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WO2012031625A2 - Sonde optique - Google Patents

Sonde optique Download PDF

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Publication number
WO2012031625A2
WO2012031625A2 PCT/EP2010/063148 EP2010063148W WO2012031625A2 WO 2012031625 A2 WO2012031625 A2 WO 2012031625A2 EP 2010063148 W EP2010063148 W EP 2010063148W WO 2012031625 A2 WO2012031625 A2 WO 2012031625A2
Authority
WO
WIPO (PCT)
Prior art keywords
optical
probe
sample
optical probe
distal end
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/EP2010/063148
Other languages
English (en)
Other versions
WO2012031625A3 (fr
Inventor
Tony Maddison
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.)
Foss Analytical AB
Original Assignee
Foss Analytical AB
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 Foss Analytical AB filed Critical Foss Analytical AB
Priority to PCT/EP2010/063148 priority Critical patent/WO2012031625A2/fr
Publication of WO2012031625A2 publication Critical patent/WO2012031625A2/fr
Anticipated expiration legal-status Critical
Publication of WO2012031625A3 publication Critical patent/WO2012031625A3/fr
Ceased legal-status Critical Current

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
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • G01N21/8507—Probe photometers, i.e. with optical measuring part dipped into fluid sample
    • 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
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/4738—Diffuse reflection, e.g. also for testing fluids, fibrous materials
    • G01N21/474—Details of optical heads therefor, e.g. using optical fibres
    • 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
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N2021/4704—Angular selective
    • G01N2021/4726—Detecting scatter at 90°
    • 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
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • G01N21/8507—Probe photometers, i.e. with optical measuring part dipped into fluid sample
    • G01N2021/8528—Immerged light conductor
    • 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
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light

