WO2006092252A2 - Sonde atr a haute temperature - Google Patents

Sonde atr a haute temperature Download PDF

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Publication number
WO2006092252A2
WO2006092252A2 PCT/EP2006/001756 EP2006001756W WO2006092252A2 WO 2006092252 A2 WO2006092252 A2 WO 2006092252A2 EP 2006001756 W EP2006001756 W EP 2006001756W WO 2006092252 A2 WO2006092252 A2 WO 2006092252A2
Authority
WO
WIPO (PCT)
Prior art keywords
probe
radiation
head
atr
fibre
Prior art date
Application number
PCT/EP2006/001756
Other languages
English (en)
Other versions
WO2006092252A3 (fr
Inventor
Stephen Etienne
Ian Weaver
Original Assignee
Astrazeneca Uk Limited
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 Astrazeneca Uk Limited filed Critical Astrazeneca Uk Limited
Publication of WO2006092252A2 publication Critical patent/WO2006092252A2/fr
Publication of WO2006092252A3 publication Critical patent/WO2006092252A3/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
    • G01N21/84—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
    • 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
    • G01N21/17—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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/55—Specular reflectivity
    • G01N21/552—Attenuated total reflection
    • 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
    • G01N21/09—Cuvette constructions adapted to resist hostile environments or corrosive or abrasive materials

