WO2005031291A1 - Sonde a fibre optique ramifiee et systeme correspondant - Google Patents

Sonde a fibre optique ramifiee et systeme correspondant Download PDF

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Publication number
WO2005031291A1
WO2005031291A1 PCT/US2004/031930 US2004031930W WO2005031291A1 WO 2005031291 A1 WO2005031291 A1 WO 2005031291A1 US 2004031930 W US2004031930 W US 2004031930W WO 2005031291 A1 WO2005031291 A1 WO 2005031291A1
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WO
WIPO (PCT)
Prior art keywords
probe
fiber optic
fibers
spec
bifurcated
Prior art date
Application number
PCT/US2004/031930
Other languages
English (en)
Inventor
Wang-Long Zhou
Yongwu Yang
Shaoqing Peng
Victor Sapirstein
Original Assignee
Wang-Long Zhou
Yongwu Yang
Shaoqing Peng
Victor Sapirstein
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 Wang-Long Zhou, Yongwu Yang, Shaoqing Peng, Victor Sapirstein filed Critical Wang-Long Zhou
Publication of WO2005031291A1 publication Critical patent/WO2005031291A1/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
    • G01N21/84—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
    • G01J3/02—Details
    • 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
    • G01N21/359—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
    • 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
    • G01N21/4738—Diffuse reflection, e.g. also for testing fluids, fibrous materials
    • G01N21/474—Details of optical heads therefor, e.g. using optical fibres
    • G01N2021/4742—Details of optical heads therefor, e.g. using optical fibres comprising optical fibres
    • G01N2021/475—Bifurcated bundle
    • 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
    • G01N2021/4764—Special kinds of physical applications
    • G01N2021/4769—Fluid samples, e.g. slurries, granulates; Compressible powdery of fibrous samples
    • 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
    • G01N2201/06—Illumination; Optics
    • G01N2201/063—Illuminating optical parts
    • G01N2201/0638—Refractive parts
    • G01N2201/0639—Sphere lens

