WO1996012174A1 - Sonde pour analyse optique en direct - Google Patents

Sonde pour analyse optique en direct Download PDF

Info

Publication number
WO1996012174A1
WO1996012174A1 PCT/SE1995/001149 SE9501149W WO9612174A1 WO 1996012174 A1 WO1996012174 A1 WO 1996012174A1 SE 9501149 W SE9501149 W SE 9501149W WO 9612174 A1 WO9612174 A1 WO 9612174A1
Authority
WO
WIPO (PCT)
Prior art keywords
probe
tube
reaction vessel
sample
light
Prior art date
Application number
PCT/SE1995/001149
Other languages
English (en)
Inventor
Robert Nobel
Original Assignee
Arums Ltd.
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 Arums Ltd. filed Critical Arums Ltd.
Publication of WO1996012174A1 publication Critical patent/WO1996012174A1/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

Definitions

  • the present invention refers to a probe for on-line optical analysis of the contents in a reaction vessel. More specifically, the invention refers to a probe for insertion into a reaction vessel in order to determine the contents thereof by on-line optical analysis, the probe comprising a first light transmitting means in a tube which extends into the vessel and is intended for transmittance of light to a measuring portion containing a sample of the contents, the light being passed through the sample, reflected against a reflector and received by a second light transmitting means in the tube for analysis of the illuminated sample outside the reaction vessel
  • optical devices have been con ⁇ structed for spectral. analysis of the reflectivity, trans- flectance and/or transmittance of a sample.
  • a device for on-line use is shown in US-A-5 044 755 wherein an op- tical rod is used for propagating light from a light source, such as an optical fibre bundle.
  • the probe com ⁇ prises furthermore reflecting means for the light leaving the optical rod as well as focusing means for the light leaving and entering the rod.
  • the reflecting means is ar ⁇ ranged at the end of the probe for altering the path-length of the light in the sample.
  • US-A-5 168 367 discloses a variable path length spectrophotometric probe surrounding a gap or a flow chamber for illuminaton of a sample, the flow chamber having an inlet and an outlet for liquid flow.
  • the probe has optical fibres arranged on one side of the flow chamber and a stepper motor for regulating a mirror - and thus the path length of the light - arranged on the opposite side of said chamber.
  • This optical probe is designed for measurements in pipings such as a middle piece on a pipe and can not be used for measurements in a reaction tank in si tu.
  • a probe for industrial processes must usually be quite robust and retain its measuring capacity throughout the process. This is especially important under harsh con ⁇ ditions.
  • proteinaecous substances often adheres to impellers or the like in the reaction vessels.
  • material is deposited on the walls inside the reaction vessel, in pipelines, and thus also on a probe if it is inserted therein. If such a film is formed on parts in the light path of the probe, a deterioration of the measuring properties is obtained.
  • Other sources of instability such as changes in sensit ⁇ ivity, lamp aging, or electronic long term changes, can cause deviations. The analysis will be affected each time this happens, and the results obtained will be unreliable.
  • the probe has to be removed for a more or less time consuming cleaning procedure with subsequent calibration of its measuring properties.
  • optical fibres are used for conveying light, energy is lost each time light passes from one medium to another.
  • a quartz rod is used for guiding an optical fibre to a lens, and energy is lost when light passes from the optical fibres to the quartz rod and vice versa.
  • the purpose of the invention is to achieve a probe for on-line optical analysis of the contents in a reaction vessel, whereby the above-mentioned problems are eliminated.
  • FIG 1 is a side view, partly in section, of the probe according to the invention.
  • FIG 2 is a magnification of a measuring portion of the probe in FIG 1.
  • the probe 1 is composed of a body 2 with a through bore 3 into an open part of a measuring portion 4 of the probe 1.
  • a tube 5 is inserted which contains two optic fibre bundles (not shown) , one for conveying light from a light source (not shown) to said open part and one for transmitting re- turning light to a detector in an instrumentation (not shown) .
  • a piston 6 is axially movable in a housing 7 integral with the body 2, a cylinder room 8 being formed at either side of the piston.
  • the piston 6 having a tubular base por ⁇ tion 9 is attached to a tubular piston rod 10 by means of a mounting nut 11.
  • the tube 5 is inserted in the piston rod 10 and attached by means of a further nut 12.
  • Via inlets 13 in the wall of the housing 7 pneumatic medium is delivered to either side of the piston 6 in the cylinder room 8 for controlling the position of the piston 6.
  • the cylinder room 8 is to the left in the drawing pro ⁇ vided with a shoulder 14 for defining one end position of the piston 6.
  • a cavity 15 at the end of the base portion 9 at least one spacer 16 is inserted between the base por ⁇ tion 9 and a shoulder on the piston rod 10.
  • the spacer en ⁇ gages the wall of said cavity when the piston 6 is moved to the right in the drawing.
  • the stroke of the piston 6 as well as the piston rod 10 and tube 5 is thus determined by the shoulder 14 and the spacer 16, respectively.
