurately measure the refractive index and density.
  • a differential refractive index detector with improved sensitivity as in Patent Document 3 has been proposed, a differential refractive index detector with higher sensitivity has been demanded in order to measure a sample with a smaller refractive index difference.
  • the problem to be solved by the present invention is to provide a differential refractive index detector having high sensitivity.
  • the differential refractive index detector according to the present invention made to solve the above problems is A flow cell having a sample solution cell and a reference solution cell partitioned by a partition; And two reflecting portions arranged opposite to each other with the sample solution cell and the reference solution cell interposed therebetween so that the measurement light passes through the partition wall three times or more and then travels toward the measurement light detector.
  • the two reflecting portions are arranged to face each other with the sample solution cell and the reference solution cell interposed therebetween, and the measurement light incident on the flow cell is reflected between the two reflecting portions. After passing through the partition wall between the sample solution cell and the reference solution cell three times or more, it goes to the measuring light detector. Each time the measurement light passes through the partition wall, it is refracted by an angle ⁇ corresponding to the difference in refractive index between the sample solution and the reference solution contained in these two cells.
  • the angle at which the measurement light is refracted also increases in accordance with the number of times.
  • the measurement light detector detects the refraction angle of the measurement light, and based on this, the refractive index of the sample solution and the concentration of the component contained in the solution are measured.
  • the differential refractive index detector may be configured such that one or both of the two reflecting portions are provided on one or both of the two wall surfaces sandwiching the sample solution cell and the reference solution cell of the flow cell. .
  • the flow cell and the reflection portion are provided separately, a fixture for fixing each of them is necessary.
  • a space for arranging the reflecting portion is also required.
  • a fixture or a space for fixing the reflecting portion is not required, and the differential refractive index detector can be miniaturized.
  • Such a reflection part can be configured by adhering a mirror to the flow cell or by depositing metal on the flow cell.
  • the reflecting part or measuring light on the wall surface on which the measuring light is incident enters the measuring light detector. It is desirable that the reflecting portion of the wall surface on the outgoing side is set shorter than the reflecting portion of the other wall surface in the direction in which the measurement light is repeatedly reflected.
  • the measurement light can enter or exit the flow cell from the short set portion, so the overall differential refractive index detector including the light source and the measurement light detector can be reduced in size. can do.
  • the normal line is the reflection of the other wall surface of the portion not provided with the reflecting portion of the shorter wall surface. It is desirable to incline toward the center side of the part.
  • the reflecting portion of the wall surface on which the measurement light is incident is shortened, the light incident from the portion of the wall surface where the reflecting portion is not provided is on the center side of the reflecting portion of the other wall surface. Because the light is refracted toward the light source, the incident light from the light source can be incident at a lower angle with respect to the normal of the reflection portion of the other wall surface, and the position of the light source can be brought closer to the measurement light detector. It becomes like this. This also leads to a reduction in the size of the entire differential refractive index detector including the light source and the measurement light detector. The same applies when the reflecting portion of the wall surface on the side from which the measurement light is emitted is shortened.
  • the measurement light incident on the flow cell passes through the partition wall between the sample solution cell and the reference solution cell at least three times, and every time it passes, the refractive index of the sample solution and the reference solution. Refraction is made at an angle corresponding to the difference.
  • FIG. 1 is a schematic configuration diagram of a differential refractive index detector according to a first embodiment of the present invention.
  • FIG. 3 is a diagram illustrating the structure of a flow cell of the differential refractive index detector according to the first embodiment of the present invention.
  • FIG. 4 is a diagram for explaining reflection of measurement light by a first reflecting portion and a second reflecting portion of the differential refractive index detector according to the first embodiment of the present invention.
  • FIG. 5 is a schematic configuration diagram of a differential refractive index detector according to a second embodiment of the present invention. The figure explaining the structure of the flow cell of the differential refractive index detector which concerns on the 2nd Embodiment of this invention.
