EP0817982A1 - Cuve a flux optique utilisee en analyse spectrale - Google Patents

Cuve a flux optique utilisee en analyse spectrale

Info

Publication number
EP0817982A1
EP0817982A1 EP96941803A EP96941803A EP0817982A1 EP 0817982 A1 EP0817982 A1 EP 0817982A1 EP 96941803 A EP96941803 A EP 96941803A EP 96941803 A EP96941803 A EP 96941803A EP 0817982 A1 EP0817982 A1 EP 0817982A1
Authority
EP
European Patent Office
Prior art keywords
flow cell
probes
optical
optical flow
end portion
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.)
Withdrawn
Application number
EP96941803A
Other languages
German (de)
English (en)
Inventor
Aharon Bornstein
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.)
Israel Atomic Energy Commission
Original Assignee
Israel Atomic Energy Commission
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 Israel Atomic Energy Commission filed Critical Israel Atomic Energy Commission
Publication of EP0817982A1 publication Critical patent/EP0817982A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/24—Coupling light guides
    • G02B6/36—Mechanical coupling means
    • G02B6/38—Mechanical coupling means having fibre to fibre mating means
    • G02B6/3807—Dismountable connectors, i.e. comprising plugs
    • G02B6/3873—Connectors using guide surfaces for aligning ferrule ends, e.g. tubes, sleeves, V-grooves, rods, pins, balls
    • 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
    • G01N21/05—Flow-through cuvettes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N2021/0346—Capillary cells; Microcells
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/24—Coupling light guides
    • G02B6/36—Mechanical coupling means
    • G02B6/38—Mechanical coupling means having fibre to fibre mating means
    • G02B6/3807—Dismountable connectors, i.e. comprising plugs
    • G02B6/3833—Details of mounting fibres in ferrules; Assembly methods; Manufacture
    • G02B6/3854—Ferrules characterised by materials
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/24—Coupling light guides
    • G02B6/36—Mechanical coupling means
    • G02B6/38—Mechanical coupling means having fibre to fibre mating means
    • G02B6/3807—Dismountable connectors, i.e. comprising plugs
    • G02B6/3873—Connectors using guide surfaces for aligning ferrule ends, e.g. tubes, sleeves, V-grooves, rods, pins, balls
    • G02B6/3874—Connectors using guide surfaces for aligning ferrule ends, e.g. tubes, sleeves, V-grooves, rods, pins, balls using tubes, sleeves to align ferrules

