WO2017060159A1 - Spectromètre à absorption - Google Patents

Spectromètre à absorption Download PDF

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Publication number
WO2017060159A1
WO2017060159A1 PCT/EP2016/073335 EP2016073335W WO2017060159A1 WO 2017060159 A1 WO2017060159 A1 WO 2017060159A1 EP 2016073335 W EP2016073335 W EP 2016073335W WO 2017060159 A1 WO2017060159 A1 WO 2017060159A1
Authority
WO
WIPO (PCT)
Prior art keywords
base
carrier
windows
shim
absorption spectrometer
Prior art date
Application number
PCT/EP2016/073335
Other languages
English (en)
Inventor
Peter Phillips
Graham NEWTON
Hugo VARGAS LLANAS
Gary Osborne
David Armstrong
Craig Fletcher
Mike Lawson
Marco CANDELARESI
Jeremy Murray
Archie Shaw Stewart
Ruth NEEDLE
Luis Gonzalez
Original Assignee
Pyreos Ltd.
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 Pyreos Ltd. filed Critical Pyreos Ltd.
Publication of WO2017060159A1 publication Critical patent/WO2017060159A1/fr

Links

Classifications

    • 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
    • G01N21/255—Details, e.g. use of specially adapted sources, lighting or optical systems
    • 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
    • G01J3/0202—Mechanical elements; Supports for 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
    • G01J3/0262—Constructional arrangements for removing stray light
    • 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
    • G01J3/0291—Housings; Spectrometer accessories; Spatial arrangement of elements, e.g. folded path arrangements
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/0303—Optical path conditioning in cuvettes, e.g. windows; adapted optical elements or systems; path modifying or adjustment
    • 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
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N2021/0346—Capillary cells; Microcells
    • G01N2021/035—Supports for sample drops
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/02—Mechanical
    • G01N2201/022—Casings
    • G01N2201/0221—Portable; cableless; compact; hand-held
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/02—Mechanical
    • G01N2201/022—Casings
    • G01N2201/0227—Sealable enclosure

