WO2017207282A1 - Dispositif pour réaliser la spectroscopie d'un échantillon en réflexion totale atténuée - Google Patents

Dispositif pour réaliser la spectroscopie d'un échantillon en réflexion totale atténuée Download PDF

Info

Publication number
WO2017207282A1
WO2017207282A1 PCT/EP2017/061907 EP2017061907W WO2017207282A1 WO 2017207282 A1 WO2017207282 A1 WO 2017207282A1 EP 2017061907 W EP2017061907 W EP 2017061907W WO 2017207282 A1 WO2017207282 A1 WO 2017207282A1
Authority
WO
WIPO (PCT)
Prior art keywords
reflection
sample
reflection element
light
spectroscopy
Prior art date
Application number
PCT/EP2017/061907
Other languages
German (de)
English (en)
Inventor
Alexander Michael Gigler
Anja Niedermayr
Remigiusz Pastusiak
Tobias Paust
Matthias Schreiter
Evamaria STÜTZ
Original Assignee
Siemens Aktiengesellschaft
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 Siemens Aktiengesellschaft filed Critical Siemens Aktiengesellschaft
Publication of WO2017207282A1 publication Critical patent/WO2017207282A1/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
    • G01N21/17—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
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/06—Illumination; Optics
    • G01N2201/063—Illuminating optical parts
    • G01N2201/0634—Diffuse illumination
    • 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
    • G01N2201/0636—Reflectors
    • 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
    • G01N2201/064—Stray light conditioning

