EP2745089A1 - Système de prélèvement de microéchantillons pour de petites quantités d'échantillons de fluide pour analyse en phase vapeur - Google Patents

Système de prélèvement de microéchantillons pour de petites quantités d'échantillons de fluide pour analyse en phase vapeur

Info

Publication number
EP2745089A1
EP2745089A1 EP12762542.4A EP12762542A EP2745089A1 EP 2745089 A1 EP2745089 A1 EP 2745089A1 EP 12762542 A EP12762542 A EP 12762542A EP 2745089 A1 EP2745089 A1 EP 2745089A1
Authority
EP
European Patent Office
Prior art keywords
micro
sampling system
block
sample
functional units
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Withdrawn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
EP12762542.4A
Other languages
German (de)
English (en)
Inventor
Károly Nagy
Bernd Schilling
Alexander Plum
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.)
Bayer AG
Original Assignee
Bayer Intellectual Property GmbH
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 Bayer Intellectual Property GmbH filed Critical Bayer Intellectual Property GmbH
Publication of EP2745089A1 publication Critical patent/EP2745089A1/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Withdrawn legal-status Critical Current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
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2205—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/12—Preparation by evaporation
    • G01N2030/126—Preparation by evaporation evaporating sample
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
    • Y10T436/2575—Volumetric liquid transfer