Definitions

  • the invention refers to an optical flow cell for use in spectral analysis.
  • the invention relates to optical flow cells for use in spectral analysis in association with suitable spectrometers, for example in liquid and gas chromatography.
  • suitable spectrometers for example in liquid and gas chromatography.
  • a stream of a monitored fluid is continuously flown though the flow cell and a radiation beam is transmitted across the flowing fluid and the exiting beam is detected and analyzed.
  • Different designs of such optical flow cells are disclosed, for example, in US 4,540,280, 4,588,893, 5,078,493 and 5,151,474.
  • optical flow cells of the kind specified comprise a housing with two intersecting throughgoing bores, one for the flow of a fluid to be analyzed and the other for the transmission of radiation which latter is fitted with means for directing the radiation towards and away from the bore.
  • the two throughgoing bores form a fluid cavity and in order to ensure a desired length of an optical path across the fluid passing through the fluid cavity and to prevent the fluid from penetrating into the radiation transmitting bore, two oppositely located transparent windows are provided which separate the fluid cavity from the adjacent portions of the radiation transmitting bore.
  • the windows are either mounted directly in the housing of the flow cell, such as for example in US 4,588,893, or they constitute the end faces of optical probes inserted in the radiation transmission bore through both ends thereof, such as for example in US 5,078,493.
  • the radiation arriving at one end of the radiation transmit ⁇ ting bore is directed via a first transparent window to a fluid sample located inside the fluid cavity whilst radiation exiting from the sample across a second window is transmitted to a spectrometer.
  • the windows In order to ensure in such prior art devices a high accuracy of measurement which in turn depends on the degree by which the dimensions of the fluid cavity correspond to design values, the windows must be appropriately manufactured and positioned so as to maximize the accuracy of compliance of the distance between the windows, known in the art as end separation, with the design value, and to minimize transverse and angular misalignments of the windows.
  • the flow cell design must provide for a high degree of repeatability on each reassembly.
  • specific measures must be taken for the windows to withstand extreme conditions, e.g. high pressure and/or high temperature, under which flow cells of the kind specified most often operate.
  • an optical flow cell for use in spectral analysis of the kind that comprises a housing formed with intersecting first and second bores forming between them a fluid cavity, which first and second bores serve, respectively, for fluid throughflow and radiation transmission, said second bore holding in a fluid tight fit and releasable fashion two radiation transmitting optical probes having each an outer end portion and an inner end portion with an inner end face, the outer end portion of one probe being linked to a radiation source and the outer end portion of another probe being linked to a spectrometer, the inner end faces of the probes facing said fluid cavity and being spaced from each other; characterized in that each of said optical probes is an optical fiber cable having a ferrule mounted on the inner end portion of the cable and firmly held in an associated radiation transmitting bore section.
  • the flow cell according to the present invention has a relatively simple construction in which the end faces of the fiber optic cables of the optical probes are in direct contact with the analyzed fluid whereby the need for windows is obviated.
  • This enables mutually engaging surfaces of the ferrule and the housing, which are involved in setting of a required distance between the end faces of the optical probes, to be disposed relatively remote from the fluid cavity, whereby practically no fluid or at least no particles, if any, comprised therein can reach the engaging surfaces.
  • the ferrules are selected from among materials, e.g. metals, which provide for the required mechanical properties and resistance to corrosion by the analyzed fluid.
  • the housing is in the form of a sleeve coaxial with the radiation transmitting bore.
  • each fiber optic probe is fitted with sealing means mounted, adjacent the inner end face thereof, between the ferrule of the probe and an end portion of the inner surface of the associated radiation transmitting bore section.
  • the sealing means may be of any suitable kind such as, for example, an O-ring or where the ferrule and the sleeve are ferromagnetic, a ferrofluid material.
  • the flow cell according to the present invention is especially advantageous when a small volume of an analyzed sample and consequently a small size fluid cavity are required.
  • the required small dimension of the fluid cavity is readily achievable by mounting the fiber optic probes in such a manner that their end faces project into the fluid cavity to an appropriate extent and further by choosing a small diameter optical fiber cable.
  • the fluid cell according to the present invention is specifically advantageous for use in IR analysis in general, and of liquid solutions in particular, which latter have very high absorption in the mid IR region and, therefore, put severe limitations on the length of the optical path.
  • Fig. 1 is a cross-sectional view of a fiber optic flow cell according to the present invention
  • Fig. 2 is a cross-sectional view of a section of the sleeve of the fiber optic flow cell shown in Fig. 1, drawn to a larger scale;
  • Fig. 3 is a cross-sectional view of a fiber optic probe used in the fiber optic flow cell shown in Fig. 1;
  • Fig. 4 shows portion A of the fiber optic flow cell shown in Fig. 1, drawn to a larger scale.
  • the fiber optic flow cell according to the present invention shown in the drawings is adapted for use in spectrometric analysis, in particular for IR absorption measurements of fluids (liquids and gases).
  • the fiber optic flow cell 1 comprises a cylindrical sleeve or adaptor 2, which is formed with a relatively broad radiation throughgoing bore 3 serving for radiation transmission and transversal fluid throughgoing bore 4 serving for the passage of a fluid F to be analyzed, bores 3 and 4 defining at their intersection a fluid cavity 5.
  • the flow cell 1 further comprises two fiber optic probes 6 and 7 inserted into the radiation transmission bore 3 of the sleeve 2 at opposite ends 8, 9 thereof.
  • One of the fiber optic probes, e.g. probe 6 transmits radiation R from a radiation source (not shown) to the fluid cavity 5 and the other probe 7 collects the radiation exiting from the fluid cavity 5 and transmitting it to a spectrometer (not shown).
  • the fiber optic probes 6 and 7 of the flow cell 1 are identical and the structure of such a probe is schematically illustrated in Fig. 3. As shown, the probe is in the form of a transparent optical fiber cable 10 surrounded by a tubular ferrule 11, both the fiber and the ferrule being made of materials inert to the fluid to be analyzed.
  • the ferrule 11 may be in the form of any standard connector.
  • the fiber optical cable used in the flow cell may be of a single mode type, in which case it may have a diameter as small as 3-5 microns, or of the multi-mode type.
  • the ferrule 11 is formed with a circumferential abutment shoulder 12 spaced from an end face 13 of the probe to an extent that ensures that when the two probes 6 and 7 are mounted in the radiation transmission bore 3 with the shoulders 12 of the probes abutting on the end surfaces 8 and 9 of sleeve 2, the end faces 13 of the probes project into the fluid cavity 5 to such an extent as to obtain a desired end separation therebetween.
  • each fiber optic probe 6, 7 is provided with a sealing 14 mounted in a space between the radiation transmission bore 3 and the ferrule 11 of the probe 6, 7 adjacent the end face 12 thereof.
  • the sealing 14 may be, for example, in the form of an O-ring (schematically shown in dotted lines in Fig. 3) or rather in the form of a ferrofluid material, in which case the ferrule and/or the sleeve or parts thereof should be made of magnetic material.
  • the fiber optic probes 6, 7 are secured in the sleeve 2 by means of connector nuts 15.
  • fluid F of which absorbance is to be measured is introduced into the fluid cavity 5 via one of the narrow fluid bores 4 and is discharged through the other bore 4 in a manner known per se and not designated in the drawings.
  • the fluid is illuminated by a radiation beam delivered through one of the fiber optic probes, say probe 6.
  • the radiation is transmitted across the fluid cavity 5, and is collected by fiber optic probe 7 and directed thereby to a spectrometer.
  • the fluid cavity of the flow cell can have very small dimensions and, consequently, can provide for an extremely small volume of sample to be analyzed, about 30 pl, whereby a high optical sensitivity of the cell is achieved so that low concentration e.g.
  • the fiber optic cell according to the present invention may have design features different from those described above.
  • the flow cell may be employed for spectrometric analysis using radiation other than infrared, in which case the fluid cavity may have a longer optical path, i.e. the distance between the end faces of the fiber optic probes may be equal to or even be greater than the width of the transverse fluid flow bores.
  • the sleeve may be other than cylindrical and may be held in an appropriate casing.
  • the abutment shoulders of the probes may be constitut- ed by annular rims around their end faces. The shoulders may be adapted to abut on spacings arranged inside the sleeve rather than abutting on outer, end surfaces thereof.
  • the fixed position of the fiber optic probes in the sleeve may be achieved by any other suitable means.