  • FIG. 3 is a diagram illustrating the structure of a flow cell of the differential refractive index detector according to the first embodiment of the present invention.
  • FIG. 4 is a diagram for explaining reflection of measurement light by a first reflecting portion and a second reflecting portion of the differential refractive index detector according to the first embodiment of the present invention.
  • FIG. 5 is a schematic configuration diagram of a differential refractive index detector according to a third embodiment of the present invention.
  • FIG. 1 is a schematic configuration diagram of a differential refractive index detector according to a first embodiment of the present invention.
  • the differential refractive index detector includes a light source 110, a condenser lens 120, a slit plate 130, a collimator lens 140, a flow cell 150, and a split photodiode 170.
  • the condenser lens 120 and the slit plate 130 are arranged in the light irradiation direction of the light source 110, and the collimating lens 140 is arranged in front of the flow cell 150.
  • the focal point of the condensing lens 120 is adjusted to be the position of the collimating lens 140.
  • FIG. 2A is a top view of the flow cell 150
  • FIG. 2B is a cross-sectional view taken along line AA of FIG. 2A.
  • a reference solution cell 150a and a sample solution cell 150b both having a right triangular prism shape are juxtaposed so as to share a hypotenuse, and a partition wall 150e is provided between the two cells.
  • a mobile phase is passed through the reference solution cell 150a, and a mobile phase or a mobile phase containing a sample is passed through the sample solution cell 150b.
  • the first reflecting portion 160a and the second reflecting portion 160b are provided on the outer wall surface on the collimating lens side of the flow cell 150 and the outer wall surface facing the collimating lens so that the reflecting surfaces face the inside of the flow cell 150, respectively.
  • the second reflecting portion 160 b is provided on the entire outer surface of the flow cell 150.
  • the first reflection unit 160a has a shorter structure than the second reflection unit 160b in the height direction (z-axis direction) of the flow cell 150 (referred to as the flow cell axial direction).
  • the reflective surfaces of the first reflective unit 160a and the second reflective unit 160b are arranged in parallel to each other.
  • an incident part 150c and an emission part 150d are provided on the upper and lower parts of the outer wall of the flow cell 150 on the collimator lens 150 side, and a first reflection is provided between the incidence part 150c and the emission part 150d.
  • Part 160a The incidence part 150c and the emission part 150d are inclined so that the normal line is directed toward the center of the wall surface on which the second reflection part 160b is provided.
  • the divided photodiode 170 (measurement light detector in the present invention) has a plus-side light-receiving element and a minus-side light-receiving element on the light-receiving surface, and a detection signal (not shown) corresponding to the illuminance of light applied to each light-receiving element.
  • the signal processing unit measures the refractive index of the sample solution and the concentration of components contained in the solution based on the detection signal.
  • the measurement light emitted from the light source 110 passes through the slits arranged in the axial direction of the flow cell 150 of the condenser lens 120 and the slit plate 130, is converted into parallel light by the collimator lens 140, and is incident on the flow cell 150.
  • FIG. 3 is a diagram for explaining the reflection of the measurement light by the first reflector 160a and the second reflector 160b.
  • the measurement light incident on the flow cell 150 has an axial direction of the flow cell 150 (z-axis direction in FIG. 3B) at an angle corresponding to the refractive index of air and the material of the flow cell 150 and the incident angle of the measurement light at the incident portion 150c. And is incident on the flow cell 150.
  • the measurement light incident on the flow cell 150 is reflected between the second reflecting portion 160b and the first reflecting portion 160a as shown in FIG. 3B and between the two cells while traveling in the axial direction of the flow cell 150.
  • the partition wall 150e is passed three times or more (six times in FIG. 3).
  • an angle ⁇ corresponding to the refractive index difference between the mobile phase flowing in the reference solution cell 150a and the mobile phase including the sample flowing in the sample solution cell 150b is shown in FIG. ) Is refracted in the y-axis direction. Then, the light is refracted at an angle corresponding to the refractive index of the material of the flow cell 150 and the air and the incident angle of the measurement light in the emission part 150 d and emitted from the flow cell 150.
