WO2017194321A1 - Dispositif et procédé de détermination de la fraction molaire de composants gazeux d'un échantillon individuel d'un mélange gazeux à plusieurs composants - Google Patents

Dispositif et procédé de détermination de la fraction molaire de composants gazeux d'un échantillon individuel d'un mélange gazeux à plusieurs composants Download PDF

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Publication number
WO2017194321A1
WO2017194321A1 PCT/EP2017/060085 EP2017060085W WO2017194321A1 WO 2017194321 A1 WO2017194321 A1 WO 2017194321A1 EP 2017060085 W EP2017060085 W EP 2017060085W WO 2017194321 A1 WO2017194321 A1 WO 2017194321A1
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WO
WIPO (PCT)
Prior art keywords
gas
gas mixture
binary
capillary column
components
Prior art date
Application number
PCT/EP2017/060085
Other languages
German (de)
English (en)
Inventor
Silvan WIRTH
Patrick REITH
Christof Huber
Original Assignee
Truedyne Sensors 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 Truedyne Sensors AG filed Critical Truedyne Sensors AG
Publication of WO2017194321A1 publication Critical patent/WO2017194321A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02—Analysing fluids
    • G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/22—Details, e.g. general constructional or apparatus details
    • G01N29/222—Constructional or flow details for analysing fluids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G01N30/8603—Signal analysis with integration or differentiation
    • G01N30/8606—Integration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • G01N9/002—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis
    • G01N2009/006—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis vibrating tube, tuning fork
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/76—Acoustical detectors
    • G01N2030/765—Acoustical detectors for measuring mechanical vibrations
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/021—Gases
    • G01N2291/0215—Mixtures of three or more gases, e.g. air
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/028—Material parameters
    • G01N2291/02818—Density, viscosity