Definitions

  • the invention relates to an absorption spectrometer.
  • spectrometers for measuring liquid samples make use of cuvettes.
  • the cuvettes with the liquid samples are placed within the spectrometer prior to measurement and are removed after the measurement.
  • the cuvettes have different optical path lengths for the liquid sample; typical values are 1 cm or 100 ⁇ .
  • the user chooses the optical path length of the cuvettes depending on the absorption properties of the liquid sample. For a sample with a high absorption the user chooses a short optical path length and for a sample with low absorption the user chooses a long optical path length.
  • the manufacturing tolerances become relatively large in comparison to the optical path length and it is therefore difficult to obtain the optical path length with a high precision and to obtain a parallel sample.
  • spectrometer that is adapted to provide an optical path length for a sample, wherein the optical path length can be obtained with a high precision and the sample has a high degree of parallelism.
  • the absorption spectrometer according to invention comprises a base, a carrier, a bearing and a shim, wherein the base
  • the carrier comprises a carrier window and the other one of the light source and the detector and the shim comprises a planar first side, a planar second side being parallel to the first side and a through hole extending from the first side to the second side, wherein the shim is arranged such that its second side contacts one of the two windows and the carrier can be moved in a direction substantially perpendicular to both windows by means of the bearing such that the other of the two windows can be contacted with the shim at its first side so that a sample space is formed by the through hole and confined by the windows and the shim so that the sample space is formed closed, wherein the at least one of the windows is supported movable such that the carrier window is parallel aligned to the base window when the two windows contact the shim to seal the sample space, wherein light emitted by the light source can pass through the windows and the sample space and can impinge on the detector for measuring the absorption of a sample placed in the sample space.
  • the absorption spectrometer according to the invention can be used for measuring the absorption of a liquid sample.
  • the carrier is moved away from the base and the sample is p laced on the lower one of the two windows .
  • the carrier is then moved towards the base into a position whe e both windows contact the shim and the absorption measurement is carried out .
  • Af e the measurement the carrier is moved again away from the base. After cleaning the two windows another sample can be placed on the lower one of the two windows and another measurement can be performed.
  • the thickness of the shim defines the optical path length of the sample.
  • the shim can be manufactured having a high
  • the shim can be manufactured with a high degree of parallelism of the first side and the second side . Together with the at least one window being supported movable which enables that the two windows are arranged parallel when the two windows contact the shim, it is advantageously achieved that also the sample within the sample space can have high degree of parallelism.
  • the shim is preferable made of a rigid material , in particular a metal , an alloy and/or a glass , such that the sh pe of the shim remains unchanged when the two windows contact the shim at its two sides .
  • the bearing is preferable adapted to enable a translational movement of the carrier .
  • the base comprises a base housing, wherein the shim is supported at its first side on the base housing inside thereof.
  • the shim is arranged such that its second side contacts the base window.
  • the base preferably comprises a frame, a flexible gasket being contacted on its one side with the base window and on its other side with the frame, and a fastening means adapted to fasten the frame to the base housing such that the base window is supported on the gasket, the gasket is supported on the frame and the shim is clamped between the base window and the base housing.
  • the bearing has such a clearance that the bearing movable supports the carrier window so that it is parallel aligned to the base window when the two windows contact the shim and/or wherein the absorption spectrometer comprises at least one flexible member, in particular a shaft of the bearing and/or a member supporting one of the two windows, such that at least one of the windows is movable supported so that the carrier window is parallel aligned to the base window when the two windows contact the shim.
  • the shim preferably has a thickness of 20 pm to 500 pm, in particular of 20 ⁇ to 200 ⁇ , most preferred 100 ⁇ .
  • the bearing comprises a shaft that is fixed on the carrier and that comprises a step, a bush that is attached to the base and in which the shaft is arranged for supporting the carrier such that it can be moved in the
  • the biasing means can be a spring, in
  • the step is preferably adapted to contact the bush when the carrier is moved in the direction substantially perpendicular to the windows away from the base to block the movement of the carrier away from the base at an end position of the carrier.
  • the absorption spectrometer preferably comprises a locking mechanism that is adapted to lock the carrier such that a movement of the carrier in a direction parallel to the windows is prevented when the two windows contact the shim. This advantageously prevents the windows f om being scratched by the shim.
  • the locking mechanism comprises a protrusion protruding from the carrier on a side facing towards the base and a recess formed on the base on a side facing towards the carrier and adapted to receive the rot rusion .
  • the detector preferably comprises a plurality of photo
  • each photo element is impinged by light that passed through a different region of the sample space. Due to the high degree of parallelism of the sample it is
  • each photo element sees the same length of the sample. It is preferred that the photo elements are in particular adapted to detect at least two different parts of the spectrum of the light. Since each photo element sees the same length of the sample, absorption spectra with a high precision can advantageously be measured. It is preferred that the light source is adapted to emit incoherent light.
  • the absorption spectrometer is preferably adapted to be held in a hand. This makes it advantageously easier for a user of the absorption spectrometer handle the absorption spectrometer, in particular to perform the absorption measurement as described before. It is preferred that the side of the carrier facing away from the base is arranged flush with a side of the base . This avoids the formation of edges and makes it more
