EP3022545A1 - Dispositif à flux continu pour système de spectrométrie et procédé pour le faire fonctionner - Google Patents

Dispositif à flux continu pour système de spectrométrie et procédé pour le faire fonctionner

Info

Publication number
EP3022545A1
EP3022545A1 EP14781832.2A EP14781832A EP3022545A1 EP 3022545 A1 EP3022545 A1 EP 3022545A1 EP 14781832 A EP14781832 A EP 14781832A EP 3022545 A1 EP3022545 A1 EP 3022545A1
Authority
EP
European Patent Office
Prior art keywords
flow
liquid
distance
optical element
measuring gap
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Withdrawn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
EP14781832.2A
Other languages
German (de)
English (en)
Inventor
Gerit Ebelsberger
Artur Jan PASTUSIAK
Remigiusz Pastusiak
Kerstin Wiesner
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.)
Siemens AG
Original Assignee
Siemens AG
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 AG filed Critical Siemens AG
Publication of EP3022545A1 publication Critical patent/EP3022545A1/fr
Withdrawn legal-status Critical Current

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
    • G01N21/01—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
    • G01N21/11—Filling or emptying of 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
    • G01N21/17—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
    • G01N21/255—Details, e.g. use of specially adapted sources, lighting or optical systems
    • 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
    • G01N21/11—Filling or emptying of cuvettes
    • G01N2021/115—Washing; Purging
    • 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
    • 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
    • G01N2201/02—Mechanical
    • G01N2201/025—Mechanical control of operations
    • 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
    • G01N2201/068—Optics, miscellaneous