  • O-rings 17 are arranged between the base portion 9 of the piston 6 and the housing 7 in order to retain the pneumatic medium with ⁇ in the cylinder room 8.
  • the probe may also be designed so that the piston is controlled by means of a stepping motor.
  • the probe is inserted in a reaction vessel, a pipe or the like and secured by means of a mounting flange 18 pro ⁇ vided with screw holes 19 for mounting screws.
  • the tube 5 can then be removed from the probe during the process in the reaction vessel without opening the reaction vessel to the ambient atmosphere.
  • the small diameter of the probe results in that it can be inserted and mounted in most of the standard flanges in the process industry.
  • the spacer 16 which is used to adjust the fixed stroke can also be replaced without opening the reaction vessel by replacing it with another spacer or inserting a new one. This is achived by dissembling the housing 7 and removing the nut 11 which is used to fasten the piston 6 to the piston rod 10.
  • the piston rod 10 is mounted from the opposite side of the probe and has a shoulder (not shown) which prevents the piston rod from being removed through the housing.
  • the part of the probe 1 which extends into the reac ⁇ tion vessel is shown in FIG 2 in more detail.
  • the open part of the measuring portion 4, threaded on the body 2, is fur ⁇ nished with four openings 20.
  • a sleeve 21, through which the two optic fibre bundles run, is threadedly attached in the end of the tube 5.
  • an annular membrane 23 is clamped by means of a nut 24, the membrane 23 also being clamped between the body 2 and the measuring portion 4 of the probe 1.
  • a lens 25 is seated against the end of the nut 24, and a sealing ring 26 is arranged within this seat.
  • the lens 25 is secured by means of a nut 27 adapted to the lens 25.
  • the two optic fibre bundles terminate close to the lens 25.
  • a metal reflector 28 is arranged at the end of the measuring portion 4, whereby a gap 29 is achieved for continuous reception of material from the reaction vessel through the openings 20.
  • the re ⁇ flector is arranged at the end of a screw 30 which is threaded into the end of the measuring portion 4 and is secured by a lock nut 31.
  • the metal parts of the probe 1 are preferably made of acid-resistant steel.
  • the purpose of the flexible membrane 23 is arranged in order to prevent material, especially under severe conditions, to penetrate between the piston rod 10 and the body 2 and for example cause scratches on the surfaces.
  • the membrane 23 is preferably made of Kalrez,, a material which is preferably also used for the sealing ring 26.
  • the lens 25 can be replaced by a window and is pre ⁇ ferably made of sapphire.
  • the reflector 28 is preferably made in one piece with the screw 30 and polished.
  • the lens 25 and the reflector 28 can also be made of other materials in order to prevent adhesion of substances in the reaction vessel.
  • the tube 5 replaces the quartz rod which is often used for guiding light in devices similar to that of the present invention, and this arrangement prevents the loss of energy when light is passed from the optical fibres to the quartz rod and vice versa.
  • the probe according to the invention can also be con ⁇ structed as a flow-through cell. Two opposite openings 20 of the measuring portion 4 are then plugged up and the two remaining openings 20 are connected to inlet and outlet ports.
  • the probe according to the invention is preferably intended to be used for analyzing the near infra red (NIR) absorbance spectrum of an illuminated sample, but other spectra can also be analyzed.
  • NIR near infra red
  • the entire NIR spectral range (400 nm - 2400 nm) of a sample in the form of a liquid, powder or slurry can be analyzed with respect to reflectivity, trans- flectance and/or transmittance.
  • the stroke of the piston and thus the tube 5 is first set and, if necessary, adjusted by means of the spacer 16 which engages the wall of the cavity 15.
  • the stroke can according to the invention be varied from 0,5 up to 6 mm, but a stroke of 2 mm is often sufficient.
  • the probe is then set up in respect to the particular application to be used by positioning the reflector 28 in relation to the lens 25.
  • the gap 29 is adjusted with the screw 30 and then firmly fixed with the lock nut 31. This gap 29 can be varied between 0,5 and 20 mm.
  • the probe is then inserted in the reaction vessel, and at regular time intervals the piston 6 is by a pneumatic controller moved from this first position to a second position, i.e. when the piston 6 en ⁇ gages the shoulder 14, the path-length of the measurings portion 4 of said probe 1 thereby being lengthened.
  • a pneumatic controller moved from this first position to a second position, i.e. when the piston 6 en ⁇ gages the shoulder 14, the path-length of the measurings portion 4 of said probe 1 thereby being lengthened.
  • the measurings immediately before and after such a change are compared, for example by dividing or subtracting the NIR spectra with or from each other, respectively.
  • the spectrum achieved with one of the path-lengths of the gap 29 is thus used as a reference or background, and the other path-length is used for the analysis.
  • the new calculated quote or difference spectrum will be an excellent spectral description of the medium, suit ⁇ able for chemometric calculations of various chemical and physical parameters, free from effects of film formation, optical changes, detector instability and light source aging.