Definitions

  • the present invention relates to an optical probe and in particular to a
  • fiber-optic probe for use in the spectrometric analysis of material.
  • Spectrometric analysis is a known technique which is used to examine stationary or moving samples and for in-line process control and monitoring.
  • optical radiation of a known spectral composition is directed at the sample which absorbs and scatters some of the radiation at various wavelengths.
  • the diffusely scattered portion of the radiation is collected and analyzed, for example using a monochromator, an interferometer or other spectrometric instrument capable of resolving wavelength dependent intensity variations, in order to characterise the sample.
  • optical radiation refers to radiation within some or all of the wavelength region between ultraviolet and infra-red. Optics, optical probes and similar words and phrases are to be interpreted accordingly.
  • the optical probe When utilizing the shorter wavelength infrared region, typically the near infrared (NIR) region at wavelengths below 1 100 nanometers (nm), the optical probe is traditionally disposed in a transmission configuration in which optical radiation is emitted from a distal end of a transmission element, through a sample to be measured which is located in a
  • the spectrometric instrument is optically coupled to a proximal end of the collection element to receive the collected light for analysis.
  • one or both of the transmission element and the collection element may comprise a fibre-optic element.
  • a fibre-optic element typically comprises a fibre-optic element.
  • the probe comprises a slot defining a measurement region into which a sample is received.
  • a transmission fibre-optic bundle and two collection fibre optic bundles are all disposed at a same side of the slot.
  • a reflection element is located at the opposing side of the slot to these bundles and is disposed to reflect light from the transmission fibre- optic bundle towards the collecting fibre-optic bundles after it has traversed the slot.
  • the transmission fibre- optic bundle and the collection fibre-optic bundle are disposed facing one another at opposite sides of the slot.
  • the transmission fibre-optic bundle and the collection fibre-optic bundle are located ⁇ -axis' relative to one another, that is, the collection element lies on an axis parallel to the direction of uninterrupted transmission of light between distal ends of the transmission and the collection elements.
  • the relatively large particle size may result in a 'pin hole' effect where the particles do not completely fill the measurement region and voids are formed in the sample to be measured which allows the light to directly pass through the spaces to the distal end of the collection element and causes blinding (or saturation) of the detector.
  • an optical probe comprising a transmission element and a collecting element each having a distal end at which optical radiation is respectively transmitted into and collected from a sample region of the probe characterised in that the respective distal ends are disposed in an off-axis configuration in which collection at the distal end of the collection element of uninterrupted radiation emitted from the distal end of the transmission element is avoided and in which the distal end of the collection element is located outside an acceptance cone of the transmission element (being generally understood by those skilled in the art to be delimited by the maximum angle of emission, i.e. acceptance angle, from the transmission element).
  • an acceptance cone of the transmission element being generally understood by those skilled in the art to be delimited by the maximum angle of emission, i.e. acceptance angle, from the transmission element.
  • the optical probe may further comprise a probe head having
  • opposing non-parallel surfaces configured as wall portions of a slot for receiving the sample, which slot may be produced either as an open ended or as a closed ended slot; a first optically transparent window disposed in a one of the non parallel surfaces to form an optical interface between received sample and a first channel disposed internal the probe head; and a second optically transparent window disposed in the other of the non parallel surfaces to form an optical interface between received sample and a second channel disposed internal the probe head.
  • the probe head may provide a degree of mechanical protection for the transmission and collection elements, is able to define the relative angle between these elements in a convenient and reproducible manner to facilitate production of the probe and may also be provided with at least a portion of its external surface which is shaped to enhance the flow of material past these elements and/or reduce the influence of the probe on the flow of bulk material in a process line.
  • a method of performing optical analysis of a sample comprising the steps of introducing into a sample distal ends of a transmission element and a collection element of an optical probe; by means of the optical probe, illuminating the sample with optical radiation emitted from the distal end of the transmission element; collecting through the distal end of the collection element the optical radiation after its interaction with the sample; and optically coupling a spectrometric instrument to a proximal end of the collection element of the optical probe to receive collected light for spectrometric analysis wherein the optical probe consist of an optical probe according to the first aspect.
  • the method has associated with it those advantages provided by the probe.
  • an optical analyser comprising a spectrometric instrument; a source of optical radiation and an optical probe having a transmission element and a collection element, the transmission element having a proximal end optically coupled to the source and a distal end for emitting radiation from the source into a sample, the collection element having a proximal end optically coupled to the spectrometric instrument and a distal end for collecting emitted radiation after its interaction with the sample; wherein the optical probe consist of an optical probe according to the first aspect of the present invention and wherein the analyser may be operated to perform the method according to the second aspect of the present invention.
  • Fig. 1 illustrates possible configurations of the transmission
  • FIG. 2 illustrates an optical analyser according to the present invention comprising an optical probe according to Fig.1 ;