Definitions

  • the invention relates to an apparatus and a method for determining the molar fraction of gas components of a discrete sample of a multicomponent gas mixture.
  • MEMS sensors are micro-electromechanical systems used in metrology for
  • MEMS sensors are regularly used in common in semiconductor technology
  • Methods e.g. Etching processes, oxidation processes, implantation processes, bonding processes and / or coating processes, using single or multi-layer wafers, especially silicon-based wafers.
  • MEMS sensors which are used to determine a measured variable of a flowing fluid, in particular a liquid or a gas, have at least one measuring tube, the interior of which forms a conduit through which the fluid flows during the measuring operation.
  • different measuring principles are used to measure different measured quantities of flowing fluids.
  • An example is the vibronic density measurement.
  • at least one measuring tube through which the fluid flows in the measuring operation is used, which comprises at least one measuring tube section that can be excited to oscillate by means of an excitation device.
  • Measuring tube section excited to oscillations at a resonant frequency The resonance frequency is dependent on the density of the flowing fluid and can thus be used to determine the density.
  • the applicant produces and sells a vibronic MEMS density sensor under the name Nanomass.
  • Gas mixtures are determined.
  • One way to determine the mixing ratio of a gas mixture consisting of three or more gas components is not known.
  • the invention has the object to provide an apparatus and a method to determine the mixing ratio of a multi-component gas mixture.
  • the object is achieved by a device for determining the mole fraction of
  • Gas components of a discrete sample of a multicomponent gas mixture comprising:
  • a capillary column for separating the gas mixture into individual gas components, through which the gas mixture mixed with a carrier gas flows, wherein the
  • Carrier gas with the individual components of the gas mixture forms binary gas mixtures
  • a vibronic sensor for determining the density of the respective binary gas mixtures, wherein the vibronic sensor is connected to an outlet of the capillary column and wherein the binary gas mixtures flow through the vibronic sensor one after the other; and an evaluation unit for determining the mole fraction of each of
  • Gas components of the gas mixture based on the determined by the vibronic sensor density of the binary gas mixtures.
  • the great advantage of the device according to the invention is that by means of a vibronic sensor, the mole fraction of the individual gas components and thus the mixing ratio of the gas mixture are determined. So far, it was only possible to determine the mixing ratio of a binary gas mixture via a density measurement. The device according to the invention now also allows the determination of the mixing ratio of a
  • Gas mixture with three or more gas components Gas mixture with three or more gas components.
  • the capillary column separates the mixed with the carrier gas gas mixture such that at the outlet of the capillary column successively binary gas mixtures of the carrier gas with the respective gas component are present, which are passed directly into the vibronic sensor. It only has to be known from which individual gas components the gas mixture consists. Furthermore, the flow rate of the gas mixture mixed with the carrier gas must be constant in the capillary column and in the vibronic sensor.
  • the customer advantage lies in the fact that a customer can carry out an analysis of his multicomponent gas mixtures with respect to the mole fraction of the individual gas components without much extra effort.
  • the device according to the invention can be integrated in a simple way into the process, for example by means of a bypass. If the customer already has a density measurement application with a vibronic sensor in his system, then this application can be easily extended to the device according to the invention.
  • the vibronic sensor is a MEMS sensor, which at least one flow-through
  • a medium in this case a gas flows through or flows around the oscillatable component, its resonant frequency changes. On the basis of the changed resonant frequency, the density of the medium flowing through or flowing around, can be determined.
  • an oscillator is used as the vibration component, a preferred embodiment of the device according to the invention provides that the oscillator has the form of a vibrating cantilever beam or a swinging tuning fork.
  • the procedure is such that the length of the capillary column is configured such that the gas components of the gas mixture pass through the outlet of the capillary column one after the other and are completely separated.
  • the separation efficiency of the capillary column is adapted to the respective gas components.
  • Capillary column is designed in the form of a glass capillary.
  • Glass capillaries are well known in the art and exist in a variety of configurations, such as diameter and composition of stationary separation phase used.
  • the capillary column is designed in the form of a MEMS microchannel.
  • a particularly advantageous embodiment of the device according to the invention provides that the inner surface of the channel wall of the MEMS microchannel has a structured surface. As a result, the separation efficiency of the capillary column is further increased, which in turn reduces the required length of the capillary column.
  • the MEMS microchannel and the vibronic sensor are configured as a common MEMS chip system.
  • the device according to the invention can thus be offered as a complete system. It is conceivable that only connections exist for the inlet and outlet of the gas mixture, or of the gas mixture mixed with the carrier gas, as well as connections for the electrical contacting of the vibronic sensor, which must be connected to the customer's application.
  • the common MEMS chip system is arranged on a single die of a wafer.
  • a die in semiconductor and microsystems engineering is the designation of a single unhoused piece of wafer, which is usually obtained by sawing or breaking the finished wafer into rectangular pieces.
  • the common MEMS chip system can thereby be produced in a common manufacturing process. This will be the one
  • the MEMS components are made of a semiconductor material, in particular silicon.
  • semiconductor materials in particular silicon.
  • other materials such as ceramics or plastics may be used.
  • the object is achieved by a method for determining the molar fraction of gas components of a discrete sample of a multicomponent gas mixture, comprising:
  • a preferred embodiment of the inventive method provides that the carrier gas flows through the capillary column permanently and wherein the carrier gas is added after defined time intervals with the gas mixture. In this way, several independent measurements can be performed one after the other.
  • the defined time intervals are selected to be at least as large that, within the defined time intervals, the step of determining the density values of the binary
  • Gas mixtures and the step of calculating the mole fraction of each of the components in the gas mixture are performed.
  • the time intervals are further selected at least as long that the carrier gas is added to the gas mixture again only when the slowest separated gas component has left the capillary column via the outlet.
  • the proportion of the respective component in relation to the inert carrier gas in the binary gas mixtures is determined on the basis of the integrals.
  • An advantageous embodiment of the method according to the invention provides that the capillary column is heated to a defined temperature.
  • the separation efficiency of the capillary column increases with increasing temperature. By heating the capillary column to a defined temperature, therefore, the required length of the capillary column is reduced.
  • the device according to the invention can thus be dimensioned even more space-saving.
  • Fig. 1 A first variant of an embodiment of the device according to the invention
  • FIG. 2 shows a second variant of an embodiment of the device according to the invention
  • Fig. 3 an example of a measurement result for explaining the operation of the device according to the invention.
  • the device basically consists of two components, a capillary column 2 and a vibronic sensor 3. These components 2, 3 are connected to one another such that the outlet of the capillary column 2 is leak-free connected to the inlet of the vibronic sensor.
  • the capillary column 2 in the embodiment shown in FIG. 1 is a
  • Glass capillary This has a diameter of less than a millimeter and is at the
  • composition of the stationary separation phase can vary depending on the application.
  • the vibronic sensor 3 is in particular a MEMS sensor. However, it is also possible to choose a vibronic sensor 3 with larger dimensions.
  • the vibronic sensor 3 contains at least one oscillatable component, for example an oscillatable measuring tube 301, through which the gas mixture GM to be analyzed flows, or an oscillator, which is flowed around by the gas mixture GM to be analyzed.
  • the measuring principle is identical for both variants.
