WO2008014937A1 - Cellule de mesure optique - Google Patents

Cellule de mesure optique Download PDF

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Publication number
WO2008014937A1
WO2008014937A1 PCT/EP2007/006673 EP2007006673W WO2008014937A1 WO 2008014937 A1 WO2008014937 A1 WO 2008014937A1 EP 2007006673 W EP2007006673 W EP 2007006673W WO 2008014937 A1 WO2008014937 A1 WO 2008014937A1
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WO
WIPO (PCT)
Prior art keywords
optical
measuring cell
sample chamber
light radiation
optical measuring
Prior art date
Application number
PCT/EP2007/006673
Other languages
German (de)
English (en)
Inventor
Frank Gindele
Markus Holzki
Original Assignee
INSTITUT FüR MIKROTECHNIK MAINZ GMBH
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 INSTITUT FüR MIKROTECHNIK MAINZ GMBH filed Critical INSTITUT FüR MIKROTECHNIK MAINZ GMBH
Publication of WO2008014937A1 publication Critical patent/WO2008014937A1/fr

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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
    • G01N21/01—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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/031—Multipass arrangements

Definitions

  • the invention relates to an optical measuring cell for measuring the extinction of light radiation in fluids.
  • the signal of a light source is guided via an optical fiber or via a free-ray optics to a sample channel.
  • the signal radiates through the sample channel and is guided on one exit side again, according to the signal coupling, to further analysis or evaluation systems.
  • the irradiated channel length or geometric path length is fixed in this case to a certain length.
  • the associated optical transmission path length is fixed in this case to a certain length.
  • An adaptation of the optical transmission path length to the change to be investigated takes place via the change in the geometric length of the cell.
  • the measurement of low concentrations or concentration changes at low concentrations by absorption of the light radiation is carried out with a measuring cell with a geometrically long path length, the measurement of a high concentration or concentration changes at high concentrations with a geometrically small path length.
  • WO 99/63369 A1 discloses a flow cell for the optical analysis of liquid dairy and food products with infrared radiation. At opposite ends of the flow cell, optical fiber cables equipped with a sapphire window are placed. Via the first fiber cable, light radiation coming from an infrared source is coupled into the flow cell and decoupled from the flow cell via the second fiber cable. The distance of the fiber cables is adjustable, whereby the geometric and thus optical transmission path length of the flow cell can be varied and is thus adaptable to different measuring tasks.
  • a monolithic optical multiple reflection cell is specified with an oval sample chamber whose walls are formed in partial areas as mirror surfaces.
  • a light beam coupled in via an inlet opening is coupled out of the sample chamber at a discharge opening only after multiple reflection and thus a very long optical transmission path length.
  • analytical investigations of gas compositions and gas concentrations can be carried out with a relatively compact sample chamber with short geometric path length, which are not feasible with short optical transmission path lengths.
  • the subject of DE 42 14 840 A1 is a measuring cell with an optical light source and with different absorption path lengths for detecting one substance each.
  • the spectral component of the light radiation relevant for the substance detection is reflected several times in the cell and then detected. This means that different spectral bands undergo a different optical absorption path.
  • the spectral separation takes place via interference filters within the measuring cell.
  • the object of the invention is to provide a compact optical measuring cell for measuring the extinction of light radiation in a fluid, which can be used over a wide measuring range.
  • fluid is understood below to mean liquid and gaseous media, as well as mixtures of various liquids and / or gases, as well as dispersions, suspensions, emulsions or aerosols.
  • light radiation essentially comprises light radiation from the UV range into the infrared range with wavelengths of 200 nm to 12 ⁇ m, particularly preferably with wavelengths in the ranges 350 nm to 1100 nm and 1200 nm to 6 ⁇ m.
  • thermal radiators with a continuous radiation pattern and, in the infrared range, to use light sources, possibly in combination with filters, to be able to use individual narrow wavelength ranges as light radiation.
  • Significant proportions of the light radiation means that at least 10%, preferably at least 25% and particularly preferably at least 50% of the portions of the light radiation are included.
  • Absorbance is generally composed of absorption, scattering, diffraction and reflection of light radiation and is wavelength dependent.
  • the extinction can be given as a numerical value as a negative decadic logarithm of the transmittance. Description of the invention