  • FIG. 3 illustrates an embodiment of an optical probe usable in the optical analyser of Fig. 2;
  • Fig. 4 illustrates a cross-section of the probe head of Fig. 3.
  • FIG. 5 illustrates a further embodiment of an optical probe according to the present invention.
  • a transmission element 4 is provided with a distal end 6 from which optical radiation is intended to be emitted to pass through a sample region 8 in an
  • the probe 2 also comprises a collection element 10 which has a distal end 12 for receiving optical radiation emitted by the transmission element 4 after its interaction with a sample in the sample region 8.
  • a collection element 10 which has a distal end 12 for receiving optical radiation emitted by the transmission element 4 after its interaction with a sample in the sample region 8.
  • the distal end 12 of the collection element is located relative to the distal end 6 of the transmission element 4 so that light passing from the transmission element 4 cannot reach the collection element 10 without first having interacted with a sample in the sample region 8.
  • both the transmission element 4 and the collection element 10 are conveniently realised as fibre-optic elements, each one of which may comprise a cooperating bundle of optical fibres. It will be appreciated that other elements that can guide optical radiation to and from the sample region 8 may be substituted for the whole or a part of the fibre-optic elements without departing from the invention as claimed.
  • the distal end 12 of the collection element 10 is disposed in an off-axis arrangement relative to the axis A at a location outside a so-called acceptance cone 14 of the transmission element 4 such that collection of emitted radiation which passes through the sample region 8 uninterrupted by any sample is avoided.
  • a fibre optic here transmission element 4
  • the half angle ⁇ of this cone is called the acceptance angle.
  • the acceptance angle ⁇ may be calculated from a knowledge of the indices of refraction of the core (n-i) and the cladding (n2) of the fibre optic element 4 and of the material into which the light will pass (n). This may be expressed as:
  • n sin ⁇ (ni2 - n 2 2 ) 1 ⁇ 2 (1 )
  • the maximum angle over which the optical element can emit or accept light is given by the equivalent, so-called, numerical aperture.
  • the relative orientation of the transmission element 4 and the collection element 10 which fulfils the criterion that light passing from the transmission element 4 cannot reach the collection element 10 without first having interacted with a sample in the sample region 8 may be calculated such relative orientations may also be simply derived experimentally dependent on the material being measured and the application in order to maximise rejection of light that has not interacted with a sample whilst defining a sampling region 8 through which a sample may easily pass.
  • the collection element 10 is
  • the analyser 16 comprises an optical probe, in this exemplary embodiment the optical probe 2 of Fig. 1 , and a spectrometric instrument 18.
  • the instrument 18 is operably connected to a proximal end 20 of the collection element 10, here a fibre-optic element, to receive light there from and to resolve wavelength dependent intensity variations in the received light.
  • a proximal end 22 of the transmission element 4 optically couples to a source of optical radiation, typically a source of NIR optical radiation 24, and functions to guide optical radiation emitted by the source 24 into a sample located in the sample region 8 between the distal ends 6,12 of the transmission fibre-optic 4 and the collection fibre-optic 10 respectively which, by way of example only, are located internal a process line 26 through which a material to be analysed is intended to flow in direction illustrated by the arrow of Fig. 2.
  • Such material may be, for example:
  • Installations in process lines will typically require installation in pipes of different diameters, or in a vessel, tank or storage container with a flat or curved surface.
  • the optical probe of the present invention allows for product to easily flow between the selected angle, such as a 'V shape between a 90° relative disposition to allow grain to easily flow in the sample region 8.
  • the present invention is not limited to applications for in-line analysis in process lines but can also be used to monitor flowing material outside a process line, such as bulk grain on a conveyor moving to or from a storage silo or as it is unloaded from a bulk transporter; in the design of bench analysers of stationary or flowing material or in the design of hand-held analysers of stationary bulk materials such as say grain at grain receiving stations or in bulk transport or storage containers.
  • the optical probe and analyser according to the present invention is immune to the 'pin hole' effect as only light that is scattered through the sample in the sample region 8 will reach the collection fiber 10 (hence reach the detector of the spectrometric instrument).
  • the optical probe according to the present invention may also include a probe head which advantageously provides a degree of mechanical protection for the transmission and collection elements, defines the relative angle between these elements in a convenient manner and also defines a sample region which can be shaped to enhance the flow of material past these elements whilst reducing the influence on the flow of bulk material in a process line.
  • a probe head which advantageously provides a degree of mechanical protection for the transmission and collection elements, defines the relative angle between these elements in a convenient manner and also defines a sample region which can be shaped to enhance the flow of material past these elements whilst reducing the influence on the flow of bulk material in a process line.
  • the optical probe 28 comprises a transmission element 4 and a collection element 10 which are both optically coupled at their distal ends to a probe head 32 that projects into the pipe-line 26 in either permanent or temporary sealing engagement so as to prevent egress of material from the pipe-line 26.
  • the probe head 32 comprises opposing non-parallel surfaces 34, 36 in which surfaces 34,36 are provided windows 38,40 for providing an optical coupling between internal and external the probe head 32.
  • the surfaces 34,36 are inclined relative to one another to form an open- ended slot or groove 49 which delimits the sample region 8 between the windows and through which sample material may readily flow.