  • the vibronic sensor 3 shown in FIG. 1 is a MEMS density sensor 3, which has an oscillatable microchannel in the form of a measuring tube 301.
  • the MEMS sensor 3 is made of a semiconductor material, in particular silicon, using common
  • a carrier gas TG is introduced into the capillary column 2. This flows through the capillary column 2 and connected to the capillary column 2 MEMS density sensor 3 with a constant flow rate.
  • the carrier gas is, for example, hydrogen or an inert carrier gas TG such as helium, neon or argon.
  • a discrete sample of a multicomponent, in this example, three-component, gas mixture is added to the carrier gas at defined time intervals.
  • the carrier gas TG serves as a mobile phase and passes the discrete sample of the gas mixture GM through the capillary column.
  • a gas mixture GM it is also possible to use a discrete sample of a substance mixture with a different state of aggregation, but this must be brought to a high temperature before addition to the carrier gas TG and thereby vaporized.
  • the individual gas components of the gas mixture GM interact with the stationary phase of the capillary column 2.
  • this is done exclusively on the basis of different boiling points of the individual gas components, wherein mainly adsorption and desorption occurs at the stationary phase.
  • the stationary phase of the capillary column 2 is configured polar, so that certain molecular groups of the individual gas components are held more firmly on the stationary phase.
  • molecular interaction forces are caused by van der Waals bonds
  • the carrier gas TG is designed so that no interaction of the carrier gas with the stationary phase of
  • the capillary column 2 is designed such that there is a complete separation of the gas components of the gas mixture GM at the outlet of the capillary column 2.
  • the individual gas components are present after the separation as binary gas mixtures BG1, BG2, BG3, consisting of the respective gas component and the carrier gas TG.
  • the degree of separation depends primarily on the separation efficiency of the capillary column 2. This is defined by different parameters, mainly by the length of the
  • Capillary column 2 by the chemical composition of the stationary phase and by the prevailing in the capillary column 2 temperature.
  • the individual binary gas mixtures BG1, BG2, BG3 flow through the MEMS density sensor 3 one after the other.
  • the measuring tube 301 of the MEMS density sensor 3 oscillates, driven by electrodes, at its resonance frequency. Now flows through a medium, as in this case, a gas or a binary gas mixture BG1, BG2, BG3, the measuring tube 301, so its resonant frequency changes.
  • An evaluation unit 4 is electrically connected to the MEMS density sensor 3. On the one hand this supplies the electric current for operating the MEMS density sensor 3, on the other hand it measures the actual resonance frequency and detects a change of the resonance frequency. On the basis of the detected change in the resonance frequency, the density of the medium located in the measuring tube 301 is detected and recorded.
  • the separation of the individual gas components should be so great that never two binary gas mixtures BG1, BG2, BG3 simultaneously in the
  • the MEMS density sensor 3 are located.
  • the carrier gas TG flows through the MEMS density sensor 3 even if no additional gas component flows through the MEMS density sensor 3, whereby its density serves as a reference value.
  • the evaluation unit 4 determines in a final process step the mole fraction of each of the gas components of the gas mixture GM. The detailed explanation of the operation will be given below in the description of FIG. 3.
  • FIG. 2 shows a second variant of an embodiment of the device 1 according to the invention.
  • the structure differs from the variant shown in FIG. 1 in that no glass capillary but a MEMS microchannel 2a is used as the capillary column 2. This also contains a stationary phase on the inner surface of its channel wall. The diameter of the MEMS microchannel 2a is only a few micrometers.
  • the outlet of the MEMS microchannel 2a is fixedly connected to the inlet of the MEMS density sensor 3.
  • the MEMS microchannel 2a and the MEMS density sensor 3 form a common MEMS chip system 5.
  • This MEMS chip system 5 is preferably arranged on a single die of a wafer. A die is in the semiconductor and
  • Microsystem technology is the term for a single, unheated piece of a wafer, which is usually obtained by sawing or breaking the finished wafer into rectangular parts.
  • the common MEMS chip system 5 can thereby be produced in a common manufacturing process.
  • the mode of operation of the MEMS microchannel 2a as capillary column 2 corresponds to that of a glass capillary described in FIG. While the length of a glass capillary is often several meters, whereby space can be saved by winding the glass capillary (see FIG. 1), the maximum length of the MEMS microchannel 2a is limited by the dimensions of the common MEMS chip system 5. In order nevertheless to achieve the desired separation efficiency, the surface of the MEMS microchannel 2a or the surface of the stationary phase is structured, in particular
  • the effective surface of the stationary phase thereby increases drastically, whereby the interactions of the individual gas components of the gas mixture GM increase with the stationary phase. In this way, the length of the MEMS microchannel 2a can be reduced.
  • Fig. 3 shows an example of a measurement result for explaining the operation of the
  • the capillary column 2 separates the gas mixture GM in such a way that the individual gas components in binary gas mixtures BG1, BG2, BG3 flow through the vibronic sensor 3 one after the other.
  • the results of the vibronic sensor are explained below:
  • the measurement is started. At this time, there is only air in the vibronic sensor 3.
  • the measuring tube 301 of the vibronic sensor oscillates at the resonant frequency f0.
  • the evaluation unit determines the density from this resonant frequency
  • the carrier gas TG flows through the measuring tube 301 of the vibronic sensor 3. As a result, its resonance frequency changes.
  • the evaluation unit determines the density p T G for the carrier gas TG, which represents the reference density.
  • the first gas component forms a binary gas mixture BG 1 with the carrier gas TG.
  • the density p B Gi now determined by the evaluation unit 4 represents the density of the binary gas mixture BG1.
  • the molar fraction of the first component of the binary gas mixture at a time t can be calculated using the special gas equation: p (t) ⁇ Z mix ⁇ R - T
  • ⁇ , ( ⁇ ) denotes the mole fraction of the respective gas component in the i-th binary
  • C denotes a correction constant.
  • the density PBGI of the first binary gas mixture BG1 is determined.
  • the dashed area of p B Gi in Fig. 3 represents the integral of the measured density p B Gi in the period t2 to t3.
  • Xi is determined by the above-mentioned method.
  • the first gas component of the gas mixture GM has completely flowed through the measuring tube 301 of the vibronic sensor 3. As shown in FIG. 3, only the carrier gas TG flows through the measuring tube 301.
  • the second flows through in addition to the carrier gas TG
  • the second gas component forms a binary gas mixture BG2 with the carrier gas TG.
  • the density p B G2 of the second binary gas mixture BG2 is determined.
  • the dashed area of p B G2 in FIG. 3 represents the integral of the measured density p B Gi in the period t4 to t5.
  • X 2 is determined by the method described above.
  • the second gas component of the gas mixture GM has completely flowed through the measuring tube 301 of the vibronic sensor 3. As shown in FIG. 3, only the carrier gas TG flows through the measuring tube 301.
  • the third gas component forms a binary gas mixture BG3 with the carrier gas TG. Between times t6 and t7, the density p B G3 of the third binary gas mixture BG3 is determined.
  • the dashed area of p BG 3 in Fig. 3 represents the integral of the measured density p B G3 in the period t6 to t7.
  • X 3 is determined by the above-mentioned method.
  • the flow rate is constant. If the amount of the discrete sample of the multicomponent gas mixture is also known, X, can be determined directly, since the correction constant C results from the sample quantity at a constant flow rate and is directly included in the calculation of the integrals. The following applies:
  • Correction constant C can be calculated.
  • the constant C is calculated: As a result, the calculated X, 'to X, can be corrected, so that here too the sum of all X, 1 results.
  • the third gas component of the gas mixture GM has completely flowed through the measuring tube 301 of the vibronic sensor 3. As shown in FIG. 3, only the carrier gas TG now flows through the measuring tube 301. From this point on, it can now be initiated that a new discrete sample of the gas mixture GM is added to the carrier gas TG, with which the measurement can proceed again with this new discrete sample.
  • the device according to the invention and the method according to the invention are not limited to the above-mentioned embodiments and are applicable to any vibronic sensors which measure the density of a substance.