Definitions

  • the invention relates to a device according to the preamble of claim 1.
  • a known method for near-surface spectroscopy egg ner sample is spectroscopy in attenuated Totalrefle ⁇ xion (abbreviated ATR spectroscopy; English attenuated total.
  • Attenuated Totalrefle- is utilized xion a beam of light at a boundary surface of a Refle ⁇ xions institutes (ATR crystal) for spectroscopy of the sample.
  • the above condition can not be met by the presence of the sample, so that the light beam or the light at least partially emerges from the reflective element, and no longer reaches the detector.
  • the light at the detector is thus attenuated.
  • the actual measurement of the sample takes place by means of an evanescent coupling of the light beam (evanescent wave) into the sample during its total reflection at the interface. If the named evanescent wave hits an absorbing material (sample), the proportion of the detected light will decrease due to the material-specific excitation of molecular vibrations. Since the absorption and the ratio of the two indices of refraction n 2 and of the frequency As a function of the wavelength, a spectroscopy of the sample can be carried out.
  • ATR spectroscopy takes place in a wavelength range that lies in the mid-infrared spectral range.
  • an infrared source is used, example ⁇
  • thermal emitters heat radiators not collimated their electromag ⁇ netic spectrum give to their environment. This reduces the Signal to Noise Ratio (SNR). This is because the light beams of the non-collimated light source pass from the light source to the detector at different angles. This problem is solved by the prior art
  • Collimator optics at least partially solved by a large portion of the light ⁇ ⁇ outgoing light rays is collimated. Only after their collimation will the
  • Collimator optics a high adjustment time and are also associated with high costs.
  • lasers can be used as light sources, although in this case the collimator optics can be dispensed with, but the costs for the construction increase significantly.
  • Collimator optics must therefore be accepted according to the prior art, a poorer signal-to-noise ratio ⁇ the. If necessary, a slightly improved signal-to-noise ratio can be obtained by means of downstream signal processing.
  • the inventive apparatus for spectroscopy of a sample in attenuated total reflection comprises a reflection element with a first side facing the sample and a second side facing away from the sample, the first side surface for guiding a provided for the spectroscopy of the Pro ⁇ be light beam via total internal reflection is seen.
  • the second side surface has a plurality of spaced-apart coated reflection regions, which are designed to reflect the light beam.
  • the reflective element is also referred to as ATR
  • the spectroscopy of the sample in attenuated total reflection is abbreviated to ATR spectroscopy.
  • the light beam is regarded as a descriptive model representation of a real spatially extended light beam known to the person skilled in the art.
  • the light beam can be generated by means of a light source.
  • the light emitted by the light source is not collimated.
  • the light beam provided for the ATR spectroscopy is totally reflected on the first side surface facing the sample.
  • the second side facing away from the sample does not undergo total internal reflection according to the invention
  • the Reflexionsbe- according to the invention are rich arranged spaced from each other, that is, it exis ⁇ advantage a disposed between the reflection areas area on which the light beam is not totally reflected the reflection element, since the above-mentioned condition for his total reflection is not fulfilled. This is the case since, according to the device according to the invention, no means are provided for collimating the light emitted by the light source. However, a collimator optics or other optical components may be provided, but are not mandatory according to the invention.
  • the possible beam paths of the light beam from the light source through the reflection element are set to a detector provided for the spectroscopy.
  • preferred beam paths of the light beam are selected. If a light beam deviates from one of the preferred beam paths, it emerges from the reflection element and / or does not reach the detector. As a result, the light beams, which have a non-preferred beam path, no longer affect the measurement signal of the detector. This is the case, therefore, since typically only light rays to reach De ⁇ Tektor that were re- flected by each of the reflection regions, and consequently have a preferred meaning in this light path.
  • an effective spatial filter and / or angle filter is thus realized, which is realized without the use of further optical components, such as, for example, collimators. If the angle required for the detection of the light beam is known, then the arrangement of the reflection areas, that is, for example, their size, width, and the dimension of their mutual distance can be determined.
  • a further advantage of the inventive device that diffuse or non-collimated light sources may be used as a spatial filter and / or angular filter is formed by means of the reflection element and to ⁇ spaced apart coated reflecting areas which selectively only light beams having preferred optical paths to the detector of the ATR Spectroscopy leads.
  • a preferred number of ATR reflections that is a Favor ⁇ te number of interactions between the light beam and the sample, allows.
  • N-1 or N + 1 ATR reflections can result.
  • N 1 give ATR reflections if the light beam is incident with respect to its direction of irradiation in the reflection element to a first of Reflection ⁇ ons Schemee and is thereby reflected to the first side surface of the reflective element, that is, to the sample.
  • the reflection member is formed as a prism and the light beam over the deck ⁇ surface (for example, the first side surface) or one of the side faces of the prism is coupled.
  • N + 1 ATR reflections may result when the light beam first strikes the first side surface with respect to its direction of incidence into the reflection element.
  • the reflection element is formed as a prism and the light beam over the base (for example, the second side surface) or one of the side surfaces of the prism is coupled.
  • the reflection areas are aperiodically arranged with respect to their gegensei ⁇ term distance.
  • This provides an advantageous arrangement of the reflection preparation ⁇ che, which leads to an improvement of the signal-to-noise ratio of the ATR spectroscopy.
  • an aperiodic arrangement of the reflection regions due to the typical geometries of known reflection elements is advantageous.
  • a periodic arrangement of the reflection areas can be provided.
  • the regions lying between the reflection regions are formed by the material of the reflection element or by a further coating, wherein the further coating has a refractive index which is substantially equal to the refractive index of the reflection element.
  • this ensures that the light rays which do not have the preferred number of ATR reflections, that is to say a ray path not selected by the reflection regions and not preferred, do not reach the detector. For example, these are guided out of the reflection element and leave it via the regions arranged between the reflection elements. This advantageously further improves the signal-to-noise ratio of ATR spectroscopy.
  • the regions lying between the reflection regions are formed by an antireflection coating.
  • the anti-reflective coating is particularly advantageous if the lying between the Ref ⁇ lexions Schemeen areas can not be formed by the material of the reflection element. In an advantageous development of the invention, the width of the reflection regions increases along the reflection element.
  • a light beam in the strict sense is a theoretical construct of geometric optics, since a light beam, that is, a plurality of light rays always emanates from the light source and enters the reflection element at different angles.