  • Measurement light emitted from the flow cell 150 forms an image on the split photodiode 170 by the collimator lens 140. Since the imaging position at this time changes according to the above-described refracted angle (6 ⁇ ⁇ ), the differential refractive index detector in the present embodiment is 3 in comparison with the conventional technique in which the partition wall 150e is passed only twice. Double sensitivity can be obtained.
  • the measurement light is configured to pass through the partition wall 150e in the flow cell 150 six times.
  • the number of times the measurement light passes through the partition can be increased by elongating the flow cell in the axial direction, for example.
  • the flow cell is lengthened, the size of the flow cell increases, and the arrangement of components such as a light source and a detector needs to be changed in accordance with the flow cell, so that the entire differential refractive index detector becomes large.
  • the inclination angle of the incident portion is reduced, or the distance between the first reflecting portion and the second reflecting portion (the thickness of the flow cell) is reduced. be able to.
  • count of passing a partition can be increased, without changing the existing arrangement
  • the first reflecting portion and the second reflecting portion are provided on the outer wall surface of the flow cell, but may be provided on the inner wall surface of the flow cell, that is, the wall surfaces of the reference solution cell and the sample solution cell.
  • FIG. 4 shows a schematic configuration diagram of the differential refractive index detector in the present embodiment.
  • the configuration of the flow cell, the first reflection unit, and the second reflection unit is different from that of the first embodiment, but the other configurations are the same, and thus description thereof will be omitted as appropriate.
  • FIG. 5A is a top view of the flow cell 250
  • FIG. 5B is a cross-sectional view taken along the line AA of FIG. 5A.
  • a reference solution cell 250a and a sample solution cell 250b both having a right triangular prism shape are juxtaposed so as to share a hypotenuse, and a partition wall 250e is provided between the two cells.
  • a mobile phase is passed through the reference solution cell 250a, and a mobile phase or a mobile phase containing a sample is passed through the sample solution cell 250b.
  • an incident part 250c and an emission part 250d are provided on the upper and lower parts of the outer wall surface of the flow cell 250 on the collimator lens 240 side.
  • the first reflecting portion 260a is provided in parallel to the surface of the reference solution cell 250a on the triangular prism on the collimator lens 240 side (the yz plane in FIG. 5A).
  • the 2nd reflection part 260b is provided so that the 1st reflection part 260a may be opposed on both sides of the flow cell 250.
  • the second reflecting portion 260b is inclined with respect to the first reflecting portion 260a (a state rotated by a predetermined angle around the y axis in FIG. 5B).
  • the measurement light emitted from the light source 210 passes through the condensing lens 220 and the slit arranged in the axial direction of the flow cell 250 of the slit plate 230, is converted into parallel light by the collimating lens 240, and is incident on the flow cell 250.
  • the measurement light incident on the flow cell 250 has an axial direction of the flow cell 250 (z-axis direction in FIG. 5B) at an angle corresponding to the refractive index of air and the material of the flow cell 250 and the incident angle of the measurement light at the incident part 250c. And is incident on the flow cell 250.
  • the measurement light that has entered the flow cell 250 is reflected between the second reflector 260b and the first reflector 260a, and passes through the partition 150e between the cells three or more times while traveling in the axial direction of the flow cell 250. .
  • the measurement light passes through the partition wall 250e, the measurement light in FIG.
  • 5A is shown by an angle ⁇ corresponding to the refractive index difference between the mobile phase flowing in the reference solution cell 250a and the mobile phase including the sample flowing in the sample solution cell 250b. Since it is refracted in the y-axis direction, the total number of passes is refracted by n ⁇ ⁇ . Then, the light is refracted at an angle corresponding to the material of the flow cell 250 and the refractive index of the air at the emission part 250 d and emitted from the flow cell 250.