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Abstract

L'invention concerne un dispositif (1) et un procédé de détermination de la fraction molaire de composants gazeux d'un échantillon individuel d'un mélange gazeux à plusieurs composants (GM), le dispositif comportant : - une colonne capillaire (2) pour séparer le mélange gazeux (GM) en composants gazeux individuels, laquelle est traversée par le mélange gazeux (GM) déplacé par un gaz porteur (TG), le gaz porteur (TG) formant des mélanges gazeux binaires (BG1, BG2, BG3) avec les composants individuels du mélange gazeux (GM), - un capteur vibronique (3) servant à déterminer la densité des mélanges gazeux binaires (BG1, BG2, BG3) respectifs, le capteur vibronique (3) étant relié à une sortie de la colonne capillaire (2) et les mélanges gazeux binaires (BG1, BG2, BG3) traversant l'un après l'autre le capteur vibronique (3) ; et – une unité d'évaluation (4) servant à déterminer la fraction molaire de chacun des composants gazeux (BG1, BG2, BG3) du mélange gazeux (GM) à l'aide de la densité, déterminée par le capteur vibronique (3), des mélanges gazeux binaires (BG1, BG2, BG3).
PCT/EP2017/060085 2016-05-13 2017-04-27 Dispositif et procédé de détermination de la fraction molaire de composants gazeux d'un échantillon individuel d'un mélange gazeux à plusieurs composants WO2017194321A1 (fr)

Applications Claiming Priority (2)

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DE102016108964.8A DE102016108964B4 (de) 2016-05-13 2016-05-13 Vorrichtung und Verfahren zur Bestimmung des Stoffmengenanteils von Gaskomponenten einer diskreten Probe eines mehrkomponentigen Gasgemischs
DE102016108964.8 2016-05-13

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WO2014072503A1 (fr) * 2012-11-09 2014-05-15 Dsm Ip Assets B.V. Procédé, dispositif et système d'analyse d'une solution
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