  • the width of the reflection areas can be filtered by the light beams without losing too much light for ATR spectroscopy. It is particularly advantageous is when the reflection element we ⁇ officialss five and a maximum of fifteen, in particular ten, Ref ⁇ lexions Suitee has.
  • the reflection element for example, ten Reflexionsbe- rich, so the light beam on the sample supplied ⁇ facing side surface is typically nine times totally reflected. This has been found to be particularly advantageous since sufficient information can be obtained from the sample without losing too much light due to the interaction of the light with the sample. Overall, characterized the signal-to-noise ratio of the ATR spectroscopy is further timiert ⁇ op. This is particularly advantageous if the reflection ⁇ onselement is designed as a prism and the light beam is coupled over the top surface or one of the side surface of the prism such that it first meets the first of the reflection elements.
  • the reflection element three, eight and a maximum of thirteen, in particular eight, Refle ⁇ xions Schemee has.
  • the reflection element is designed as a prism and the light beam is coupled in such a way over the base surface or one of the side surface of the prism that it first strikes the first side surface.
  • the reflection element is prism-shaped.
  • Reflection element formed as a rotational body with trapezoidal in cross-section or longitudinal section sections.
  • the rotational body may have a cavity in which the sample is arranged.
  • the formed as Rota ⁇ tion body reflection element then surrounds the sample at least partially. This improves the interaction of the light beam with the sample, which further optimizes ATR spectroscopy for signal-to-noise ratio.
  • the device comprises a light source, wherein the light source and the device are formed such that the light of the light source not collimated into the reflection element ⁇ occurs.
  • the ATR spectroscopy can be carried out by means of the non-collimated light source. This is advantageous because additional optical components for collimating the light of the light source, such as Lenses or collimators are not required. But these can be provided.
  • the light source is designed as an infrared light source.
  • This is of advantage as the responsible for the absorption of the light beam char- acteristic energy states of the sample are typically in infraro ⁇ spectral range. The energy states are associated with characteristic molecular vibrations within the sample.
  • the penetration depth of the light beam ⁇ reduced in the sample with increasing wavelength of the light beam so that the signal of the ATR spectroscopy is less intense with increas ⁇ mender wavelength.
  • the reflection element comprises at least one of the materials zinc sulfide, zinc selenide, germanium, silicon, silver chloride or diamond.
  • FIG. 1 a sectional view of a first device according to the invention
  • Figure 2 is a sectional view of a second device according to the invention.
  • the first device 1 according to the invention is shown schematically in specific ⁇ a sectional view. In this case, the cut takes place in accordance with a longitudinal direction of the device 1 according to the invention.
  • the inventive apparatus 1 comprises a Reflexionsele ⁇ element 2, which has a first side surface 21 and a second Be ⁇ ten Chemistry 22nd
  • the first side surface 21 faces the sample to be spectroscoped.
  • the second side surface 22 faces away from the sample to be spectroscoped.
  • the reflector ⁇ xionselement 2 is prism-shaped, wherein the first side surface 21 is formed as a top surface and the second side surface 22 as a base.
  • the base area of the spectroscopic specimen that is wider in relation to the top surface may face, so that the reflection element 2 in FIG. 1 would be rotated through 180 degrees.
  • the reflection element 2, the first side surface 21 as the base surface and the second side surface 22 is formed as a top surface of the prism-shaped Reflexi ⁇ onsiatas 2.
  • the apparatus 1 further comprises a non-collimated light source 8, for example an infrared light source, and ei ⁇ NEN detector 10. From the light source 8 is a plurality of light beams, which are symbolized by way of example by the beam paths 101, 102 and 103 from. On the second side surface 22 of the reflection element 2, a plurality of coated reflection regions 42 are provided.
  • the reflection elements 42 at a distance from each other. In particular, they always have the same Distance to each other. As a distance of the reflection elements in this case is the distance of their respective geometric
  • the area between two adjacent reflection areas 42 is formed by a further coating 6.
  • the further coating 6 has essentially the same refractive index as the reflection element 2.
  • the light beams 101, 102, 103 are under different
  • Angles are coupled into the reflection element 2, since the light of the light source is not collimated. Due to the dung OF INVENTION ⁇ provided in accordance with arrangement of the reflection regions 42, a preferred angle or a preferred range of angles is defined. Typically, only light ⁇ rays having an angle in the said preferred angular range, guided by the reflection element to the detector. For example, the light beam 101 has an angle in the preferred angular range mentioned. The further light beams 102 and 103 each have an angle which is not in the preferred angular range, so that they do not reach the detector. This is the case because the light beams 102, 103 do not strike all the reflection areas 2 because of their angle, but rather to one of the further coatings 6.
  • the light beam 101 has five ATR reflections (ATR bounces), the light beam 101 being reflected six times by means of the reflection regions 42.
  • the reflection regions 42 can be formed by means of a mirrored coating.
  • an angle filter is formed by the reflection regions 42, which allows the non-collimated light source 8 for the ATR spectroscopy of the sample to use.
  • the light rays having an angle in the preferred angular range, for example the light beam 101 also have an advantageous number of ATR reflections, for example nine.
  • the entire second side surface 22 of the reflection ⁇ element 2 typically mirrored, so that almost all entering the reflective element 2 of light beams, in particular, the light beams 102, 103, to the detector 10 are passed, so that it comes adversely to a reduction of the signal-to-noise ratio.
  • the device 1 according to the invention overcomes this disadvantage known from the prior art.
  • Figure 2 illustrates another embodiment of the ER- inventive device 1, i.e. the second inventive device 1.
  • Figure 2 shows in Wesentli ⁇ chen the same elements as already Figure 1, wherein the Refle ⁇ xionselement 2 is rotationally symmetrically formed as a hollow body.
  • this has two trapezoidal sections.
  • ⁇ In an interior of the hollow body to be spectroscoped sample 3 is arranged ⁇ .
  • the interior is arranged concentrically with the axial axis of the rotationally symmetrical hollow body and he ⁇ extends along said axial axis.
  • the sections of the reflection element 2 which are trapezoidal in the sectional view are formed by two regions which are opposite one another with respect to the axial axis.
  • the signal-to-noise ratio of the ATR spectroscopy is enhanced by the rotational symmetry of the Ref ⁇ lexions institutes 2, since the sample more than once by the Light beam 101 interacts with the sample 3 via total internal reflection.
  • a solid angle filter is formed by means of the hollow body, so that not, as shown in Figure 1, an angle is selectively preferred by the reflection regions 42, but a preferred solid angle. All light rays which have a solid angle in the aforementioned preferred solid angle range are guided by the light source 8 via the reflection element 2 to the detector 10. In this case, all these light beams interact with the sample 3, whereby the intensity of the measurement signal is increased. Overall, this improves the ATR spectroscopy of Sample 3. For further discussion, reference is made to FIG.