  • the object of the invention is achieved by an optical measuring cell for carrying out measurements of the extinction of light radiation in fluids, wherein the optical measuring cell in a sample filled with a fluid or a fluid through a sample chamber, a first optical element for the coupling of light radiation in the Sample chamber, which is at least partially permeable to light radiation coming from outside the sample chamber and light radiation from the interior of the sample chamber at least partially reflected back into the sample chamber and a second optical element, which is designed such that there is a first portion of the light radiation coming from the sample chamber reflected substantially in the direction of the first optical element and decouples a further portion of the sample chamber has.
  • the optical measuring cell according to the invention is provided as part or replacement part of a measuring device, wherein the measuring device can also have a light source and a detector for measuring the light radiation emerging from the sample chamber. Furthermore, the measuring device may also include an electronics downstream of the detector, which further processes, evaluates and / or displays the measured values obtained at the detector.
  • the light source and / or detector can also each be components of the optical measuring cell.
  • a light source for example in the form of a thermal radiator, an LED or another light source, is arranged outside the sample chamber in the vicinity and with an optical connection to the first optical element on the optical measuring cell.
  • a detector for example, in a CCD array or a photocell, outside the sample chamber in the vicinity and with optical connection to the second optical element at the optical measuring cell can be arranged.
  • optical measuring cell designed according to the invention, light radiation having a simple optical transmission path length and the multiple optical transmission path length is coupled out at the same time on the second optical element and on a subsequent detector or sensor superimposed, that is coupled to the second optical element simultaneously and spatially superimposed light radiation with different optical path length.
  • light beams with a simple and approximately three times the optical transmission path length are simultaneously coupled out.
  • the information obtained at the detector thus simultaneously contains the information of the extinction of the light radiation in the fluid after single and multiple or preferably approximately three times the optical transmission path length. In this way, changes in the fluid or fluids with divergent properties over a much larger range of parameters are to be determined than with the known devices, each measuring only the extinction obtained over an optical transmission path length.
  • the proportions of light radiation with single and multiple optical transmission path lengths are determined, which are measured together on a detector.
  • the first optical element is preferably designed such that it reflects at least significant portions of the light radiation coming from the sample chamber back into the sample chamber.
  • the measuring cell can be adapted to the measuring tasks.
  • the ratio of single to multiple optical transmission path length will be in the range from 10: 1 to 1:10, particularly preferably in the range from 3: 1 to 1: 3.
  • the optical measuring cell with the decoupling of the light radiation with a single and multiple optical transmission path length on an optical element, only one detector or sensor is required. An electronic system for processing and evaluating the measured values obtained at the detector is also sufficient.
  • such a designed optical measuring cell can build very compact, since different optical transmission path lengths (single and multiple) are measured with a geometric path length and fewer components than in measuring cells with multiple, different optical transmission paths are needed. If it is an optical measuring cell through which a fluid flows during operation, this can be used for on-line, in-line and at-line measurements and / or continuous measurement of a fluid.
  • the first and / or second optical element for the light radiation on transparent / transparent and reflective / mirrored areas.
  • the portion of the light radiation from the sample chamber which impinges on light transmissive areas of the second optical element is coupled out of the sample chamber, i.
  • the translucent area light radiation with single and multiple optical path lengths is coupled out simultaneously and spatially superimposed.
  • the portion of the light radiation from the sample chamber which strikes the reflective areas of the second optical element is reflected again into the sample chamber substantially in the direction of the first optical element.
  • the optical elements are arranged opposite one another, preferably in the walls of the sample chamber.
  • the elements are preferably arranged symmetrically on an optical axis.
  • the optical elements have components for beam shaping, such as, for example, lenses, reflectors, gratings, filters and / or prisms.
  • the light radiation of a light source coupled into the sample chamber on the first optical element is directed with suitable components, such as, for example, lenses, substantially directly in the direction of the second optical element.