  • the probe head 32 may be provided with a surface 39 ("leading edge") generally perpendicular to and facing the direction of flow shaped to reduce any adverse influence that the probe head 32 may have on the flow of material through the pipe-line 26 and/or aid flow of material through the sample region 8 by acting to preferentially direct material to that region 8.
  • the probe head 32 is illustrated in partial cross-section in Fig. 4. As can be seen, an optical window 38 and 40 is located in and parallel to a
  • each window 38, 40 is located in a sealing engagement with an associated channel 42,44 which passes through the probe head 32.
  • optical fibres 46,48 of the transmission element 4 and the collection element 10 respectively pass along an associated channel 42, 44 and terminate with their distal ends 6,12 at or close to the associated window 38,40.
  • each channel 42, 44 may itself act as an optical waveguide to guide optical energy into and out of the sample region 8.
  • the non-parallel opposing surfaces 34,36 are configured to form a groove 49 and are disposed relative to one another such that the fibre core axes A,B of the transmission fibre-optic 46 and the collection fibre-optic 48 respectively are substantially perpendicular to one another so that collection is minimised of optical irradiation by fibre-optic 48 of the collection element 10 which passes from the fibre-optic 46 of the transmission element 4 uninterrupted by any sample in the sample region 8.
  • this is realised by locating the window 40 associated with the collection element 10 outside of the acceptance cone 14 of the transmission element 4, as previously described with respect to the embodiment of Fig. 1.
  • the probe head 32 is also provided with a
  • peripheral flange 51 and compressible ⁇ ' ring 53 by which it is intended to releasably seal the probe head 32 in connection with the pipe-line 26 (or similar wall portions of other material containers such as reaction vessels, ingredient, intermediate final or waste product storage tanks).
  • the flange 51 is here provided with through holes 55 for receiving bolts to engage with threaded portions of the pipe-line 26.
  • Such a releasable connection facilitates the removal of the probe head 32 for cleaning, repair or replacement.
  • the probe-head 32 may be sealed in a more permanent manner to the appropriate wall section by means of welds or the like.
  • the optical probe 50 comprises an elongate, here generally cylindrical, rigid body portion 52 having, at its distal end a generally conical probe head 54 forming a 'tip' that, due to its shape, can provide a reduced resistance to insertion into a sample material.
  • the probe head 54 may be formed from or provided with a coating of low friction material (PTFE for example).
  • the probe head 54 has, in the present embodiment, formed in it a closed slot 56 which is delimited by opposing, non-parallel surfaces 58,60.
  • An optically transparent window 62 is located in sealing connection with a one of the non-parallel surfaces 58 to form a protective optical interface between a distal end of an internal transmission fibre-optic 66 and a sample region 68 within the slot 56.
  • the transmission fibre-optic 66 is provided to transmit optical radiation from external the probe 50, along internal the body portion 52 to exit the optical window 62 and illuminate sample within the sample region 68.
  • an optically transparent window 64 is located in a sealing
  • the collection fibre-optic 70 is provided to transmit optical radiation emitted from the transmission fibre-optic 66 after its interaction with sample material in the sample region 68 along internal the body portion 52 to exit the optical probe 50 at a proximal end 72.
  • the locations of their associated windows 62,64 are selected such that the associated fibre core axes are not parallel with one another and such that window 64 associated with the collection fibre-optic 70 lies outside the acceptance cone of the transmission fibre-optic 66.
  • the collection by the collection fibre-optic 70 of radiation which passes uninterrupted through the sample region 68 from the transmission fibre- optic 66 is at least reduced and preferably avoided.
  • the size of the slot is not limited by the absorption properties of the material being sampled and so the risk of sample failing to be exchanged as the material under analysis and the optical probe are moved relative to one another is reduced.
  • the transmission fibre-optic 66 and the collection fibre-optic 70 may be replaced with any suitable optical waveguide without departing from the invention as claimed.
  • the probe head 54 may be formed with an open- ended slot 49 similar to that of the head 32 described in relation to Fig. 3 and Fig.4 and that the probe head 32 of Figs. 3 and 4 may be formed with a closed slot similar to that slot 56 described in respect of the head 50 of Fig. 5.
  • a flexible optical coupling 74 is optically
  • optical waveguides most suitably fibre-optic guides 76,78, which provide an optical connection between the transmission fibre-optic 66 and a source of optical radiation (not shown) and between the collection fibre- optic 70 and a spectrometric instrument or other optical analyser (not shown).
  • this probe 50 may be formed as a 'lance' in which the rigid body portion 52 may be of the order of 1 meter of more for insertion, for example into stationary bulk granular material in a silo or container. In another embodiment this probe 50 may be formed as a 'pen' in which the rigid body portion 52 may be of the order of a few tens of centimetres for insertion into small, bench-top, sample volumes of granular or liquid material.
  • the probe head 54 is introduced into a sample causing sample to flow into the sample region 68 formed by slot 56 whereby distal ends of the
  • transmission element 66 and the collection element 70 of the optical probe are optically coupled to the sample via associated windows 62,64.
  • the sample is then illuminated with optical radiation emitted from the distal end of the transmission element 66 which is collected through the distal end of the collection element 70 after its interaction with the sample in the sample region 68. Relative movement of the probe and the sample will cause new sample material to be exchanged with the old sample material that was in the sample region 68.
  • a spectrometric instrument is provided optically coupled to a proximal end of the collection element of the optical probe to receive collected light for spectrometric analysis.