Landscapes

  • 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

L'invention concerne un dispositif (1) pour réaliser la spectroscopie d'un échantillon (3) en réflexion totale atténuée qui comprend un élément réfléchissant (2) avec des première et seconde surfaces latérales (21, 22) respectivement tournées vers et éloignées de l'échantillon (3), la première surface latérale (21) étant prévue pour guider un faisceau lumineux (101) prévu pour la spectroscopie de l'échantillon (3) par réflexion totale interne. Selon l'invention, la seconde surface latérale (22) présente une pluralité de zones réfléchissantes (42) revêtues et écartées les unes des autres conçues pour réfléchir le faisceau lumineux (101).
PCT/EP2017/061907 2016-05-30 2017-05-18 Dispositif pour réaliser la spectroscopie d'un échantillon en réflexion totale atténuée WO2017207282A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102016209287.1A DE102016209287A1 (de) 2016-05-30 2016-05-30 Vorrichtung zur Spektroskopie einer Probe in abgeschwächter Totalreflexion
DE102016209287.1 2016-05-30

Publications (1)

Publication Number Publication Date
WO2017207282A1 true WO2017207282A1 (fr) 2017-12-07

Family

ID=58794054

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2017/061907 WO2017207282A1 (fr) 2016-05-30 2017-05-18 Dispositif pour réaliser la spectroscopie d'un échantillon en réflexion totale atténuée

Country Status (2)

Country Link
DE (1) DE102016209287A1 (fr)
WO (1) WO2017207282A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000036458A1 (fr) * 1998-12-11 2000-06-22 Abraham Katzir Formage d'elements cristallins transparents par ecrouissage et leur utilisation dans des systemes infrarouges
WO2001053822A2 (fr) * 2000-01-21 2001-07-26 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Procede et dispositif pour la determination de parametres dependant de la temperature, tels que les parametres d'association/dissociation et/ou la constante d'equilibre de complexes constitues d'au moins deux composants
JP2005091306A (ja) * 2003-09-19 2005-04-07 Horiba Ltd 油分濃度測定方法および油分濃度測定装置
DE102008015065A1 (de) * 2008-03-19 2009-09-24 Endress + Hauser Conducta Gesellschaft für Mess- und Regeltechnik mbH + Co. KG ATR-Sonde
WO2015156777A1 (fr) * 2014-04-08 2015-10-15 Pandata Research Llc Système de mesure optique ayant un élément de réflexion interne intégré et un détecteur de réseau