  • the detector comprises a pyroelectric sensitive material, in particular ieaa-zirconare-t itanate, the light source i s adapted to emit light in the infrared
  • the windows are transparent for the light in the infrared wavelength region, wherein the windows in particular comprise calcium fluoride .
  • Figure 1 shows a front view of an absorption spectrometer according to the invention
  • Figure 2 shows a detail of Figure 1
  • Figure 3 shows a sectional view of line A-A of Figure 1
  • Figure 4 shows a sectional view of line X-X of Figure 2
  • Figure 5 shows a sectional view of line Y-Y of Figure 2
  • Figure 6 shows a sectional view of line B-B of Figure 1
  • an absorption spectrometer 1 comprises a base 2 and a carrier 3.
  • the base 2 comprises a control element 28 for controlling an absorption measurement and a display 29 in particular for reading out a result of the absorption measurement.
  • the base 2 comprises a base housing 11, a base window 7 arranged on the base housing 11 and a detector 10 arranged inside the base housing 11.
  • the carrier 3 comprises a carrier housing 12, a carrier window 8 arranged on the carrier housing 12 and a light source 9 arranged inside the carrier housing 12. It is also conceivable to arrange the light source 9 in the base housing 11 and the detector 10 in the carrier housing 12.
  • Figure 3 shows that the absorption spectrometer 1 furthermore comprises a bearing 22. The carrier 3 can be moved in a
  • the carrier 3 can be moved towards the base 2 to a position in which a sample space 23 is formed.
  • the carrier 3 can be moved away from the base 2 to an end position of the carrier .
  • the spectrometer 1 furthermore comprises a shim 4.
  • the shim 4 comprises a planar first side 24, a planar second side 25 being parallel to the first side 24 and a through hole 26 extending from the first side 24 to the second side 25.
  • the shim is made of a rigid material, in particular a metal, an alloy and/or a glass, such that the shape of the shim remains unchanged when the two windows contact the shim at its two sides.
  • the shim can have a thickness of 20 pm to 500 pm, in particular of 20 pm to 200 pm, most preferred 100 pm .
  • the shim 4 is arranged such that its second side 25 contacts the base window 7.
  • the shim 4 is supported at its first side 24 on the base housing 11 inside thereof.
  • the base 2 For mounting the shim 4 and the base window 7 the base 2 comprises a frame 19, a flexible gasket 21 and a fastening means 20.
  • the flexible gasket 21 is contacted on its one side with the base window 7 and on its other side with the frame 19.
  • the fastening means 20 is adapted to fasten the frame 19 to the base housing 11 such that the base window 7 is supported on the gasket 21, the gasket 21 is supported on the frame 19 and the shim 4 is clamped between the base window 7 and the base housing 11.
  • Figures 3 to 5 show that the carrier 3 comprises a carrier frame 5 that protrudes from the carrier 3.
  • the carrier window 8 is arranged inside the carrier frame 5 and protrudes from the carrier frame 5.
  • the carrier window 8 is sealed with respect to the carrier housing 12, in particular by means of a sealing and/or by means of a glue that attaches the carrier window 8 to the carrier housing 12.
  • the carrier window 8 By moving the carrier 3 towards the base 2 the carrier window 8 can be contacted with the shim 4 at its first side 24 so that the sample space 23 is formed by the through hole 26 and is confined by the windows 7, 8 and the shim 4 so that the sample space 23 is formed closed. Furthermore, at least one of the windows 7, 8 is supported movable such that the carrier window 8 is parallel aligned to the base window 7 when the two windows 8 contact the shim 4 to seal the sample space 23. To achieve this, the bearing 22 can have such a clearance that the bearing 22 movable supports the carrier window 8 so that it is parallel aligned to the base window 7 when the two windows 7, 8 contact the shim 4. It is also conceivable that the absorption
  • spectrometer 1 comprises at least one flexible member, in particular a shaft 13 of the bearing and/or a member supporting one of the two windows 7 , 8, such that at least one of the windows 7, 8 is movable supported so that the carrier window 8 is parallel aligned to the base window 7 when the two windows 7, 8 contact the shim 4.
  • Figures 3 to 5 show the case that the two windows 7, 8 contact the shim 4.
  • light emitted by the light source 9 ca pass through the windows 7, 8 and the sample space 23 and can impinge on the detector 10 for
  • Each detector 10 comprises a plurality of detectors 10. Each detector 10
  • each detector 10 comprises a respective wavelength filter for letting pass a different part of the spectrum of the light emitted by the light source 9, so that at least two different parts of the spectrum of the light can be detected .
  • a detector 10 with a row or a two- dimensional array of photo elements and a linear variable filter for letting pass different parts of the spectrum of the light emitted by the light source 9.
  • Each detector 10 comprises at least one photo element so that the absorption spectrometer 1 comprises a plurality of photo elements, wherein during operation of the absorption spectrometer 1 each photo element is impinged by light that passed through a different region of the sample space 23.
  • the detector 10 comprises a pyroelectric sensitive material , in particular lead-zirconate-titanate .
  • the light source 9 is adapted to emit light in the infrared wavelength region and to emit incoherent light.
  • the windows 7, 8 are transparent for the light in the infrared wavelength region, wherein the windows 7 ,
  • the bearing 22 comprises the shaft 13 that is fixed on the carrier 3 and that comprises a step 15, a bush 16 that is attached to the base 2 and in which the shaft 13 is arranged for supporting the carrier 3 such that it can be moved in the direction substantially perpendicular to both windows 7, 8, and a biasing means 14 that is supported on the inner side of the base housing 11 of the base 2 and on the step 15 to biase the carrier 3 towards the base 2.
  • the step 15 can be formed by a collar.
  • the biasing means 14 is a
  • the absorption spectrometer 1 comprises a locking mechanism 27 that is adapted to lock the carrier 3 such that a movement of the carrier 3 in a direction parallel to the windows ⁇ , 8 is prevented when the two windows 1, 8 contact the shim 4.
  • the locking mechanism 27 comprises a protrusion 17 protruding from the carrier 3 on a side facing towards the base 2 and a recess 18 formed on the base 2 on a side facing towards the carrier 3 and adapted to receive the protrusion .
  • the absorption spectrometer 1 is adapted to be held in a hand.
  • the side of the carrier facing away from the base 2 is arranged flush with a side of the base 2.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Optical Measuring Cells (AREA)