Definitions

  • the invention relates to a flow-through device for a spectrometer system according to the preamble of patent claim 1 and a method for operating such a flow-through device.
  • Spectroscopy is a nondestructive material analysis method that uses light, typically between 1 and 500,000 nm wavelength. Spectroscopy is used primarily for the quantitative determination of known substances, their identification, for process control and monitoring and quality assurance.
  • a spectroscopic measurement setup includes a spectrometer for separating and measuring the various light components and a measuring head for optical coupling to the sample. Depending on the measurement method, a light source is also required.
  • measurements of the ingredients or properties of liquid samples usually employ either immersion probes or flow cells.
  • a flow-through device for a spectrometer system has a first, to a spectrometer op- table couplable optical element and a second, to a
  • Light source couplable optical element which are arranged spaced from one another in the region of a measuring gap through which a liquid can flow, wherein in the region of this
  • Messspaltes emerging from the second optical element and in the first optical element reaching light beam is at least partially absorbable by the liquid.
  • a flow rate of the liquid through the measuring gap can be influenced by changing the distance between the two optical elements.
  • the distance of the optical elements can be changed both by moving one of the two or by moving both optical elements.
  • the distance of the two optical element is controllable.
  • the size of the measurement gap can be controlled during a measurement, so that a best light efficiency can be set from a spectroscopic point of view.
  • the flow-through device can in particular also be adapted to inhomogeneities in the sample substance.
  • the distance between the two optical elements can be controlled with a micrometer screw or hydraulically. This has the advantage that the distance can be set very accurately and thus the different Properties of different sample liquids in fine gradations can be well taken into account.
  • a control device is provided, with which the distance between the two optical elements can be automatically increased or reduced in dependence on a light intensity, which can be measured by a measuring device optically coupled to the first optical element.
  • a measuring device optically coupled to the first optical element.
  • a by-pass system is part of the flow-through device, by means of which a further liquid as a reference liquid can be introduced into the measuring gap.
  • a reference spectrum which is basically required for each position or each distance of the optical elements for the evaluation of data, does not have to be read from a database, but can be measured in each case in situ.
  • a new reference spectrum can be recorded for each new position of the optical elements, in which, after a change in the size of the measuring gap, firstly said reference liquid is examined.
  • the by-pass system is designed to automatically introduce a cleaning fluid during operation and then, in consequence, to introduce the reference fluid into the measurement gap.
  • the reference spectrum can be recorded particularly reliably, because it is ruled out that residues of other liquids falsify the reference spectrum.
  • the flow-through device is substantially tubular.
  • it may take the form of a capillary.
  • the flow-through device can easily be connected to existing superstructures and is easy to clean.
  • a pump or the like may possibly be dispensed with. It is here that an adaptation of the size of the measuring gap to sample properties is advantageous, since in this way the respective different properties of different samples with respect to the capillary effect can be taken into account.
  • At least one expandable membrane in particular a very extensible and / or deformable membrane, is arranged between the associated optical element and an inner wall region of the flow-through device.
  • the membrane deforms in a change in the distance between the two optical elements so that it forms a bottleneck with the optical elements, so the measuring gap.
  • the selection of the material from which the membrane is to be produced is free here except for the requirements of ductility and / or ductility and can be chosen to be process-specific, in particular as a polymer membrane or as a mixed-matrix membrane.
  • the material of the membrane is preferably selected so that it is able to withstand the liquids to be examined or individual components of these liquids, so in particular by this, as well as by any cleaning agents used, is not chemically attacked.
  • This has the advantage that with the membrane a possible collection of solid particles, as they occur in inhomogeneous liquids, can be prevented at the optical elements in the flow device.
  • the cleaning of the flow-through device, ie the flow cell, is also considerably simplified by the use of the membrane.
  • the membrane seals the system of leaks, on the other hand, it is so stretchable that at the maximum distance of the optical elements a strong
  • Measurement gap realized bottleneck in the liquid flow is reduced and the flow of the process liquids remains laminar in a wider range.
  • Also part of the invention is a method for operating such a flow device for a spectrometer system, wherein a flow rate of the liquid is influenced by the measuring gap by changing the distance of the two optical elements.
  • FIG. 1 shows a schematic representation of an exemplary
  • FIG. 2 shows a schematic representation of another exemplary flow-through device in an embodiment of the invention
  • FIG. 3 shows a schematic representation of an additional exemplary flow-through device in an embodiment of the invention.
  • FIG. 4 shows a schematic representation of the membrane shown in FIG.
  • FIG. 1 shows a flow device 1 is shown.
  • a liquid 8 flows along a plurality of wall regions 12 and through a measuring gap 6 which is arranged through two optical elements 2, 3 which are arranged at a distance 10 from one another.
  • swirling occurs in two regions 9 near the measuring gap.
  • the optical elements 2, 3 are movable here parallel to the drawing plane, so that they can be changed in their distance 10.
  • the size of the measuring gap 6 is variable, and the amount of liquid 8, which can flow in a predetermined time through the measuring gap 6 is thus changed by a change in the distance 10 of the two optical elements 2, 3.
  • the liquid 8 now flows through the measuring gap 6 and at least partially absorbs light which emerges from the second optical element 3. Thus, only a certain proportion of the light emerging from the second optical element 3, which has a reduced spectrum, enters the first optical element 2
  • Flow device 1 are used for another liquid 8, so in the measuring gap 6 at the set distance for the preceding liquid 8 may either be too much or too little light absorbed. If too much light is absorbed, that is to say if it is a substantially darker liquid, the distance 10 must be reduced so that it is still possible to draw conclusions about the properties of the liquid 8 from the light reaching the first optical element 2. If, however, it is a very fluid, largely transparent liquid 8, for example, the measuring gap 6 must be increased so that the amount of liquid 8 between the two optical elements 2, 3 is sufficient, for example, to produce a measurable absorption of light. Other properties, such as the viscosity of the liquid 8, can thus be taken into account by adjusting the measuring gap 6.
  • FIG. 2 shows a flow-through device 1 in which, very similar to the flow-through device 1 shown in FIG. 1, a liquid 8 flows between wall regions 12 and two optical elements 2, 3 through a measuring gap 6.
  • the two regions 9, in which Verwirbe- take place significantly smaller than in the example shown in FIG 1.
  • the membranes 11 are fastened between edges of the measuring gap 6 and inner edges of the wall regions 12 of the flow-through device 1.
  • the membranes 11 adapt to the changed geometry of the wall regions 12 and the two optical elements 2, 3 due to their flexibility.
  • the membrane 11 in the example shown, even less acute angles occur at the corner regions of the wall regions 12 and the optical elements 2, 3. This is the cause of the already mentioned advantageous reduction of the areas 9, in which the liquid 8 swirls.
  • FIG. 3 shows a flow-through device 1 in a built-in state in a spectrometer system.
  • Two displaceable cylinders 13 receive here the two Optikele- elements 2, 3 and form here a mechanical guide.
  • the distance 10 between the two optical elements 2, 3 is adjustable, for example via a micrometer screw.
  • a light source 5 for example a halogen lamp or an LED element
  • a light beam 7 passes first into the second optical element 3, then into the measuring gap 6, and finally via the first optical element 2 into a spectrometer 4.
  • a Liquid 8 are the spectral parts of the light beam 7 absorbed.
  • the liquid 8 is in the example shown via two tubes 16, which via the membrane 11 with the
  • Measuring gap 6 are connected, passed through the measuring gap 6. If an excessively high or too low brightness is detected in the spectrometer 4, the measuring gap 6 can be adjusted in the example shown by displacing the cylinders 13. If too much light enters the spectrometer 4, the measuring gap 6 will be increased, but if too little light enters the spectrometer 4, the measuring gap 6 will be reduced so as to ensure the best possible measurement result, ie for different sample substances.
  • the system can, for example, additionally be equipped with a by-pass system, which is set up in such a way that, after changing the distance 10 of the two optical elements 2, 3, it first automatically ensures that the measuring gap 6 is flushed with a cleaning fluid Follow a reference liquid to introduce into the measuring gap 6, so that the spectrometer 4 can be adjusted or calibrated based on the reference liquid for the now used distance 10. After the adjustment process, the liquid 8 to be analyzed is again introduced into the measuring gap 6 via the two tubes 16.
  • a fully automated analysis of a wide variety of substances can be carried out or, for example, carried out. also the process flow can be varied.
  • FIG. 4 shows a schematic representation of the membrane 11 used in the example shown in FIG. 3.
  • the two openings 15, which in the present case are the larger of the openings 14, 15, are intended to seal the flow-through device 1 in the region of the two optical elements 2, 3 with the associated cylinders 13.
  • the two smaller openings 14 accommodate two tubes 16 and thus seal the throughflow device 1 in the direction of the supply and discharge of the liquid 8 to be examined. Since the mem- ran 11 is highly elastic or highly flexible, it can simultaneously adapt to a changed geometry by moving the cylinder 13 with the optical elements 2, 3 and get their sealing function. In addition, edges that can be used to collect residues of the sample or other liquids and substances are avoided constructively by the round shapes used.