Landscapes

  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • 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

Sonde (1) destinée à être introduite dans une cuve de réaction afin de déterminer le contenu de cette dernière par analyse optique en direct. Ladite sonde comprend un premier dispositif émetteur de lumière situé dans un tube (5) qui s'étend dans la cuve et est destiné à transmettre de la lumière à une partie de mesure (4) contenant un échantillon du contenu. La lumière est envoyée à travers l'échantillon, réfléchie par un réflecteur (28) et reçue par un second dispositif émetteur de lumière situé dans le tube (5) en vue de l'analyse de l'échantillon illuminé à l'extérieur de la cuve de réaction. Des dispositifs (6-8) situés à l'extérieur de la cuve de réaction à l'extrémité du tube sont disposés de manière à modifier la longueur de parcours entre le dispositif émetteur de lumière dans le tube (5) et le réflecteur (28) pour obtenir différentes mesures de l'échantillon.
PCT/SE1995/001149 1994-10-18 1995-10-06 Sonde pour analyse optique en direct WO1996012174A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE9403543A SE9403543D0 (sv) 1994-10-18 1994-10-18 Method and probe for on-line optical analysis
SE9403543-3 1994-10-18

Publications (1)

Publication Number Publication Date
WO1996012174A1 true WO1996012174A1 (fr) 1996-04-25

Family

ID=20395644

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/SE1995/001149 WO1996012174A1 (fr) 1994-10-18 1995-10-06 Sonde pour analyse optique en direct

Country Status (2)

Country Link
SE (1) SE9403543D0 (fr)
WO (1) WO1996012174A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0806653A1 (fr) * 1996-05-09 1997-11-12 Perstorp Analytical, Inc. Une sonde à longueur de parcours optique variable pour l'analyse spectrométrique des substances visqueuses au moyen de mesures de la transmission ou de la réflexion optique, et mèthode pour son emploi
US6244118B1 (en) 1997-12-23 2001-06-12 Astrazeneca Ab Sampling apparatus
US7259848B2 (en) 2001-06-28 2007-08-21 Endress + Hauser Conducta Gesellschaft Fur Mess-Und Regeltechnik Mbh + Co. Kg Process measuring point
WO2008034945A1 (fr) * 2006-09-20 2008-03-27 Moventas Oy Procédé et dispositif destinés à surveiller l'état d'un milieu
US8873057B2 (en) 2009-12-10 2014-10-28 Foss Analytical A/S Variable path length probe
WO2023041787A1 (fr) 2021-09-20 2023-03-23 Implen GmbH Sonde à immersion présentant une longueur de trajet variable

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0145877A2 (fr) * 1983-11-04 1985-06-26 Hartmann & Braun Aktiengesellschaft Photomètre pour l'analyse en continu d'un milieu (gaz ou liquide)
US5044755A (en) * 1989-03-03 1991-09-03 Lt Industries Probe for transmitting and receiving light from a sample
US5168367A (en) * 1991-01-16 1992-12-01 Rourke Patrick E O Variable path length spectrophotometric probe

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0145877A2 (fr) * 1983-11-04 1985-06-26 Hartmann & Braun Aktiengesellschaft Photomètre pour l'analyse en continu d'un milieu (gaz ou liquide)
US5044755A (en) * 1989-03-03 1991-09-03 Lt Industries Probe for transmitting and receiving light from a sample
US5168367A (en) * 1991-01-16 1992-12-01 Rourke Patrick E O Variable path length spectrophotometric probe

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0806653A1 (fr) * 1996-05-09 1997-11-12 Perstorp Analytical, Inc. Une sonde à longueur de parcours optique variable pour l'analyse spectrométrique des substances visqueuses au moyen de mesures de la transmission ou de la réflexion optique, et mèthode pour son emploi
US6244118B1 (en) 1997-12-23 2001-06-12 Astrazeneca Ab Sampling apparatus
US7259848B2 (en) 2001-06-28 2007-08-21 Endress + Hauser Conducta Gesellschaft Fur Mess-Und Regeltechnik Mbh + Co. Kg Process measuring point
WO2008034945A1 (fr) * 2006-09-20 2008-03-27 Moventas Oy Procédé et dispositif destinés à surveiller l'état d'un milieu
US8873057B2 (en) 2009-12-10 2014-10-28 Foss Analytical A/S Variable path length probe
WO2023041787A1 (fr) 2021-09-20 2023-03-23 Implen GmbH Sonde à immersion présentant une longueur de trajet variable
DE102021210443A1 (de) 2021-09-20 2023-03-23 Implen GmbH Tauchsonde mit variabler Pfadlänge
DE102021210443B4 (de) 2021-09-20 2023-07-27 Implen GmbH Tauchsonde mit variabler Pfadlänge

Also Published As

Publication number Publication date
SE9403543D0 (sv) 1994-10-18

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