  • the light emitted from the flow cell 250 forms an image on the split photodiode 270 by the collimator lens 240. Since the imaging position at this time changes according to the above-described refracted angle (n ⁇ ⁇ ), the differential refractive index detector in the present embodiment obtains higher sensitivity than the conventional technique in which the flow cell is passed only twice. be able to.
  • the differential refractive index detector of the present embodiment may have a structure in which the first reflection unit 260a and the second reflection unit 260b are provided integrally with the flow cell 250. At this time, the outer surface of the flow cell 250 provided with the second reflection part 260b is shaped to match the inclination of the second reflection part 260b, so that the second reflection part 260b is inclined and the structure is integrated with the flow cell 250. can do.
  • FIG. 6 is a schematic configuration diagram of the differential refractive index detector according to the present embodiment.
  • the differential refractive index detector includes a light source 310, a condenser lens 320, a slit plate 330, a first collimator lens 340a, a flow cell 350, a second collimator lens 340b, and a split photodiode 370.
  • the condenser lens 320 and the slit plate 330 are arranged in the irradiation direction of the light source 310, the first collimating lens 340a is arranged on the front surface of the flow cell 350, and the second collimating lens 340b is arranged on the rear surface of the flow cell 350.
  • the focus of the condensing lens 320 is adjusted so that it may become the position of the collimating lens 340a.
  • FIG. 7A is a top view of the flow cell 350
  • FIG. 7B is a cross-sectional view taken along the line AA of FIG. 7A.
  • a reference solution cell 350a and a sample solution cell 350b both having a right triangular prism shape are juxtaposed so as to share a hypotenuse, and a partition wall 350e is provided between the two cells.
  • a mobile phase is passed through the reference solution cell 350a, and a mobile phase or a mobile phase containing a sample is passed through the sample solution cell 350b.
  • the first reflecting portion 360a is arranged on the outer wall surface of the flow cell 350 on the first collimating lens 340a side
  • the second reflecting portion 360b is arranged on the outer wall surface on the second collimating lens 340b side so that the reflecting surface faces the inside of the flow cell 350. Is provided.
  • the first reflecting portion 360 a and the second reflecting portion 360 b are provided on the entire one surface of the outer wall of the flow cell 350.
  • the first reflecting unit 360a and the second reflecting unit 360a, 360b have two reflecting surfaces arranged in parallel.
  • the first reflecting portion 360a and the second reflecting portion 360b are arranged at positions shifted in the height direction (z-axis direction) of the flow cell, and the incident portion 350c is disposed above the first reflecting portion 360a, and the second reflecting portion.
  • the emission part 350d is provided in the lower part of 360b, respectively.
  • the incident part 350c is inclined so that its normal line is directed toward the center side of the outer wall surface provided with the second reflecting part 360b, and the emitting part 350d is the center of the outer wall face provided with the first reflecting part 360a. Inclined to the side.
  • the split photodiode 370 has a plus-side light-receiving element and a minus-side light-receiving element on the light-receiving surface, and transmits a detection signal corresponding to the illuminance of light irradiated to each light-receiving element to a signal processing unit (not shown).
  • the signal processing unit measures the refractive index of the sample solution and the concentration of components contained in the solution based on the detection signal.
  • Measurement light emitted from the light source 310 passes through a slit arranged in the axial direction of the flow cell 350 of the condensing lens 320 and the slit plate 330, is converted into parallel light by the collimating lens 340, and is incident on the flow cell 350.
  • the measurement light incident on the flow cell 350 has an axial direction of the flow cell 350 (z-axis direction in FIG. 7B) at an angle corresponding to the refractive index of the air and the material of the flow cell 350 and the incident angle of the measurement light at the incident portion 350c. And is incident on the flow cell 350.
  • the measurement light incident on the flow cell 350 is reflected between the second reflection unit 360b and the first reflection unit 360a, and passes through the partition wall three times or more while traveling in the axial direction of the flow cell 350.