  • the optical elements can have light attenuation components and filters for spectral filtering.
  • optical measuring cell provides that the components of the optical elements at least partially light radiation reflective and / or partially translucent and transparent to light radiation
  • the components can have reflective layers or masks can be used as independent, further components for shading or reflection of light radiation.
  • the inner walls of the sample chamber may be equipped with a light radiation absorbing surface.
  • a light radiation absorbing surface In this way, only light radiation, which passes directly through the sample chamber, and light radiation, which is coupled out after a first or further reflections between the optical elements, on the detector.
  • Light-absorbing surface areas are formed, for example, by blackened surfaces, surface coatings and / or surface treatments.
  • the optical measuring cell is preferably made of non-transparent materials, such as metals, plastics, glass and / or ceramic.
  • the optical elements or the components of the optical elements can be made of any material transparent to the light radiation, such as glass, sapphire, semiconductor materials and / or plastic.
  • the reflective coating of the optical components, preferably the lenses, can be done with silver, aluminum, gold or other metals, or with semiconductors or other reflective materials.
  • the focal length of the first lens or all components of the optical element for coupling the light radiation into the sample chamber is preferably greater than the geometric path length of the sample chamber.
  • the focal length of the lenses or all optical components of the optical elements for coupling and decoupling the light radiation is in this case preferably matched to one another in the direction from the first to the second lens or from the first to the second optical element a common focus outside the sample chamber to have.
  • the distance from the first lens to the second lens is particularly preferably selected such that the first lens lies within the focal length of the second lens.
  • the focal length of the first lens is chosen in this case such that the focal length is greater than the distance between the first and the second lens and the focal point is outside the sample chamber.
  • concave, convex, plano-convex, plano-concave, spherical, aspherical lenses, paraboloidal, ellipsoidal lenses, cylindrical lenses, surfaces with two or more different spheres can be arranged concentrically, for example, or even freeform surfaces can be used.
  • lenses and / or reflectors within an optical element as both beam shaping and beam directing components for coupling and uncoupling the light beam minimizes the number of components required.
  • Shaping by a ray is understood in this context to mean that light radiation is focused, collimated, dispersed or scattered.
  • beam the change of the propagation direction of the light beam is understood, for example by reflection or refraction.
  • the detector may be part of the second optical element, for example an integrated component of a lens.
  • the optical measuring cell can be designed as a replacement part of a measuring device, wherein the optical measuring cell is, for example, used in a suitable recording of the measuring device.
  • the measuring device then comprises further components, such as light source, detector and / or optical grids, which are permanently mounted or likewise form exchangeable components of the measuring device.
  • the measuring cell can therefore be adapted and easily inserted into the measuring device or replaced in the event of wear and dirt, without having to replace all or expensive components.
  • an adjustment of the individual components of the Measuring device can be facilitated by receiving the components in corresponding recesses in a platform in this way or completely avoided completely passive adjustment.
  • the further components of a measuring device such as light source, detector and / or other components, may be integrated components of the optical measuring cell.
  • This compact design can form a complete measuring device.
  • the measuring devices equipped with the optical measuring cell according to the invention can be used, for example, by a spectrometer as part of the measuring device for the spectrally resolved measurement of the extinction.
  • the optical measuring cell preferably contains a flow-optimized sample chamber in order to avoid dead volumes and turbulences. Because of this measurements could have undesirable fluctuations or at least temporarily falsified and the pressure loss can be increased unnecessarily. Consequently, abrupt changes in cross section, sharp edges and undercuts in the shaping of the sample chamber in the direction of flow are avoided.
  • the optical measuring cell from at least one or more molded components, for example injection-molded components, wherein the optical elements can be integrated in these components, as indicated similarly in German patent application DE 102005062174 (not yet published).
  • the components containing the optical measuring cell may also contain other components, such as fluid channels, reaction chambers, fluid mixers, etc., and form individual parts of a so-called lab-on-a-chip.