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (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)
  • Optical Measuring Cells (AREA)

Abstract

Cuve (1) à flux optique conçue pour être utilisée en analyse spectrale et comprenant un boîtier (2) pourvu de premier et second passages (4, 3) venant en intersection l'un avec l'autre et constituant entre eux une cavité (5) à fluide. Ces premier et second passages (4, 3) servent, respectivement, à la circulation du fluide et à la transmission du rayonnement. Le deuxième passage (3) renferme, de façon étanche et détachable, deux sondes optiques (6, 7) transmettant le rayonnement et possédant chacune une partie terminale extérieure et une partie terminale intérieure comportant une face terminale intérieure (13). La partie terminale extérieure d'une sonde (6) est reliée à une source de rayonnement et la partie terminale extérieure d'une autre sonde (7) est reliée à un spectromètre, les faces terminales intérieures (13) des sondes faisant face à la cavité (5) à fluide et étant éloignées l'une de l'autre. Chacune des sondes optiques (6, 7) se présente sous la forme d'un câble (10) à fibres optiques, dont la partie terminale intérieure comporte une virole (11) maintenue solidement dans une section du passage associé de transmission de rayonnement.
EP96941803A 1996-01-31 1996-12-31 Cuve a flux optique utilisee en analyse spectrale Withdrawn EP0817982A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
IL11697296 1996-01-31
IL11697296A IL116972A0 (en) 1996-01-31 1996-01-31 Optical flow cell for use in spectral analysis
PCT/IL1996/000195 WO1997028477A1 (fr) 1996-01-31 1996-12-31 Cuve a flux optique utilisee en analyse spectrale