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)
  • Spectroscopy & Molecular Physics (AREA)
  • Optical Measuring Cells (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne un dispositif à flux continu (1), destiné à un système de spectrométrie, qui comprend un premier élément optique (2), couplable optiquement à un spectromètre (4), et un deuxième élément optique (3), couplable optiquement à une source de lumière (5), qui sont disposés espacés l'un de l'autre dans la zone d'une fente de mesure (6) dans laquelle un liquide (8) peut s'écouler et dans la zone de laquelle un faisceau lumineux (7) sortant du deuxième élément optique (3) et pénétrant dans le premier élément optique (2) peut être absorbé au moins en partie. En faisant varier la distance (10) entre les deux éléments optiques (2, 3), il est possible d'influer sur le débit du liquide (8) à travers la fente de mesure (6) afin de pouvoir utiliser le système de spectrométrie avec une pluralité d'échantillons différents. L'invention concerne également un procédé permettant de faire fonctionner un tel dispositif à flux continu (1).
EP14781832.2A 2013-09-27 2014-09-24 Dispositif à flux continu pour système de spectrométrie et procédé pour le faire fonctionner Withdrawn EP3022545A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201310219544 DE102013219544A1 (de) 2013-09-27 2013-09-27 Durchflusseinrichtung für ein Spektrometersystem und Verfahren zum Betreiben einer solchen
PCT/EP2014/070290 WO2015044157A1 (fr) 2013-09-27 2014-09-24 Dispositif à flux continu pour système de spectrométrie et procédé pour le faire fonctionner