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004047078A1 (de) * 2004-09-29 2006-04-13 Robert Bosch Gmbh ATR-Photometer und Photometerarray
DE102013211814A1 (de) * 2013-06-21 2014-12-24 Siemens Aktiengesellschaft Bildgebung durch abgeschwächte Totalreflexion (ATR)

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000036458A1 (fr) * 1998-12-11 2000-06-22 Abraham Katzir Formage d'elements cristallins transparents par ecrouissage et leur utilisation dans des systemes infrarouges
WO2001053822A2 (fr) * 2000-01-21 2001-07-26 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Procede et dispositif pour la determination de parametres dependant de la temperature, tels que les parametres d'association/dissociation et/ou la constante d'equilibre de complexes constitues d'au moins deux composants
JP2005091306A (ja) * 2003-09-19 2005-04-07 Horiba Ltd 油分濃度測定方法および油分濃度測定装置
DE102008015065A1 (de) * 2008-03-19 2009-09-24 Endress + Hauser Conducta Gesellschaft für Mess- und Regeltechnik mbH + Co. KG ATR-Sonde
WO2015156777A1 (fr) * 2014-04-08 2015-10-15 Pandata Research Llc Système de mesure optique ayant un élément de réflexion interne intégré et un détecteur de réseau

Also Published As

Publication number Publication date
DE102016209287A1 (de) 2017-11-30

Similar Documents

Publication Publication Date Title
EP2356432B1 (fr) Ensemble capteur
EP0344364B1 (fr) Dispositif de détéction
DE102015101847B4 (de) Strahlteiler und Anordnung zur Untersuchung einer mittels elektromagnetischer Strahlung anregbaren Probe
EP1845349A1 (fr) Unité d'analyse spectrale dotée d'un réseau de diffraction
EP1523669B1 (fr) Dispositif d'analyse spectrometrique infrarouge d'un milieu solide, liquide ou gazeux
DE4243144A1 (de) Objektiv für ein FT-Raman-Mikroskop
WO2017101895A2 (fr) Sonde de mesure transparente pour balayage de rayonnement
DE102016212088A1 (de) Vorrichtung zum Begrenzen eines Einfallswinkels für ein Spektrometer und Verfahren zum Betreiben einer solchen Vorrichtung
DE102013219830B4 (de) Optische Vorrichtung zur Reflexionsmessung unter diffuser Beleuchtung und Verfahren zum Optimieren einer solchen, sowie Verwendung der Vorrichtung
DE4030836A1 (de) Vorrichtung zur qualitativen und/oder quantitativen bestimmung der zusammensetzung einer zu analysierenden probe
WO2017207282A1 (fr) Dispositif pour réaliser la spectroscopie d'un échantillon en réflexion totale atténuée
WO2014023498A2 (fr) Système de mesure pour la détermination de caractéristiques de réflexion de matériaux de miroirs solaires et procédé de détermination de qualité d'un échantillon de matériau de miroir
EP2217912A2 (fr) Sonde atr
EP1124146B1 (fr) Spectromètre optique avec guide d'onde optique
DE10316514A1 (de) Vorrichtung zur IR-spektrometrischen Analyse eines festen, flüssigen oder gasförmigen Mediums
WO2018224068A1 (fr) Sonde de mesure pour l'analyse de rayons
EP0099494B1 (fr) Dispositif pour la mesure de la réflexion
DE4201024A1 (de) Tragbares spektralphotometer zur in situ untersuchung des absorptionsspektrums eines stoffes
EP1873572B1 (fr) Dispositif destiné à la transmission de signaux optiques
DE102018217731A1 (de) LiDAR-Vorrichtung
DE102019107963A1 (de) Messlichtquelle sowie Messanordnung zum Erfassen eines Reflexionsspektrums
DE102022110651B4 (de) Kompaktes optisches Spektrometer
DE102017115660A1 (de) Optisches System
DE102018114969B4 (de) Verfahren und Vorrichtung zur Einkopplung von Licht in einen Lichtleiter und Sensor
DE19713483B4 (de) Spektrometer

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17726232

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 17726232

Country of ref document: EP

Kind code of ref document: A1