Definitions

  • This invention relates to attenuated total reflection (so-called "ATR") probes.
  • Such probes typically comprise an elongated, tubular body having a specially configured head at one end.
  • Such probes also typically comprise means, remote from the head, for generating infra-red ("IR") radiation, and for passing it along the elongated body to the head, which is placed in communication with a fluid which it is desired to investigate (hereinafter called “sample fluids"); the relative refractive indices of the head material and the sample fluid being contrived such that most of the IR energy is reflected back into the probe, where it is directed onto a sensor device capable of recording the amount of IR energy incident thereon.
  • sample fluids a fluid which it is desired to investigate
  • the amount of IR radiation received by the sensor when compared with the known amount of IR radiation originally generated and passed along the probe, provides an indication as to whether or not the sample fluid contains certain constituents, and can also be used to evaluate the relative amounts of such constituents in the sample fluid.
  • the wavelength of the IR radiation used can be varied in a known manner to produce a plot of radiation loss versus wavelength which can be used in known manner to identify or otherwise characterise the sample fluid and/or constituents thereof.
  • the invention has especial, though not exclusive, application to the transmission of radiation in the mid infra-red wavelength range down a conduit to and from an ATR head in a manner which facilitates usage of the ATR probe in contact with hot sample fluids.
  • An additional aspect of the invention relates to the incorporation of a diamond ATR head constructed and configured to be utilised at n
  • MIR mid-infra-red region
  • NIR near-infra-red
  • fibre types are particularly robust and they can only be operated at moderate temperatures.
  • One such fibre type (chalcogenide) can only be operated at temperatures up to around 10OC, whilst the second type (silver halide) suffers from cold flow, a phenomenon which causes the putty-like silver halide material to flow gradually with time, thereby potentially disrupting the integrity of MIR transmission. Cold flow is exacerbated as the temperature is increased.
  • hollow waveguides do not, in general, suffer from the above difficulties, and can be employed in the MIR, their use in ATR probes has hitherto been inhibited, since their use renders it difficult to make the probe as a whole substantially explosion proof.
  • solid fibres running in and out of a tubular probe can be encapsulated, thereby eliminating flame paths, so rendering the
  • ATR probe tips at MIR wavelengths.
  • These standard materials are optically efficient because, in addition to transmitting in the MIR, they can easily be fashioned into the required shape or form, such as a corner cube reflector. These materials show varying degrees of chemical resistance. If a particularly aggressive and reactive chemical product is to be probed, however, a diamond tip must be used. This is not only extremely expensive but is optically inferior to probes using tips fabricated from the aforementioned standard materials. Diamond, by necessity of cost and manufacture, tends to be used either in the form of small crystals or in thin sheets.
  • Coupling IR radiation to and from a small crystal or a thin sheet is not optically efficient, and optical throughputs are significantly reduced compared with those achievable for materials that can be made into large corner cube designs. It is also difficult to configure a narrow probe to have a high number of internally reflecting interactions with the sample fluid under investigation.
  • the present invention aims to address at least one of the foregoing problems or difficulties associated with the fabrication of ATR probes, particularly for use at MIR wavelengths.
  • an ATR probe formed with an elongate, generally tubular body with a head at one end comprises at least one high temperature tolerant hollow waveguide means disposed in a region of the body exposed, in use of the probe, to relatively high temperatures and at least one solid fibre means disposed in a region of the body exposed, in use of the probe, to relatively low temperatures; the waveguide means and the fibre means being disposed to sequentially convey infra-red ("IR”) radiation to and/or from said head.
  • IR infra-red
  • The, or each, hollow waveguide may conveniently comprise a light pipe, and an internal surface of at least one such light pipe may be coated to reduce radiation losses associated with reflections thereat.
  • a waveguide means and a fibre means are optically coupled together in end-to-end relationship.
  • go and return paths for IR radiation along said tubular probe comprise respectively: (a) a first fibre means optically coupled to a first hollow waveguide means; and (b) a second hollow waveguide means optically coupled to a second fibre means.
  • the optical coupling comprises at least one lens means, and it is further preferred that the waveguide means is optically coupled to a tip device incorporated in said head of the probe.
  • the tip device is typically, in operation of the probe, disposed in direct contact with a sample fluid.
  • encapsulant means is provided around the said fibre means and configured and located so as to seal said tubular body.
  • a diamond tip device may be provided; said device being resistive to chemical attack by the sample fluid and/or configured to enhance optical coupling and to enable a variable number of interacting internal reflections to be achieved.
  • a further aspect of the invention provides an ATR probe comprising a tubular body provided at one end with a head intended to be placed in communication with a sample fluid and radicals
  • substantially planar member formed substantially of diamond; the body containing respective channels for conveying IR radiation towards and away from the head and means for coupling said radiation from and to a coupling zone of said head; wherein the substantially planar member extends away from said coupling zone towards a tip-like extremity of the member; the width of said member being relatively broad in the region of said coupling zone and relatively narrow at said extremity, characterised in that the member is inclined to the axis of the tubular body, causing in use radiation coupled into the member to repeatedly bounce between opposite surfaces thereof to enhance interaction of the radiation with the sample fluid, and that the coupling zone of the member is angled to accommodate the inclination.
  • Figure 1 shows, in longitudinal cross sectional view, components of an ATR probe in accordance with one example of the invention
  • Figure 2 shows graphs explanatory of relationships between certain parameters of the probe shown in Figure 1 ;
  • Figures 3, 4, 5 and 6 show respective views of a preferred configuration usable at the head of an ATR probe.
  • a standard ATR probe typically constitutes a tubular body with solid fibre optics disposed to run, in a generally longitudinal direction, along a substantial part of the length of the body.
  • the fibre optic material is, as mentioned above, typically either chalcogenide or silver halide.
  • IR radiation from a suitable source, is focussed into a first fibre and then collimated at the fibre exit plane by an appropriately placed first lens. This radiation is directed toward, and transits, an ATR head which is typically formed with a tip-like extremity, and is then focussed back into a second (return) fibre, disposed parallel to the first fibre, by a second lens placed at an equivalent, but offset, position to the first lens.