Publications (1)

Publication Number Publication Date
EP3022545A1 true EP3022545A1 (fr) 2016-05-25

Family

ID=51688030

Family Applications (1)

Application Number Title Priority Date Filing Date
EP14781832.2A Withdrawn EP3022545A1 (fr) 2013-09-27 2014-09-24 Dispositif à flux continu pour système de spectrométrie et procédé pour le faire fonctionner

Country Status (7)

Country Link
US (1) US20160209321A1 (fr)
EP (1) EP3022545A1 (fr)
KR (1) KR20160065918A (fr)
CN (1) CN105556281A (fr)
DE (1) DE102013219544A1 (fr)
SG (1) SG11201601930QA (fr)
WO (1) WO2015044157A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110327996B (zh) * 2019-09-03 2019-12-24 中国科学院上海高等研究院 微流控芯片、微流控系统及红外微流控分析方法

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GB1054813A (en) * 1964-01-16 1967-01-11 Apparatus for the spectral examination of liquids
CN85200040U (zh) * 1985-04-01 1985-12-20 清华大学 池厚连续可调加温高压红外流动池
JPS61231435A (ja) * 1985-04-08 1986-10-15 Hitachi Ltd フロ−セル
ATE60133T1 (de) * 1987-07-22 1991-02-15 Ciba Geigy Ag Prozesskuevette.
US5351120A (en) * 1993-07-12 1994-09-27 American Air Liquide Spectroscopic cell design
DK173073B1 (da) * 1996-11-01 1999-12-20 Foss Electric As Fremgangsmåde og flowsystem til spektrometri og en kuvette til flowsystemet
JP3615438B2 (ja) * 1999-11-04 2005-02-02 住江織物株式会社 自動調色検定装置及び染液の自動調液システム
US6974938B1 (en) * 2000-03-08 2005-12-13 Tibotec Bvba Microscope having a stable autofocusing apparatus
US7027147B2 (en) * 2001-03-19 2006-04-11 E. I. Dupont De Nemours And Company Method and apparatus for measuring the color properties of fluids
US6762832B2 (en) * 2001-07-18 2004-07-13 Air Liquide America, L.P. Methods and systems for controlling the concentration of a component in a composition with absorption spectroscopy
ITMI20021192A1 (it) * 2002-05-31 2003-12-01 Loris Bellini S P A Macchina di tintura con controllo automatico in linea dell'esaurimento del bagno
DE102005052752A1 (de) * 2005-11-04 2007-05-10 Clondiag Chip Technologies Gmbh Vorrichtung und Verfahren zum Nachweis von molekularen Wechselwirkungen
US8303894B2 (en) * 2005-10-13 2012-11-06 Accuri Cytometers, Inc. Detection and fluidic system of a flow cytometer
FR2903775B1 (fr) * 2006-07-12 2009-01-16 Tethys Instr Soc Par Actions S Dispositif d'ecoulement d'un fluide et appareillage de mesure optique utilisant un tel dispositif.
US7593101B2 (en) * 2007-04-10 2009-09-22 Schlumberger Technology Corporation High-pressure cross-polar microscopy cells having adjustable fluid passage and methods of use
DE102009037240A1 (de) * 2009-08-12 2011-02-17 Siemens Aktiengesellschaft Verfahren und Vorrichtung zur Bestimmung chemischer und/oder physikalischer Eigenschaften von Betriebsstoffen in einer Maschinenanlage

Non-Patent Citations (1)

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Also Published As

Publication number Publication date
SG11201601930QA (en) 2016-04-28
DE102013219544A1 (de) 2015-04-02
WO2015044157A1 (fr) 2015-04-02
US20160209321A1 (en) 2016-07-21
CN105556281A (zh) 2016-05-04
KR20160065918A (ko) 2016-06-09

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