WO2002027302A2 - Dispositif et procede permettant l"analyse de liquides - Google Patents

Dispositif et procede permettant l"analyse de liquides Download PDF

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Publication number
WO2002027302A2
WO2002027302A2 PCT/EP2001/010843 EP0110843W WO0227302A2 WO 2002027302 A2 WO2002027302 A2 WO 2002027302A2 EP 0110843 W EP0110843 W EP 0110843W WO 0227302 A2 WO0227302 A2 WO 0227302A2
Authority
WO
WIPO (PCT)
Prior art keywords
optical conductor
analysis device
light source
coating
fluid
Prior art date
Application number
PCT/EP2001/010843
Other languages
German (de)
English (en)
Other versions
WO2002027302A3 (fr
Inventor
Karsten Sassenscheid
Original Assignee
Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
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 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. filed Critical Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
Priority to EP01982323A priority Critical patent/EP1320744A2/fr
Publication of WO2002027302A2 publication Critical patent/WO2002027302A2/fr
Publication of WO2002027302A3 publication Critical patent/WO2002027302A3/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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/7703—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides
    • 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
    • G01N21/84—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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/7703—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides
    • G01N2021/7706—Reagent provision
    • G01N2021/773—Porous polymer jacket; Polymer matrix with indicator
    • 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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7769—Measurement method of reaction-produced change in sensor
    • G01N2021/7783—Transmission, loss
    • 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
    • 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