  • the lenses are positioned so as to abut the ATR head. Part at least of the region of the tubular body around the solid fibres is encapsulated to render the probe substantially explosion proof.
  • an ATR probe 10 high temperature operation of an ATR probe 10 is facilitated by incorporating into a tubular body 15 of the probe, made from Hastelloy (Registered Trade Mark) or stainless steel or any other self-supporting and otherwise suitable material, solid fibres 20, 30 and collimating lenses 40, 50 substantially as described above.
  • the fibres 20 and 30 do not approach the head (100) of the probe; instead, collimated radiation exiting from lens 40 is directed into a hollow waveguide, such as a first light pipe 60, which optically couples the lens 40 to the ATR head 100.
  • a second hollow light pipe 70 disposed parallel to the first light pipe 60, is used to collect radiation returning from the ATR head 100 and the second lens 50 re-focuses the returning radiation into the second fibre 30.
  • the fibre 20 and the waveguide 60 are disposed to sequentially convey MIR radiation to the head.
  • the waveguide 70 and the fibre 30 are disposed to sequentially convey MIR radiation away from the head 100, along the probe and towards a suitable sensor (not shown).
  • the fibres 20, 30 and the light pipes 60, 70 are all disposed so as to run generally longitudinally of the tubular body 15 of the probe 10.
  • An interface adapter 95 locates the waveguides 60, 70 relative to the head 100 and the end of the tubular body 15.
  • each fibre 20, 30 and its respective hollow waveguide 60, 70 are optically coupled together, via the lenses 40, 50 respectively, in end-to-end relationship.
  • Each of the hollow waveguides 60, 70 is, moreover, optically coupled to the head 100 of the probe.
  • the hollow light pipes 60, 70 are subjected to the high temperature of the sample fluid, but the solid fibres 20, 30 are disposed in a cooler region. Part at least of the region of tubular body 15 surrounding the solid fibres 20, 30 is encapsulated, as indicated at 90, to render the probe 10 substantially explosion proof.
  • the collimating lens 40 which directs outgoing radiation into light pipe 60 does not yield a perfectly collimated beam of IR due, mainly, to the finite size of the optical components in the probe.
  • the radiation exiting from lens 40 therefore exhibits a range of angles, centred on a collimated beam, causing some radiation to "bounce" down the inside of the light pipe 60.
  • N (LVD)tan ⁇ , where L is the length of pipe, D is the internal diameter and ⁇ is the average glancing angle.
  • the overall system will be characterised by a figure of merit "F/#", with radiation directed from the exit plane of the fibre 30 onto a detector (not shown) at a particular F/# being matched to the F/# of radiation being directed into the fibre 20; radiation overfilling the re-focusing 'collimating' lens, giving a lower F/# than the system F/#, will be lost.
  • the optical arrangement is symmetrical, with two identical collimating lenses and two light pipes of equal diameter, then the optimum diameter of the light pipes is that which maintains the system F/#.
  • the internal diameters of the light pipe 60 should match the diameter of the radiation beam exiting the first collimating lens 40.
  • Figure 2 details the transmission of light pipes of varying length as a function of diameter for radiation of divergence half angle 12.5 degrees, indicating that, for these particular parameters, optimum transmission occurs at a pipe diameter of 3mm.
  • radiation is coupled from a first fibre 20 via a collimating lens 40 to the light pipe 60 - ATR head 100 - light pipe 70 complex and then back to a second fibre 30 using a second (focussing) lens 50, which effectively provides the reverse optical function to the collimating lens 40, to maintain the F/#.
  • the free space radiation divergence of radiation in the system is relatively small, to simply couple optical fibres directly to the respective light pipes.
  • the divergence half angle within the ATR probe is decreased by the ratio of free space to material refractive index. If the free space divergence half-angle is 12 degrees and the fibre material is ZnSe, the equivalent divergence angle within the ATR probe is 5 degrees, which is acceptable. Using this option, a large number of optical fibres can be used to both couple radiation to the output light pipe and collect radiation from the return light pipe.
  • one particularly preferred head arrangement utilises a thin sheet-like member 200 of diamond, shaped and configured as shown in Figure 3.
  • the member 200 tapers to a tip 210, having a 90 degree apex angle, and is formed with an optical insertion/extraction surface 220 (facing into the tubular probe body), angled such that the diamond member 200 as a whole is inclined at 45 degrees to the longitudinal axis of the tubular probe body, and thus to the insertion and extraction radiation beam lines, whilst the insertion/extraction optical surface 220 is disposed normal to these beam line directions. This is shown in Figures 4 and 5.
  • This configuration promotes "bouncing" of radiation inserted into the optical face 220 from a lens collimating from a fibre or from a light pipe (e.g. the light pipe 60 of the probe shown in Figure 1 ) or any other suitable optical conduit, whereby the radiation propagates through the member 200 by undergoing repeated total internal reflections at 45 degrees at the top and bottom surfaces 230, 240 as shown in figure 4. Radiation is reflected across the tip 210 at its 90 degree apex; travels back to the optical surface 220 and is collected by an element of an optical extraction system (such as the light guide 70 of the probe shown in figure 1 ). The repeated "bouncing" of the radiation between the top and bottom surfaces of member 200 enhances interaction between the radiation and the sample fluid. By varying the length and width of the diamond member 200, it will be appreciated that different numbers of interacting reflections can be realised.
  • the diamond member 200 can conveniently be mounted to a probe 10 in the manner indicated in Figure 6, such that its front surface 230 is framed by a suitably angled and knife-edged window aperture 260 supported by the tubular probe body 15 and thereby exposed to the sample fluid.
  • the inner lip of the knife- edged window aperture 260 is provided with a gold frame, against which the front surface 230 is urged by a pressure fitment applied from behind the rear surface 240 of the member 200; and applied to the rear surface 240 by way of a second gold frame squeezed between the periphery of the rear surface 240 and the rear pressure fitment such that the main portion of the rear surface 240 is free standing.
  • the diamond member 200 is sealed into the window 260 with low risk of damage, and the majority of its rear surface 240 is left clear of contact with any of the fitting components, thus avoiding any significant compromise on the internal reflection performance of that surface of the diamond 200.
  • the entrance/exit surface 220 of the diamond member 200 is, in this example, similarly mounted, using a gold frame, to the ATR probe's tubular body.
  • the diamond member 200 may be brazed into the body 15 of the probe 10.
  • the present invention provides a high temperature, substantially explosion proof ATR probe and enables operation of an efficient and easily configurable chemically resistant ATR probe, where these novel concepts can be configured separately or together as a high temperature, substantially explosion proof and chemically resistant ATR probe.