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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)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne une sonde optique comprenant une tête de sonde (32) renfermant un élément de transmission (4), comprenant de préférence une fibre optique (46) et un élément collecteur (10), et comprenant de préférence une fibre optique (48), lesquels possèdent chacun une extrémité distale (6, 12) au niveau de laquelle le rayonnement optique est respectivement transmis dans et recueilli par un volume de réception d'échantillon (8) défini au moins en partie par les parois latérales opposées et non parallèles (34, 36) de la tête de sonde (32) dans laquelle les extrémités distales respectives (6, 12) se terminent. Les extrémités distales respectives (6, 12) sont disposées selon une configuration hors axe dans laquelle l'extrémité distale (12) de l'élément collecteur (10) se situe à l'extérieur du cône d'acceptance (14) de l'élément de transmission (4) afin d'éviter le recueil, à l'extrémité distale (12) de l'élément collecteur (10), d'un rayonnement ininterrompu émis par l'extrémité distale (6) de l'élément de transmission (4).
PCT/EP2010/063148 2010-09-08 2010-09-08 Sonde optique Ceased WO2012031625A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/EP2010/063148 WO2012031625A2 (fr) 2010-09-08 2010-09-08 Sonde optique

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2010/063148 WO2012031625A2 (fr) 2010-09-08 2010-09-08 Sonde optique

Publications (2)

Publication Number Publication Date
WO2012031625A2 true WO2012031625A2 (fr) 2012-03-15
WO2012031625A3 WO2012031625A3 (fr) 2013-03-28

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2010/063148 Ceased WO2012031625A2 (fr) 2010-09-08 2010-09-08 Sonde optique

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6137108A (en) 1998-06-17 2000-10-24 Foss Nirsystems Incorporated Instrument and method for spectroscopic analysis by reflectance and transmittance
US6737649B2 (en) 2002-04-16 2004-05-18 Foss Nirsystems, Inc. Infrared analysis instrument with offset probe for particulate sample

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4934811A (en) * 1988-04-01 1990-06-19 Syntex (U.S.A.) Inc. Apparatus and method for detection of fluorescence or light scatter
US5278412A (en) * 1992-08-18 1994-01-11 Nirsystems Incorporated System for measuring the moisture content of powder and fiber optic probe therefor
US5835649A (en) * 1997-06-02 1998-11-10 The University Of British Columbia Light directing and collecting fiber optic probe
JP4316818B2 (ja) * 2001-03-01 2009-08-19 大塚電子株式会社 光散乱測定プローブ
US6879741B2 (en) * 2002-11-04 2005-04-12 C Technologies, Inc Sampling end for fiber optic probe
WO2007000166A1 (fr) * 2005-06-27 2007-01-04 Sfk Technology A/S Enregistrement de spectres d’absorption de longueur d’onde spécifiques à la position
DE202005011177U1 (de) * 2005-07-15 2006-11-23 J & M Analytische Mess- Und Regeltechnik Gmbh Vorrichtung zur Analyse, insbesondere fotometrischen oder spektralfotometrischen Analyse

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6137108A (en) 1998-06-17 2000-10-24 Foss Nirsystems Incorporated Instrument and method for spectroscopic analysis by reflectance and transmittance
US6737649B2 (en) 2002-04-16 2004-05-18 Foss Nirsystems, Inc. Infrared analysis instrument with offset probe for particulate sample

Also Published As

Publication number Publication date
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