Definitions

  • the invention relates to a device and a method for analyzing fluids, in particular fuels and lubricants such as oils or fats.
  • composition of a particular fluid it has so far been necessary to examine this fluid in a complex reagent analysis in a chemical laboratory. However, this applies not only to the composition of a particular fluid, but also to its condition to determine its fitness for a particular purpose.
  • Motor oil is the class of substances that, in addition to the basic components made from mineral oil, also contain additives such as viscosity index improvers (VI), dispersants. Contain greedings, wear inhibitors, antioxidants as well as corrosion protection substances and / or other additives. This term also includes synthetic alternative substances as well as natural oils and fats.
  • VI viscosity index improvers
  • dispersants Contain greedings, wear inhibitors, antioxidants as well as corrosion protection substances and / or other additives.
  • This term also includes synthetic alternative substances as well as natural oils and fats.
  • an analysis device for the optical examination of fluids in particular of fuels and lubricants such as oils or fats, with an optical conductor arranged between a light source and a light sensor, the optical conductor being at least partially in contact with the fluid;
  • an analysis method for the optical examination of fluids in particular fuels and lubricants such as oils or fats, which has the following steps: emitting light rays from a light source, forwarding the emitted light rays through an optical conductor, recording the light rays from a light sensor, and evaluating the rays detected by the light sensor, the optical conductor being at least partially brought into contact with the fluid.
  • the degree of wear of fluids can be determined by spectrally detecting the change in the optical properties of the fluid, in particular its absorption behavior, due to its use. Because of the possible The method according to the invention is superior to the conventional methods in terms of selectivity and sensitivity, since it can also be carried out spectroscopically without reagent while the fluid is in use.
  • ATR Attenuated Total Reflection
  • the refractive index in the light guide in relation to the refractive index in the sample
  • the angle of reflection of the light at the interface must be chosen so that total reflection of the light takes place.
  • an evascent wave penetrates the neighboring medium (the sample).
  • An absorption that occurs leads to a weakening of the intensity of the light transported in the light guide. This weakening of light can be evaluated depending on the wavelength in order to obtain information about the composition and the condition of the sample from the spectrum.
  • an ATR fiber coated with a polymer, through which infrared radiation is guided is preferably used.
  • the components of the engine oil that are characteristic for the assessment of the oil condition can diffuse and come into contact with the fiber, whereas remaining oil components such as metal parts, soot particles etc. can be retained.
  • a possible proportion of water and / or a possible proportion of fuel in the engine oil is spectroscopically accessible, a detected proportion of water and / or fuel allowing important conclusions to be drawn about the engine oil quality.
  • the device according to the invention thereby enables a particularly high selectivity of the measurement, which also has a positive effect on its reliability and accuracy.
  • 1 is a schematic representation of a coated fiber waveguide
  • Fig. 3 is a schematic view of the analysis device according to the invention in measuring operation.
  • an analysis device 1 comprises a light source 2, which is preferably designed as an infrared radiation source.
  • a light source 2 which is preferably designed as an infrared radiation source.
  • an incandescent lamp is used which is selected for emissions in the desired wavelength range.
  • An amplitude modulator 5, which is also referred to as a chopper, is arranged immediately in front of it, the amplitude modulator 5 having a fixed frequency, the so-called chopper frequency, and modulating an amplitude of a radiation emitted by the incandescent lamp.
  • the amplitude modulator 5 can be designed as an impeller chopper.
  • the selection also only take place before the radiation penetrates into an optical conductor 4 onto which the selection device has been impressed.
  • a collimator 6 Before the rays emitted by the incandescent lamp enter the optical conductor 4, they pass through a collimator 6 by being parallelized.
  • the beams then pass through a filter device 7.
  • This can be designed, for example, as a wheel-shaped filter device, in which various bandpass filters are accommodated, which can be placed alternately in the beam path, in order to enable the fluid to be examined for different components or features.
  • the beams emitted by the light source 2 After passing through the filter device 7, the beams emitted by the light source 2 are bundled and focused on a first end face or fiber facet of the optical conductor 4.
  • the optical conductor which is at least partially in contact with the measuring fluid 8 on its outside, is traversed by the rays up to its second fiber facet.
  • the radiation emerging from the second fiber facet of the optical conductor 4 is imaged on the radiation receiver, the light sensor 3.
  • the light sensor 3 can be designed as an infrared-sensitive pyroelectric detector or as a thermopile.
  • the analysis device 1 is preferably constructed or arranged as shown in FIG. 3.
  • the entire optics and electronics are located in a separate housing 14.
  • the optical conductor 4 emerges from the housing and is at least partially immersed in the fluid 8 to be examined, for example an engine oil, before it re-enters the housing 14.
  • a protective cylinder or protective jacket 12 surrounds the optical conductor 4, the fluid 8 being able to penetrate through the openings 13 formed in the protective jacket 12 and coming into contact with the optical conductor 4.
  • the optical conductor is preferably U-shaped or V-shaped, with a measuring section at its curved or pointed end 10 is provided.
  • the housing 14 is preferably arranged at the highest point from which the optical conductor 4 extends downward, so that the measuring section 10 lies at the lowest point of the analysis device, as shown in FIG. 3.
  • the second fiber facet which emits the light signal or the light beams to the light sensor 3, is arranged within the housing 14 at approximately the same height as the first fiber facet of the optical conductor 4.
  • the incoming radiation power is detected by the light sensor 3 and converted into a measurement signal which can be further processed by a downstream measuring electronics for modulation and signal processing.,.
  • the optical conductor 4 is described in more detail below with reference to FIG. 1.
  • the optical conductor 4 is preferably designed as a coated phase waveguide.
  • an ATR fiber coated with a polymer can be used.
  • the coating is matched to the properties of the fluid to be measured.
  • the fiber waveguide is provided with a thin layer 9 of a correspondingly selected polymer on its outer surface, which is surrounded by the fluid 8 to be analyzed.
  • the layer thickness is to be chosen so that the evanescent field does not extend into the surrounding fluid 8.
  • the layer thickness should be chosen to be as small as possible, since this is the only way to enable a sufficiently rapid enrichment process in which the fluid 8 can diffuse through the coating 9 to the ATR fiber.
  • the decisive factor is the choice of a suitable polymer which, in contrast to previous water analysis, only enriches special components of the fluid to be measured, in particular the lubricant such as an oil or grease.
  • a particularly suitable polymer for this purpose is polyurethane and / or modified polyurethanes, for example those in which the OH component is replaced by an NH 2 component.
  • polyurethane and / or modified polyurethanes for example those in which the OH component is replaced by an NH 2 component.
  • the adaptation to the fluid 8 to be examined or the analytes contained therein, which should penetrate through the polymer layer to the fiber waveguides, takes place by the layer being formed together with this analyte becomes.
  • this is done by mixing an engine oil with the corresponding layer patterns, in particular a manomer or prepolymer.
  • the layer composition should be chosen such that the analyte as well as the entire fluid is inert to this layer so that it is neither degraded nor otherwise chemically changed.
  • any coating 9 can be used, into which a matrix with cavities and / or diffusion channels can be applied, which are adapted to a component of the fluid 8 to be determined.
  • the analyte of the fluid 8 to be examined can be stored in accordance with its concentration or can be removed again in the fluid when the analyte has a low concentration.
  • Such adapted coatings 9 can be produced as molecular embossing, as a result of which the coating can be manufactured industrially at low cost.
  • the structure of a coating 9 provided with cavities or diffusion channels described in this way preferably surrounds the optical conductor only in the area of the measuring section 10, which is in any case continuously surrounded by the fluid to be examined.
  • the remaining area of the optical conductor 4 outside the measuring section 10 is preferably provided with an impenetrable coating. It is also possible to arrange a plurality of measurement sections 10 with different molecular characteristics for different characteristic components of the fluid 8 to be examined next to one another on a plurality of measurement sections 10.
  • the coating 9 is preferably designed such that it enriches the respective analyte in the fluid 8 as high as possible, while at the same time it has a repellent effect on interfering components such as soot particles.
  • the absorption bands of the coating material preferably overlap with those of the fluid, for example motor oil, as little as possible.
  • the measuring section 10 of the optical conductor 4 is preferably designed as a strongly curved fiber in the form of a tip or an arc at the lowest point of the optical conductor, which results in a higher coupling-out of radiation and thus a higher sensitivity.
  • the spectral evaluation of several wavelengths ensures a reference formation during the measuring process, as shown in FIG. 1 with the aid of field distributions in different modes 16.
  • the optical conductor 4 is preferably surrounded by a heating device 11, as a result of which the optical conductor 4 can be cleaned again more easily, since heating contributes to the unification of the cavities and diffusion channels of the coating 9.
  • the mechanical structure of the analysis device 1 is preferably such that the optical conductor 4 can be replaced by a plug or screw connection or a similarly suitable mechanism.
  • the optical conductor 4 is at least partially surrounded by a protective cylinder or jacket 12, which prevents mechanical damage to the optical conductor outside the housing 14.
  • This protective cylinder 12 is preferably also removably connected to the optical conductor 4 or the housing 14 by means of a screw-plug, plug-in or other connection.
  • the inner wall of the protective cylinder 12 preferably has a screw-like surface in order to ensure an exchange of the motor oil or the fluid 8 to be examined in the vicinity of the optical conductor, in particular of the measuring section 10.
  • the optical conductor 4 or its measuring section 10 is preferably arranged at the lowest point of an oil pan or an oil sump or a corresponding container of another measuring liquid. The arrangement at the tip of an oil dipstick is also conceivable.
  • the processing electronics 15 can also be set such that they automatically recalibrate the analysis device as soon as it detects that the measuring fluid 8 has been refilled due to increased levels or changed measured values.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Engineering & Computer Science (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