Abstract

L'invention concerne une sonde à réflexion totale atténuée (ATR) comprenant un corps allongé doté d'une tête à une extrémité. Cette sonde est conçue pour être utilisée avec des échantillons fluidiques très chauds et présente des avantages particuliers lors d'utilisation de rayonnements infrarouges situés dans la zone de rayonnement infrarouge moyen (MIR) du spectre, généralement acceptée comme s'étendant dans la plage de longueurs d'onde allant de 3 à 10 µm. Afin de surmonter les difficultés qui surviennent lors d'utilisation de matériaux ATR classiques utilisés pour construire de telles sondes, la sonde ATR de l'invention comprend un guide d'ondes creux monté dans une zone du corps exposé à des températures relativement élevées, et une fibre solide disposée dans la zone du corps exposée à des températures relativement faibles. Le guide d'ondes et la fibre sont agencés pour transmettre séquentiellement des rayonnements infrarouges jusqu'à la tête de la sonde et/ou à partir de la tête de la sonde. Le guide d'onde creux comprend de préférence un conduit léger. L'invention concerne également une tête ATR en diamant construite et conçue pour être utilisée à hautes températures et permettant d'améliorer la résistance chimique de la sonde ATR dans son ensemble à des matière potentiellement corrosives contenues dans les échantillons fluidiques.
PCT/EP2006/001756 2005-03-01 2006-02-27 Sonde atr a haute temperature WO2006092252A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0504148A GB2423816A (en) 2005-03-01 2005-03-01 High Temperature ATR Probe
GB0504148.8 2005-03-01

Publications (2)

Publication Number Publication Date
WO2006092252A2 true WO2006092252A2 (fr) 2006-09-08
WO2006092252A3 WO2006092252A3 (fr) 2006-10-26

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2006/001756 WO2006092252A2 (fr) 2005-03-01 2006-02-27 Sonde atr a haute temperature