  • a splitting of the light beam in the sample chamber into spectral components can take place upon entry of the light radiation via the first optical element, the respective spectral components being directed in the direction of different second optical elements and there are coupled and superimposed on each single and multiple optical transmission path length.
  • Figure 2 cross-sectional view of a first embodiment of an optical measuring cell according to the invention
  • FIG. 3 a shows a first side view of a further embodiment of an optical measuring cell according to the invention
  • FIG. 3b shows a cross-sectional view of the embodiment of the optical measuring cell shown in FIG. 3a along the section line A-A contained in FIG. 3a
  • FIG. 3c shows a second side view of the embodiment of the optical measuring cell shown in FIG. 3a and FIG. 3b
  • FIG. 3d second cross-sectional representation of the embodiment of the optical measuring cell shown in FIGS. 3a-3c along the section line BB contained in FIG. 3c
  • FIG. 4 Top view of a measuring device with optical measuring cell
  • FIG. 5 shows the normalized radiation intensity as a function of
  • FIG. 6 shows measurement results with a measuring device according to FIG. 4 with an optical measuring cell according to the invention and a spectrometer
  • FIG. 8 Measurement results for the measurement of a chromium sulfate solution with logarithmic Y axis
  • FIG. 1 schematically shows an optical measuring cell (10) in cross-section with the beam guide, a first (1) and second optical element (2) and a sample chamber (3).
  • the beam propagation is schematically indicated by arrows.
  • a first optical element (1) for coupling the light radiation into the sample chamber (3) the light radiation emanating from a light source (7) in the direction of the sample chamber (3) is introduced into the sample chamber (3) via a first planoconvex lens (1) optical measuring cell (10) coupled.
  • the first plano-convex lens (1) is convex on its side facing away from the sample chamber (3) and provided with a reflective surface layer (11) outside a central, circular area (12) concentric with the optical axis (9), so that only the part the light radiation from the light source is coupled into the sample chamber (3) which strikes the central region (12) of the first lens (1).
  • the light radiation is coming from the light source (7) initially divergent and is refracted at the convex surface of the first lens (1) and directed in the direction of the second optical element (2).
  • the second optical element (2) is also embodied in the form of a plano-convex lens (2) in this exemplary embodiment.
  • the convex side of the lens (2) lies on the side facing away from the sample chamber (3) and also has a reflective surface (13) outside of a central, circular region (14) concentric with the optical axis (9).
  • the light radiation coming from the first optical element (1) and striking the mirrored region (13) of the second lens (2) is again reflected and collimated in the direction of the first optical element (1), so that the Light radiation with the least possible loss through the optical cell (10) can be directed (extinction losses excluded by the fluid).
  • the portion of the light radiation which strikes the second lens (2) in the central, transparent region (14) is decoupled from the sample chamber (3) and directed in the direction of a focal point (4).
  • the portion of the light radiation reflected at the second lens (2) traverses the sample chamber (3) a second time and is reflected and focused by the first lens (1) in the direction of the transparent surface areas (14) of the second lens (2).
  • the convergent light radiation is focused after the renewed transmission through the sample chamber (3) through the second lens (2) outside the sample chamber (3) in the focal point (4).
  • the focal length of the first lens (1) is greater than the lens pitch of the first (1) and second lenses (2), so that the radiation is focused at a focal point (4) outside the cell.
  • the optical transmission path length for the reflected portion of the radiation with respect to the geometric path length of the sample chamber (3) is extended by a factor of 3 to 3.5 (the influence of the refractive index of Fluids are ignored here).
  • the measurement sensitivity for this radiation fraction is increased by a corresponding factor compared to a measurement of the light extinction with a simple transmission path length of the sample chamber filled with a fluid to be measured.
  • the radiation fraction coupled out of the sample chamber (3) after the above-mentioned beam guidance is superimposed in the common focal point (4) with a further radiation component which is decoupled after the third pass through the sample chamber.
  • the two radiation components are now coupled in, for example in an optical system (eg spectrometer), spectrally split and detected.
  • This embodiment of an optical measuring cell (10) coupled to a spectrometer is shown in FIG.
  • FIG. 2 shows an embodiment according to the invention of an approximately trapezoidal optical measuring cell (10) in plan view with a fluid inlet connection (21) and fluid outlet connection (22).
  • the fluid connections (21, 22) are designed here as threaded bores (23) for receiving fluid lines (not shown).