Definitions

  • the present invention relates to an analytical probe device. More specifically, the invention relates to a bifurcated fiber optic probe and system that minimizes internal reflectance and maximizes the capture of signal light.
  • Analytical probes are commonly used to monitor and control various environmental, biological, and industrial conditions. Such probes may be used to sample matter ranging from pure liquids, pastes and slurries to powders, solids and gases, all of which can be sampled at varying temperature, pressure and pH values. Such probes may be provided in a variety of sizes, shapes and optical configurations in order to accommodate the variety of matter being sampled.
  • Some probe designs include moving parts and a plurality of optical components.
  • the movable parts contribute to focusing and alignment errors, and the plurality of optical components can lead to imprecise sampling analyses however.
  • Other probe designs include at least one optical component shielded by a flat window surface. Contaminants gathered on the flat window can degrade a probe's efficacy over time however.
  • Still other probes include a focusing lens and an illuminating source, whereby the sample positioned some fixed distance from the lens is
  • Some conventional probe systems incorporate a light source, an optical analyzer with a detector, and a light transport conduit.
  • the light transport conduit is often comprised of fiber optic cables.
  • the light source is typically a laser or a filtered white light source, such as a xenon or mercury lamp.
  • single fiber solutions are used in combination with a dichroic beam splitter and well-aligned coupling optics.
  • the efficacy of such single-fiber solutions is questionable, however, as back-scattered excitation and illumination light at the fiber- coupling site are difficult to reduce. Further, the suppression of auto-fluorescence induced in the fiber optic cable by excitation light is also difficult to reduce in such single-fiber systems.
  • NIR Near Infra Red
  • An analytical probe device that is easy to assemble and use, and that minimizes internal reflectance while maximizing the capture of signal light is desirable.
  • the invention accomplishes the minimizing of internal relectance and the maximizing of light captured by using a ball lens in combination with a dual-fiber bundle.
  • an NIR probe comprising a bifurcated fiber optic probe usable with a spectrometer or other computer-controlled instrument.
  • the bifurcated fiber optic probe comprises a probe tube having a first end and a second end; a lens mount placed within the probe tube proximate the first end; a ball lens received within the lens mount; a fiber optic bundle extending within said probe tube between the lens mount and the second end; and a probe handle connecting the probe to the spectrometer or other computer-controlled instrument, wherein the ball lens and fiber optic bundle combining to minimize internal reflectance and maximize light gathering of objects analyzed by the probe.
  • Figure 1 illustrates schematically the probe with the ball lens and fiber optic bundle according to the invention.
  • Figures 2 A and 2B illustrate various aspects of the fiber bundle arrangement according to the invention.
  • Figure 3 illustrates the light collection efficiency pattern of the ball lens and the fiber bundle according to the invention.
  • Figure 4 shows the back reflection of the fiber bundle, ball lens and optical window according to the invention.
  • Figure 5 illustrates a bifurcated probe with a handle and a serial port extension according to the invention.
  • Figure 6 illustrates a probe handle with a trigger according to the invention.
  • Figure 7 illustrates a serial port connection for a trigger and LED's according to the invention.
  • the invention comprises a bifurcated fiber optic probe and system.
  • the probe provides for incoming and outgoing light for instruments such as Near Infra Red (NIR) and Fourier Transform (FT) IR spectrometers.
  • NIR Near Infra Red
  • FT Fourier Transform
  • the probe is ideally suited for research, process and quality control in chemical, agricultural, food and pharmaceutical applications.
  • the system coordinates spectrometer functions and analysis by activating spectral acquisition.
  • the bifurcated fiber optic probe of the system is designed for low internal reflection and efficient light gathering of the samples being analyzed. This effect is achieved preferably by the combination of a geometrically arranged fiber optic bundle coupled with, or in proximity with, a ball lens of defined aperture.
  • the design of the probe and system permits easy use thereof in repetitive testing environments. Therefore, without limiting the applicability of the invention to such, the invention will be described in such environment.
  • the components of the present invention will be described, with reference now to the drawings.
  • Figure 1 shows a probe 100 with a ball lens 120 and optical window 130 in accordance with the principles of the present invention.
  • the probe 100 comprises a
  • the optical window 130 protects the ball lens 120 from scratches, dirt, contaminants or other undesirable conditions. In similar manner, the optical window 130 also protects the fiber optic bundle 150 housed within the fiber bundle ferrule 140 of the probe 100.
  • the optical window 130 is a sapphire window, though the artisan will appreciate that any material of known optical and spectral properties providing for the transmission of the source and reflected light therethrough can be used.
  • the fiber bundle ferrule 140 is shown to hold the fiber optic bundle 150 in place within the probe, the artisan will appreciate that other known devices such as holders, fasteners and sleeves can also be used to position the fiber optic bundle 150 in place within the probe.
  • the optical design of the probe 100 comprises using a ball lens 120.
  • the ball lens 120 is particularly useful for creating large diverged beam, as is preferred in measuring powder samples.
  • the ball lens 120 aspect of the invention provides advantages over conventional plano-convex or convex-convex lenses.
  • the ball lens 120 tends to increase alignment precision due to its ball shape and tends to yield higher efficiencies due to its shorter focal length as compared to probes using conventional plano-convex or convex-convex lenses having longer focal lengths.
  • the ball lens 120 is held within a lens mount 110 such that the ball lens rests on the fiber bundle ferrule 140 in a horizontally centered position within the probe 100, as shown in Figure 1.
  • the top of the fiber bundle should be at or near the focal plane of the ball lens.
  • the lens mount 110 may be machined to accommodate this positioning, whereby the lens mount is machined to allow for a distance (D) between a top of the fiber optic bundle 150 and a bottom of the ball lens 120. Therefore, this distance will be equal or close to the back focal length of the spherical lens, i.e., the focal length minus spherical radius. It's normally less than a few millimeters, depending on the diameter and refractive index of the ball lens.
  • the lens mount 110 is preferably made of stainless steel since the probe may be used in corrosive environments.
  • any material known in the art can instead be employed as the lens mount, such as, for
  • the lens mount 110 is machined to automatically center and align the spherical lens when placed within the lens mount, assembly of the probe 100 is simplified.
  • the compact configuration of the fiber optic bundle 150, lens mount 110, spherical lens 120 and optical window 130 within the probe 100 also tends to minimize vibrations. Analytical results tend to be more consistent as a result.
  • Figures 2 A and 2B illustrate an exemplary geometric arrangement of the fiber optic bundle 150 in accordance with the principles of the invention.
  • a plurality of fibers 151 are arranged generally concentrically around a central one of the fibers 151 to comprise the closely packed fiber optic bundle 150.
  • the total number of fibers 151 may vary, but the total number is preferably one of a set of numbers 7, 19, 37, 61, 91, ..., for forming a closely packed hexagon pattern.
  • the number of fibers is 37, as shown in Figures 2A and 2B, in order to almost equally separate the fibers 151 into two regions, i.e., an outer layer 160 and an inner layer 170.