Country Status (3)

Country Link
AR (1) AR052678A1 (fr)
GB (1) GB2423816A (fr)
WO (1) WO2006092252A2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007058611A1 (de) * 2007-12-04 2009-06-10 Endress + Hauser Conducta Gesellschaft für Mess- und Regeltechnik mbH + Co. KG ATR-Sonde
DE102015007844A1 (de) 2014-06-30 2015-12-31 Engel Austria Gmbh Kunststoffherstellung auf Basis eines diskontinuierlich polymerisierenden Monomers

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201012764D0 (en) * 2010-07-30 2010-09-15 Element Six N V A diamond window component for a laser tool
GB201015379D0 (en) * 2010-09-15 2010-10-27 Element Six N V A diamond optical component for an optical tool

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5051551A (en) * 1989-05-18 1991-09-24 Axiom Analytical, Inc. Immersion probe for infrared internal reflectance spectroscopy
US5170056A (en) * 1991-02-28 1992-12-08 Galileo Electro-Optics Corporation Optical fiber coupled devices for remote spectroscopy in the infrared
US5418615A (en) * 1994-02-25 1995-05-23 Axiom Analytical, Inc. Probe for liquid sample analysis by light transmission
US5703366A (en) * 1994-05-13 1997-12-30 Asi Applied Systems, L.L.C. Optical sensing with crystal assembly sensing tip
US5923808A (en) * 1997-06-23 1999-07-13 Melling; Peter J. Mid-infrared fiber-optic spectroscopic probe for use at elevated temperatures
WO2004013621A1 (fr) * 2002-07-24 2004-02-12 Endress + Hauser Conducta Gmbh+Co. Kg Dispositif d'analyse spectrometrique infrarouge d'un milieu solide, liquide ou gazeux

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GB1294176A (en) * 1969-06-24 1972-10-25 Wilks Scientific Corp Analysing device
US6205272B1 (en) * 1998-02-27 2001-03-20 Equitech Int'l Corp. Fiber optic probe for attenuated total internal reflection spectrophotometry
US5991029A (en) * 1998-04-06 1999-11-23 Axiom Analytical, Inc. Attenuated total reflecance probe employing large incidence angles
JP2004085433A (ja) * 2002-08-28 2004-03-18 Nippon Denshi Raiosonikku Kk 高温高圧試料用ａｔｒプローブおよび高温高圧試料用セル

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5051551A (en) * 1989-05-18 1991-09-24 Axiom Analytical, Inc. Immersion probe for infrared internal reflectance spectroscopy
US5170056A (en) * 1991-02-28 1992-12-08 Galileo Electro-Optics Corporation Optical fiber coupled devices for remote spectroscopy in the infrared
US5418615A (en) * 1994-02-25 1995-05-23 Axiom Analytical, Inc. Probe for liquid sample analysis by light transmission
US5703366A (en) * 1994-05-13 1997-12-30 Asi Applied Systems, L.L.C. Optical sensing with crystal assembly sensing tip
US5923808A (en) * 1997-06-23 1999-07-13 Melling; Peter J. Mid-infrared fiber-optic spectroscopic probe for use at elevated temperatures
WO2004013621A1 (fr) * 2002-07-24 2004-02-12 Endress + Hauser Conducta Gmbh+Co. Kg Dispositif d'analyse spectrometrique infrarouge d'un milieu solide, liquide ou gazeux

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007058611A1 (de) * 2007-12-04 2009-06-10 Endress + Hauser Conducta Gesellschaft für Mess- und Regeltechnik mbH + Co. KG ATR-Sonde
DE102015007844A1 (de) 2014-06-30 2015-12-31 Engel Austria Gmbh Kunststoffherstellung auf Basis eines diskontinuierlich polymerisierenden Monomers

Also Published As

Publication number Publication date
WO2006092252A3 (fr) 2006-10-26
GB0504148D0 (en) 2005-04-06
GB2423816A (en) 2006-09-06
AR052678A1 (es) 2007-03-28

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