  • the optical elements (1, 2) for coupling and uncoupling the light radiation are arranged opposite one another in side walls (15) of the sample chamber (3) in precisely fitting recesses (25, 26) of the measuring cell (10).
  • the light source (7) is also included in this embodiment.
  • the light source (7) is a thermal radiator.
  • the fluid flowing through the sample chamber (3) during operation of the optical measuring cell (10) is irradiated by the light beam coupled to the first optical element (1) essentially perpendicular to its direction of flow.
  • a lens (1) provided on its side facing away from the sample chamber (3) is provided with a reflective layer (11) as an optical element (1) for coupling and simultaneous shaping used by the light beam.
  • a lens (2) is used to decouple the light beam, which is permeable to light radiation around its optical axis on its side facing away from the sample chamber (3) only in the inner circular region (14) and has a mirrored ring around the center Surface (13).
  • a detector (16) is also attached to the passing through the transparent area of the second lens (2)
  • FIGS. 3a to 3d show a further optical measuring cell (10) with improved flow properties for the fluid flowing through the optical measuring cell (10) during operation in several sectional drawings.
  • the better flow characteristics are that e.g. the complete flow through the sample chamber (3) without a relevant dead volume, turbulence, etc. is achieved.
  • the optical measuring cell (10) shown is tested up to a pressure of 3 bar, but by design adjustments of this embodiment, applications at much higher pressure ranges are possible.
  • the optical measuring cell (10) contains the sample chamber (3), which flows through in operation, the holder for the optical elements (1, 2). Images for the light source and a coupling region to a subsequent analysis system are in this embodiment not part of the optical measuring cell (10) itself, but, as shown in the following in Figure 4 embodiment, part of the entire measuring device (5).
  • FIG. 3a shows a side view of the optical measuring cell (10) from the side of the fluid inlet (21) and fluid outlet (22).
  • FIG. 3b shows a sectional drawing of the optical measuring cell (10) along the section line AA contained in FIG. 3a.
  • the recesses (25, 26) for the optical elements (1, 2) are also shown thereon.
  • FIG. 3c shows a side view of the optical measuring cell (10), in which the recess (25) for the first optical element and the sample chamber (3) can be seen.
  • FIG. 3d shows a sectional drawing of the optical measuring cell (10) along the section line BB contained in FIG. 3c.
  • the individual components of the measuring device (5) such as optical measuring cell (10), mirror (17, 18, 19), optical grating (20) and CCD sensor (16) of the spectrometer (6), and light source (7) are respectively inserted into the exact recesses of a platform (8) and are fixed and sealed by placing a flat lid (not shown) in the measuring device (5).
  • the optical measuring cell (10) is interchangeable in this example and can be changed or replaced separately from other components of the measuring device (5).
  • the arrangement of the components in accurate recordings of a platform (8) allows precise production and alignment of the components to each other without special manufacturing methods.
  • the sample chamber (3) is continuously flowed through by a liquid, so that an on-line measurement can be carried out.
  • the light beam coming from the optical measuring cell (10) is reflected by two mirrors (17, 18) onto an optical grating (20), separated spectrally and transmitted to the detector (16) via another mirror (19). focused and detected.
  • FIG. 5 shows a comparison of the normalized intensity profile of a light beam transmitted through an optical measuring cell as a function of the concentration and for different optical path lengths.
  • the graphs I (L1) and 1 (10L1) describe the intensity profile for the passage of a light beam once or 10 times through one with a Fluid filled sample chamber of an optical measuring cell.
  • the intensity attenuation I (L1) is small for small concentration differences at a first concentration d.
  • the possible concentration resolution is low for a simple cell passage of the light signal at low concentrations.
  • the intensity attenuation at 1 (10L1) in the range of the same concentration d is significantly greater and thus the concentration resolution much higher.
  • FIG. 6 shows the extinction spectra of air (Air) and various engine oils (V%), Wherein the first and the second measurement are respectively identified at the end of the identity numbers in the legend by an a or b.
  • the experiment with an optical measuring cell according to the invention shows an extended detectable concentration range with a clear deviation from the simple exponential curve from c ⁇ 4000 ppm.
  • the experimental results (denoted in Figure 8 as measured values and shown in the form of dots) are over a two-fold exponential decrease describe. The reason for this is the superimposition of the signals of the two optical path lengths within the measuring cell. Two exponents therefore determine the experimental course.
  • a simple exponential drop would result and the resolution of the transmission values at high concentrations would be significantly reduced.