  • the outer layer 160 (also referred to as the source fibers) form an almost circular annulus of 18 fibers, whereas the inner layer 170 (also referred to as the signal fibers) form an inner core with 19 fibers.
  • the outer layer 160 also referred to as the source fibers
  • the inner layer 170 also referred to as the signal fibers
  • each individual fiber can range from 25 micron to 700 micron, but is preferably between 100 ⁇ 400 micron in considering light collecting efficiency and fiber bundle flexibility. Basically, a smaller diameter fiber has a bigger portion of dead area (cladding and buffer) that does not collect light, while a larger diameter fiber is prone to breaking when bended.
  • the combination of the ball lens 120 and the geometry of the fiber optic bundle 150 described above tends to produce a minimum amount of internal reflection (reflected light entering fibers going back to the spectrometer) and a maximum amount of signal light capture (sample reflection or acquisition efficiency).
  • the ratio of the captured signal to the internal reflection (noise) to reflected signal is preferably larger than 5:1.
  • Figure 3 illustrates an example of the high efficiency light gathering effect of a probe having a ball lens 120 used in combination with the lens mount 110 and geometry of the fiber optic bundle 150, as described above.
  • the angle ⁇ can be approximately calculated as
  • the efficiency of scattered light collection using a ball lens 120 and the geometry of the fiber optic bundle 150, according to the invention, is thus more than 3 times larger than the efficiency of scattered light collected by conventional planoconvex or convex-convex lenses.
  • the increased efficiency is due in part to the shorter focal length of the spherical lens 120 as compared to the longer focal length of a regular lens having the same aperture.
  • the spherical lens 120 thus allows for high precision when monitoring a range of mixed compositions or systems, such as solids, particles, liquids, vapors, powders and slurries.
  • Figure 4 illustrates other advantages of the combination of the ball lens 120 and the geometric fiber optic bundle 150 in a probe according to the invention. More specifically, Figure 4 illustrates that the combination of the ball lens 120 and the geometry of the fiber optic bundle 150 according to the invention tends to minimize back reflection from various components of the probe. Measurements taken show that the back reflection with uncoated ball lens and window is between 0.1% and 0.5%, typically 0.2 ⁇ 0.3%, compared to the typical value of -1% for the case with a planoconvex lens and a window.
  • the back reflection from the flat surfaces of the optical window 130 should preferably be approximately zero, regardless of whether a ball lens or a plano-convex lens is used, since the incoming light from each of the source fibers 160 is collimated and the reflection of one side should go to the opposite source fibers 160 (not signal fibers 170).
  • Theoretical calculation shows that, even with a plano-convex lens, the back reflection could be less than 0.05%.
  • back reflection due to perfect alignment, collimation, and centralization of the fiber bundle relative to ball lens, etc., back reflection is non-avoidable. In other words, the value of measured back reflection reflects the degree of imperfectness of assembly of the lens, window, and fibers. This is why the back reflection with a plano-convex lens is much higher than that with a ball lens, because the centralization and alignment with a plano-convex lens are much more difficult than the case with a ball lens.
  • Figure 5 shows an exemplary NIR probe system according to the invention.
  • the system is comprised of the probe that houses, ter alia, the ball lens 120, the lens mount 1 10, and the geometric fiber optic bundle 150, as discussed above.
  • the system further comprises a probe handle 504 and a serial port connection cable 506.
  • the probe handle 504 connects the probe 100 to the spectrometer (not shown), or other computer-controlled instrument, via the serial port connection cable 506.
  • the serial port connection cable 506 includes a serial port connector 505 (shown schematically in Figure 7) that connects the probe 100 via the cable 506 to the spectrometer, for example.
  • the probe handle 504 further comprises a trigger 503.
  • the trigger 503 is connected via the serial port 505 to the spectrometer, or other known computer-controlled instrument, to co-ordinate signal acquisition and data analysis of the samples being observed by the probe 100.
  • a software program for example, may be used to help co-ordinate the signal acquisition and data analysis by the spectrometer or other instrument.
  • depression of the trigger 503 activates the spectrometer, or other instrument, to which the probe 100 is connected in order to begin processing the data received from the probe 100.
  • the activation of the spectrometer in this manner is evidenced by indicator means, such as LED's 501 and 502, provided in the probe handle 504 as also shown in Figure 6.
  • the serial port connector 505 connects the trigger 503, the LED's 501, 502, and the probe 100 in general, for example, to the spectrometer.
  • a four-wire configuration maybe used to wire the trigger 503, the LED's 501, 502 and the probe 100 to the spectrometer using the serial port connector 505. Because the trigger 503 is powered through the serial port connection 505, the LED's 501, 502 are powered by the spectrometer, or other computer-controlled instrument, rather than from the probe 100, to indicate the status of the system overall.
  • the serial port connector 505 is a 9- ⁇ in RS-232 (recommended standard 232) serial port connector.
  • the RS-232 standard supports two types of connectors, a 25-pin D-type connector (DB-25) and a 9-pin D-type connector (DB-9).
  • DB-25 25-pin D-type connector
  • DB-9 9-pin D-type connector
  • a 9-pin connector was used in developing the invention, the artisan will appreciate that other than a 9-pin connector can be used as is known in the art.
  • the serial interface itself including the trigger 503, LED's 501 and 502, and the pin connection structure, uses the serial port Clear To Send (pin 8) or Data Set Ready (pin 6) to read back serial inputs, and sends out Window Commands to change states of Request To Send (pin 7) and Data Terminal Ready (pin 4).
  • the serial inputs can come from a simple trigger switch or character commands.
  • the power from an RTS or DTR line for the CTS or DSR line is used to monitor the serial inputs. This eliminates the need for using a battery for CTS or DSR line monitoring which is ordinarily used.
  • the interface class can also be modified for read and write through commonly used USB ports.
  • the serial interface of the present invention serves as an object (“class”) that can read, write and monitor up to all serial ports.
  • the present invention can send data to the instrument control system, data analysis system, laboratory information management system and/or data archival system to which it interfaces when an event occurs on any of the ports monitored.
  • the "class” creates a thread for reading, writing and monitoring the available ports, while the main program operation can go unimpeded.
  • These systems include but are not limited to any of the known software packages on the market including LABVIEW®, MERLIN®, GRAMS®, and ERECORD MANAGERTM.
  • the system of the present invention can encompass other embodiments including increasing the fiber diameter, which is preferably 400 micron. This change may necessitate an increase in spherical lens diameter (and lens mount diameter), and an alteration in lens-fiber separation distance to compensate for these changes while preserving internal reflection and light gathering functions. Such changes should be readily appreciated by the artisan to be made in proportions or dimensions as would accommodate the desired ratio of signal capture to internal reflectance as described hereinabove. Similarly, the number of fibers in the bundle can be increased as long as the annular geometry of the outer fibers is maintained. Although described herein with respect to NIR or (FT)NIR spectroscopy, the artisan should readily appreciate that the system can also be used for other forms of reflective spectroscopy including fluorescence. Likewise, the system can also be performed in UV mode if the lens and fibers are converted to quartz, or other appropriate materials known in the art.