La présente invention concerne un dispositif d"analyse et un procédé d"analyse permettant l"analyse optique de liquides, notamment de carburants et de lubrifiants, d"huile et/ou d"analytes à teneur en graisses tels que des huiles et des graisses. Ledit dispositif comprend un conducteur optique disposé entre une source de lumière et un détecteur de lumière, le conducteur optique étant au moins partiellement en contact avec le liquide. Les rayons émis par la source de lumière sont acheminés par le conducteur optique et détectés par le détecteur de lumière.
PCT/EP2001/010843 2000-09-19 2001-09-19 Dispositif et procede permettant l"analyse de liquides WO2002027302A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP01982323A EP1320744A2 (fr) 2000-09-19 2001-09-19 Dispositif et procede permettant l'analyse de liquides

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10046234.0 2000-09-19
DE10046234 2000-09-19

Publications (2)

Publication Number Publication Date
WO2002027302A2 true WO2002027302A2 (fr) 2002-04-04
WO2002027302A3 WO2002027302A3 (fr) 2002-08-22

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PCT/EP2001/010843 WO2002027302A2 (fr) 2000-09-19 2001-09-19 Dispositif et procede permettant l"analyse de liquides

Country Status (2)

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EP (1) EP1320744A2 (fr)
WO (1) WO2002027302A2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2454192A (en) * 2007-10-30 2009-05-06 Evanesco Ltd Fibre optic discrimination sensor
DE102013017377A1 (de) * 2013-10-21 2015-05-07 Schott Ag Messvorrichtung zur detektion der strahlung und/oder bestimmung der strahlungsleistung von mindestens einer quelle, die elektromagnetische strahlung emittiert, insbesondere für eine entkeimungs- oder desinfektionsvorrichtung

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5244813A (en) * 1991-01-25 1993-09-14 Trustees Of Tufts College Fiber optic sensor, apparatus, and methods for detecting an organic analyte in a fluid or vapor sample
DE19630181A1 (de) * 1996-07-26 1998-01-29 Inst Physikalische Hochtech Ev Kompakter Lichtleitfasersensor zur Detektion chemischer oder biochemischer Substanzen
WO1998032012A1 (fr) * 1997-01-15 1998-07-23 University Of Strathclyde Detecteur de furfuraldehyde et procede de fabrication dudit detecteur

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5244813A (en) * 1991-01-25 1993-09-14 Trustees Of Tufts College Fiber optic sensor, apparatus, and methods for detecting an organic analyte in a fluid or vapor sample
DE19630181A1 (de) * 1996-07-26 1998-01-29 Inst Physikalische Hochtech Ev Kompakter Lichtleitfasersensor zur Detektion chemischer oder biochemischer Substanzen
WO1998032012A1 (fr) * 1997-01-15 1998-07-23 University Of Strathclyde Detecteur de furfuraldehyde et procede de fabrication dudit detecteur

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2454192A (en) * 2007-10-30 2009-05-06 Evanesco Ltd Fibre optic discrimination sensor
DE102013017377A1 (de) * 2013-10-21 2015-05-07 Schott Ag Messvorrichtung zur detektion der strahlung und/oder bestimmung der strahlungsleistung von mindestens einer quelle, die elektromagnetische strahlung emittiert, insbesondere für eine entkeimungs- oder desinfektionsvorrichtung

Also Published As

Publication number Publication date
EP1320744A2 (fr) 2003-06-25
WO2002027302A3 (fr) 2002-08-22

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