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  • 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)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Optical Measuring Cells (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

Cellule (10) de mesure optique pour mesurer l'extinction d'un rayonnement lumineux dans un fluide. Selon l'invention, la cellule (10) de mesure optique présente une chambre (3) à échantillon remplie d'un fluide ou traversée par un fluide pendant le fonctionnement, un premier élément (1) optique pour l'injection du rayonnement lumineux dans la chambre (3) à échantillon, lequel est au moins partiellement transparent pour le rayonnement lumineux en provenance de l'extérieur de la chambre (3) à échantillon et réfléchit de nouveau au moins partiellement dans la chambre (3) à échantillon le rayonnement lumineux en provenance de l'intérieur de la chambre (3) à échantillon, un deuxième élément (2) optique qui est configuré de telle sorte qu'il réfléchit une première partie du rayonnement lumineux en provenance de la chambre (3) à échantillon sensiblement en direction du premier élément (1) optique et extrait une autre partie de la chambre (3) à échantillon.
PCT/EP2007/006673 2006-07-29 2007-07-27 Cellule de mesure optique WO2008014937A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200610035581 DE102006035581B3 (de) 2006-07-29 2006-07-29 Optische Messzelle
DE102006035581.4 2006-07-29

Publications (1)

Publication Number Publication Date
WO2008014937A1 true WO2008014937A1 (fr) 2008-02-07

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WO (1) WO2008014937A1 (fr)

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CN110114655A (zh) * 2016-11-11 2019-08-09 微波实验室技术股份公司 具有带多个光路的放电灯的分光计

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DE102012013241A1 (de) 2011-06-27 2012-12-27 Institut Für Photonische Technologien E.V. Mikrofluid-Durchflussküvette
CN104713852A (zh) * 2015-02-05 2015-06-17 中国民航大学 一种可控能见度大气模拟系统
DE102016204234A1 (de) 2016-03-15 2017-09-21 Robert Bosch Gmbh Mikrofluidische Vorrichtung und Verfahren zur Durchführung von chemischen, biochemischen und/oder biologischen Untersuchungen

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US3936196A (en) * 1974-10-21 1976-02-03 Spectrotherm Corporation Fluid chamber having manipulatable window elements
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CN110114655A (zh) * 2016-11-11 2019-08-09 微波实验室技术股份公司 具有带多个光路的放电灯的分光计

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