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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)

Abstract

La présente invention concerne un système de sonde à fibre optique ramifiée (100), conçu pour permettre l'obtention d'une réflexion interne limitée et d'un rassemblement de lumière efficace. Le système est une combinaison d'un faisceau de fibres optiques (150) de géométrie particulière couplé à, ou à proximité d'une lentille sphérique (120) d'ouverture définie alignée au centre de la sonde. Le système permet l'acquisition spectrale et l'analyse spectrale d'échantillons grâce à différents types de spectroscopie, en ciblant un rapport de la lumière capturée sur la réflectance interne pour chaque échantillon observé par la sonde. La géométrie de la sonde à fibre optique et sa relation par rapport à la lentille sphérique (120) joue un rôle pour atteindre le rapport souhaité.
PCT/US2004/031930 2003-09-22 2004-09-22 Sonde a fibre optique ramifiee et systeme correspondant WO2005031291A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US50552503P 2003-09-22 2003-09-22
US60/505,525 2003-09-22

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WO2005031291A1 true WO2005031291A1 (fr) 2005-04-07

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007006039A3 (fr) * 2005-07-05 2007-06-14 Univ Texas Procede et appareil de spectroscopie a resolution en profondeur
FR2949560A1 (fr) * 2009-09-02 2011-03-04 Centre Nat Rech Scient Systeme de spectroscopie a guide d'onde pour l'analyse de particules dans un milieu
WO2018147498A1 (fr) * 2017-02-13 2018-08-16 (주)이오테크닉스 Coupleur optique et dispositif laser le comprenant

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6608671B2 (en) * 1998-07-17 2003-08-19 Vertex Pharmaceuticals (San Diego) Llc Detector and screening device for ion channels
US20030191398A1 (en) * 2002-04-05 2003-10-09 Massachusetts Institute Of Technology Systems and methods for spectroscopy of biological tissue

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6608671B2 (en) * 1998-07-17 2003-08-19 Vertex Pharmaceuticals (San Diego) Llc Detector and screening device for ion channels
US20030191398A1 (en) * 2002-04-05 2003-10-09 Massachusetts Institute Of Technology Systems and methods for spectroscopy of biological tissue

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007006039A3 (fr) * 2005-07-05 2007-06-14 Univ Texas Procede et appareil de spectroscopie a resolution en profondeur
US7499161B2 (en) 2005-07-05 2009-03-03 The Board Of Regents Of The University Of Texas System Depth-resolved spectroscopy method and apparatus
FR2949560A1 (fr) * 2009-09-02 2011-03-04 Centre Nat Rech Scient Systeme de spectroscopie a guide d'onde pour l'analyse de particules dans un milieu
WO2011027067A1 (fr) * 2009-09-02 2011-03-10 Centre National De La Recherche Scientifique - Cnrs Système de spectroscopie de fluorescence par corrélation temporelle pour l'analyse de particules dans un milieu
WO2018147498A1 (fr) * 2017-02-13 2018-08-16 (주)이오테크닉스 Coupleur optique et dispositif laser le comprenant

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