Publications (1)

Publication Number Publication Date
EP0817982A1 true EP0817982A1 (fr) 1998-01-14

Family

ID=11068492

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96941803A Withdrawn EP0817982A1 (fr) 1996-01-31 1996-12-31 Cuve a flux optique utilisee en analyse spectrale

Country Status (4)

Country Link
EP (1) EP0817982A1 (fr)
AU (1) AU1107897A (fr)
IL (1) IL116972A0 (fr)
WO (1) WO1997028477A1 (fr)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6008055A (en) * 1998-06-30 1999-12-28 Transgenomic, Inc. Modular component fiber optic fluorescence detector system, and method of use
US6752537B2 (en) * 2001-02-12 2004-06-22 Polymicro Technologies, Llc Connector ferrule and method of sealing
US6888636B2 (en) 2001-03-19 2005-05-03 E. I. Du Pont De Nemours And Company Method and apparatus for measuring the color properties of fluids
EP2124036A1 (fr) * 2008-05-20 2009-11-25 Agilent Technologies, Inc. Pré-positionnement et mécanisme de guidage pour insérer une cellule à flot continu dans un détecteur
WO2011093775A1 (fr) * 2010-01-28 2011-08-04 Ge Healthcare Bio-Sciences Ab Détecteur optique à cuve de circulation
DE102010050679B3 (de) * 2010-11-05 2012-03-01 Institut Für Photonische Technologien E.V. Justierbare Aufnahmevorrichtung für mikrofluidische Chips mit einzukoppelnder optischer Faser / einzukoppelnden optischen Fasern
GB201506095D0 (en) 2015-04-10 2015-05-27 Ge Healthcare Bio Sciences Ab Optical flow cell for an optical measuring device
GB201506132D0 (en) * 2015-04-10 2015-05-27 Ge Healthcare Bio Sciences Ab Device for holding a light guide, and method for manufacturing such a device
CN117538348B (zh) * 2023-11-17 2025-03-07 北京锐达仪表有限公司 大测量范围的插入式高精度辐射检测装置

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4374620A (en) * 1981-01-29 1983-02-22 Altex Scientific, Inc. Photometric flow cell
DE3337131A1 (de) * 1983-10-12 1985-04-25 Siemens AG, 1000 Berlin und 8000 München Glasfaserdurchfuehrung durch eine wandoeffnung eines gehaeuses
DE3338315A1 (de) * 1983-10-21 1985-05-02 Standard Elektrik Lorenz Ag, 7000 Stuttgart Optoelektrische koppelanordnung
US4844869A (en) * 1985-09-09 1989-07-04 Ord, Inc. Immunoassay apparatus
JPH01129161A (ja) * 1987-11-16 1989-05-22 Hitachi Ltd 粒子計測用フローセル光学系
US5302272A (en) * 1992-03-05 1994-04-12 Beckman Instruments, Inc. Fiber optic flow cell for detection of electrophoresis separation with a capillary column and method of making same
US5291030A (en) * 1992-06-04 1994-03-01 Torrex Equipment Corporation Optoelectronic detector for chemical reactions

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9728477A1 *

Also Published As

Publication number Publication date
IL116972A0 (en) 1996-05-14
WO1997028477A1 (fr) 1997-08-07
AU1107897A (en) 1997-08-22

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