  • the measurement light of FIG. 7A is shown by an angle ⁇ corresponding to the refractive index difference between the mobile phase flowing in the reference solution cell 350a and the mobile phase including the sample flowing in the sample solution cell 350b.
  • the total number of passes is refracted by n ⁇ ⁇ . Then, the light is refracted at an angle corresponding to the refractive index of the material of the flow cell 350 and the air and the incident angle of the measurement light in the emission part 350 d and emitted from the flow cell 350.
  • Measurement light emitted from the flow cell 350 forms an image on the split photodiode 370 by the second collimating lens 340b. Since the imaging position at this time changes according to the above-described refracted angle (n ⁇ ⁇ ), the differential refractive index detector in the present embodiment has higher sensitivity than the conventional technique in which the partition 150e is passed only twice. Obtainable.
  • the measurement light is reduced by reducing the angle of inclination of the incident part or reducing the distance (flow cell thickness) between the first reflecting part and the second reflecting part.
  • the number of times that passes through the partition wall can be increased.
  • both the first and second reflecting portions are provided on the wall surface of the flow cell, but both or one of them may be provided at a position away from the wall surface.

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Abstract

L'invention concerne un détecteur d'indice de réfraction différentiel présentant une sensibilité élevée. Le détecteur d'indice de réfraction différentiel comprend : une cellule à circulation 150 qui comprend une cellule à solution d'échantillon 150b et une cellule à solution de référence 150a séparées l'une de l'autre par une paroi de séparation 150e ; et deux parties de réflexion 160a, 160b qui sont disposées de sorte à être agencées en regard l'une de l'autre, la cellule à solution d'échantillon 150b et la cellule à solution de référence 150a étant interposées entre celles-ci de sorte que la lumière de mesure soit dirigée vers un détecteur 170 de lumière de mesure après avoir traversé la paroi de séparation 150e trois fois ou plus, le nombre de fois où la lumière de mesure est réfractée par la cellule à circulation 150 pouvant par là-même être supérieur ou égal à trois, une sensibilité plus élevée que jusqu'à présent pouvant ainsi être obtenue.
PCT/JP2015/076450 2015-09-17 2015-09-17 Détecteur d'indice de réfraction différentiel Ceased WO2017046913A1 (fr)

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PCT/JP2015/076450 WO2017046913A1 (fr) 2015-09-17 2015-09-17 Détecteur d'indice de réfraction différentiel

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PCT/JP2015/076450 WO2017046913A1 (fr) 2015-09-17 2015-09-17 Détecteur d'indice de réfraction différentiel

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS51110385A (fr) * 1975-03-25 1976-09-29 Toyo Soda Mfg Co Ltd
JPH0361559U (fr) * 1989-10-19 1991-06-17
JPH0552748U (ja) * 1991-12-11 1993-07-13 株式会社島津製作所 示差屈折計
JPH05288676A (ja) * 1992-04-09 1993-11-02 Shimadzu Corp 示差屈折計
JP2007121322A (ja) * 2007-02-13 2007-05-17 Japan Science & Technology Agency 全反射吸収測定用プリズムおよびこれを用いた全反射吸収測定装置
JP2008268233A (ja) * 2008-07-30 2008-11-06 Shimadzu Corp 示差屈折率検出器

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS51110385A (fr) * 1975-03-25 1976-09-29 Toyo Soda Mfg Co Ltd
JPH0361559U (fr) * 1989-10-19 1991-06-17
JPH0552748U (ja) * 1991-12-11 1993-07-13 株式会社島津製作所 示差屈折計
JPH05288676A (ja) * 1992-04-09 1993-11-02 Shimadzu Corp 示差屈折計
JP2007121322A (ja) * 2007-02-13 2007-05-17 Japan Science & Technology Agency 全反射吸収測定用プリズムおよびこれを用いた全反射吸収測定装置
JP2008268233A (ja) * 2008-07-30 2008-11-06 Shimadzu Corp 示差屈折率検出器

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