Abstract

L'invention concerne un spectromètre à absorption (1) ayant une base (2), un support (3), un palier (22) et une cale (4), la base (2) comprenant une fenêtre de base (7) et l'un d'une source de lumière (9) et d'un détecteur (10), le support (3) comprenant une fenêtre de support (8) et l'autre de la source de lumière (9) et du détecteur (10), et la cale (4) comprenant un premier côté plat (24), un second côté plat (25) étant parallèle au premier côté (24) et un trou traversant (26) s'étendant du premier côté (24) au second côté (25), la cale (4) étant agencée de telle sorte que son second côté (25) est en contact avec l'une des deux fenêtres (7, 8) et le support (3) peut être déplacé dans une direction sensiblement perpendiculaire aux deux fenêtres (7, 8) au moyen du palier (22) de telle sorte que l'autre des deux fenêtres (7, 8) peut être mise en contact avec la cale (4) sur son premier côté (24) de telle sorte qu'un espace d'échantillon (23) est formé par le trou traversant (26) et confiné par les fenêtres (7, 8) et la cale (4) de telle sorte que l'espace d'échantillon (23) est formé fermé, ladite au moins l'une des fenêtres (7, 8) étant portée de façon mobile de telle sorte que la fenêtre de support (8) est parallèlement alignée à la fenêtre de base (7) lorsque les deux fenêtres (8) sont en contact avec la cale (4) pour sceller l'espace d'échantillon (23), une lumière émise par la source de lumière (9) pouvant passer à travers les fenêtres (7, 8) et l'espace d'échantillon (23) et pouvant frapper le détecteur (10) pour mesurer l'absorption d'un échantillon placé dans l'espace d'échantillon (23).
PCT/EP2016/073335 2015-10-07 2016-09-29 Spectromètre à absorption WO2017060159A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015117063.9A DE102015117063B4 (de) 2015-10-07 2015-10-07 Absorptionsspektrometer
DE102015117063.9 2015-10-07

Publications (1)

Publication Number Publication Date
WO2017060159A1 true WO2017060159A1 (fr) 2017-04-13

Family

ID=57042885

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2016/073335 WO2017060159A1 (fr) 2015-10-07 2016-09-29 Spectromètre à absorption

Country Status (2)

Country Link
DE (1) DE102015117063B4 (fr)
WO (1) WO2017060159A1 (fr)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB840736A (en) * 1955-11-28 1960-07-13 Perkin Elmer Corp Absorption cell assembly
WO2004034038A1 (fr) * 2002-10-10 2004-04-22 Council For The Central Laboratory Of The Research Cellule a echantillon
US20060044554A1 (en) * 2004-08-26 2006-03-02 Mertz Edward L Flow-through, thermal-expansion-compensated cell for light spectroscopy
US20060109467A1 (en) * 2004-11-24 2006-05-25 Evans Richard W Devices, methods, and systems for measuring an optical property of a sample
WO2009039920A1 (fr) * 2007-09-20 2009-04-02 Technische Universität München Système, procédé et détecteur pour la détection de paramètres d'un liquide
US20100045980A1 (en) * 2006-10-06 2010-02-25 Shimadzu Corporation Spectrophotometer
US20100085571A1 (en) * 2008-10-03 2010-04-08 Robertson Jr Charles W Optical Path Length Sensor and Method for Optimal Absorbance Measurements
US20100182599A1 (en) * 2009-01-20 2010-07-22 Scott Albin Spectrometer flip top sample head
WO2015090891A1 (fr) * 2013-12-17 2015-06-25 Pyreos Ltd. Spectromètre infrarouge atr

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004008685A1 (de) * 2004-02-21 2005-09-29 Roche Diagnostics Gmbh Transmissionsspektrometer zur Untersuchung einer flüssigen Probe
DE102011075530A1 (de) * 2011-05-09 2012-01-26 WTW Wissenschaftlich-Technische Werkstätten GmbH Fotometer zur In-situ-Messung in Fluiden

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB840736A (en) * 1955-11-28 1960-07-13 Perkin Elmer Corp Absorption cell assembly
WO2004034038A1 (fr) * 2002-10-10 2004-04-22 Council For The Central Laboratory Of The Research Cellule a echantillon
US20060044554A1 (en) * 2004-08-26 2006-03-02 Mertz Edward L Flow-through, thermal-expansion-compensated cell for light spectroscopy
US20060109467A1 (en) * 2004-11-24 2006-05-25 Evans Richard W Devices, methods, and systems for measuring an optical property of a sample
US20100045980A1 (en) * 2006-10-06 2010-02-25 Shimadzu Corporation Spectrophotometer
WO2009039920A1 (fr) * 2007-09-20 2009-04-02 Technische Universität München Système, procédé et détecteur pour la détection de paramètres d'un liquide
US20100085571A1 (en) * 2008-10-03 2010-04-08 Robertson Jr Charles W Optical Path Length Sensor and Method for Optimal Absorbance Measurements
US20100182599A1 (en) * 2009-01-20 2010-07-22 Scott Albin Spectrometer flip top sample head
WO2015090891A1 (fr) * 2013-12-17 2015-06-25 Pyreos Ltd. Spectromètre infrarouge atr

Also Published As

Publication number Publication date
DE102015117063A1 (de) 2017-04-13
DE102015117063B4 (de) 2018-11-15

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