Definitions

  • Micro-sampling system for small quantities of fluid samples for analysis in the
  • the present invention relates to a micro sampler system for fluid samples for analysis in the vapor phase.
  • Fluids are liquids as well as gases or vapors.
  • the liquids are completely evaporated or vaporized and the sample transferred to the gas phase is homogeneously mixed before the actual analysis, for example in the mass spectrometer.
  • numerous devices are known, for example, from the patent literature. US 2010/122564 A I, CN 2667484, EP 1 174 703 A I, US 2009/107640 A I and J P 61 180136 disclose only some of these devices.
  • the small amount of sample is important not only because of the economical use of the fluid from which the sample is taken. Another reason is that the sample taken from a process could contain environmentally harmful, toxic or hazardous components, so that the sample must be appropriately disposed of after analysis. This involves costs that should be minimized in order to contribute to an economic and environmentally friendly analysis.
  • a fast reaction time is desirable since in production processes individual components are often detected via mass spectrometers and, based on the data, the regulation of dependent process parameters takes place. This is particularly important if production is to be optimized with regard to one or more components in order to avoid technical and economic disadvantages. For example, the production of unwanted by-products can be prevented and product quality increased at the same time, which in turn results in low production costs.
  • the requirements for a small amount of sample with simultaneously fast reaction time appear to be contradictory, since the sample has to be directed from the place of sampling to the evaporator and this distance can not be made arbitrarily short, inter alia because of the necessary connections and screw connections.
  • the lines can not be arbitrarily thin due to the threat of blockages. Conversely, direct introduction of a small sample into the evaporator would cause a long reaction time.
  • the line between the evaporator and meter must be heated to avoid condensation in the line.
  • the present invention is therefore a micro-sampling system according to claim 1 and advantageous embodiments according to the subclaims. Furthermore, the subject of the present invention is the use of the micro-sampling system according to the invention. Accordingly, the present invention relates to a microsampling system for vapor phase fluid samples having at least the following integrated functional units: a bypass block for delivering a targeted amount of the fluid sample to a microevaporation block, a microevaporation block for selectively vaporizing the fluid sample, a filter element for filtration the vaporized fluid sample, a pressure drop and discharge unit for selectively generating a pressure drop of the fluid sample vaporized in the microevaporation block and for discharging excess vapor, and at least one lid.
  • a bypass block for delivering a targeted amount of the fluid sample to a microevaporation block
  • a microevaporation block for selectively vaporizing the fluid sample
  • a filter element for filtration the vaporized fluid sample
  • a pressure drop and discharge unit for selectively
  • the term "functional units” is understood to mean the individual elements of the device that make up the entire micro-sampling system only when interacting.Therefore, the terms functional element or functional module are synonymous with the term “functional unit.”
  • the modular concept enables easy disassembly of the functional units and thus also the simple replacement of individual components or their cleaning or maintenance, the term “integrated functional units” being the compact one Understanding structure of the entire system, in which the individual functional units are arranged according to their function one behind the other and as such form a functional unit in which can be dispensed with long distances between the individual elements and thus superfluous lines, connections and connections. As a result, short reaction times can be guaranteed.
  • the integration of the functional units also ensures that the individual modules have the same operating temperature during operation and thus no condensation or fractionation of the sample threatens. An additional temperature control by further heating elements on individual functional units, however, can be additionally provided.
  • the various functional units enable the handling and preparation of very small sample quantities.
  • the device is designed so that the individual functional units can be easily exposed and not only chemically, but also mechanically cleaned, or replaced. Through the microstructures of the functional elements and the predetermined flow paths of the sample, the unwanted fractionation of a complex sample matrix is eliminated and a constant homogeneous vapor stream is prepared for analysis.
  • fluid samples is understood to mean both liquid and gaseous samples, but preferably liquid samples, but the micro-sampling system can also be used for gases.
  • the micro-sampling system For fast and continuous sampling of fluids and for delivering a targeted amount of the fluid sample to the microevaporator, the micro-sampling system includes a bypass block.
  • the mass flow can be any size. From this mass flow, the desired amount of sample in the direction of micro-evaporator is derived.
  • an exchangeable orifice is arranged between the bypass block and the micro-evaporator block.
  • the orifice can be adapted to the different media of different viscosity and density and is located directly at the entrance of the micro-evaporator. This very short path can be overcome quickly by the mass flow of the sample.
  • the high mass flow in the bypass and the short path to the micro-evaporator ensure a short reaction time.
  • the length of the line to the bypass is therefore not critical, so that possibly other devices, such.
  • pressure regulators, flow controllers or sensors can be connected to realize constant operating parameters.
  • the amount of fluid sample to be evaporated can be controlled by the pressure in the bypass.
  • the bypass block is designed for a pressure in the bypass of 1, 1 to 1, 8 bar, preferably from 1, 2 to 1, 6 bar, more preferably from 1, 3 to 1, 4 bar.
  • the pressure becomes specific to the fluid and the desired amount of sample customized. Accordingly, different pressure ranges than the aforementioned are possible depending on the sample fluid.
  • the system works preferably with slight overpressure in the bypass, with 2 bar usually not be exceeded.
  • the functional units are designed for fluid samples with flow rates of 20 ⁇ 1 / min to 5 ml min in the bypass block, wherein the sampling takes place continuously.
  • flow rates 20 ⁇ 1 / min to 5 ml min in the bypass block, wherein the sampling takes place continuously.
  • the micro-evaporator block of the micro-sampling system comprises an evaporation chamber having an inlet and an outlet side, a microstructured drain plate covering the evaporation chamber at the outlet side, heaters for heating elements and a temp rs ensor and in which a sample size ⁇ 1 ml min, preferably ⁇ 100 ⁇ ! minute more preferably ⁇ 10 ⁇ / min is continuously converted into homogeneous steam. The steam is then ready for analytical purposes.
  • micro-sampling system for a reaction time of 3 s, preferably 2 s, more preferably 1 s designed. This is the transit time of the mass flow from the bypass input to the capillary inlet into the screw connection to the analyzer.
  • micro-sampling system s ind the Bypassb lock arranged connections for the fluid leading capillaries. Via these capillaries, the connection of the microsyringe system with the production unit to be monitored is established.
  • the functional units are stacked on top of each other.
  • the stacked functional units are fixed with screws. This results in a compact design of the micro-sampling system, in which the individual func t io nse i nhei th lined up close to each other s i nd and unnecessary lines or connectors can be avoided.
  • the functional units are arranged around the microstructure block as block heights or integrated into the micro-evaporator block as individual modules. In this case, all functional units remain separately disassembled, so that individual functional units can be easily removed, maintained, replaced or cleaned, without that the entire system must be taken apart.
  • the central functional unit is the micro-evaporator, which is preferably made of a stainless steel block. Between the evaporator block embedded in the stainless steel block and the bypass block, only the diaphragm is arranged, so that the path between these two functional units is reduced to a minimum.
  • the amount of liquid sample introduced into the evaporator is evaporated in a very short time. For a liquid sample, the resulting vapor volume is significantly larger than the initial volume of the fluid sample. This causes a very fast vapor flow at the outlet of the evaporator chamber as well as in the other functional units and connected lines.
  • the exit of the vaporization chamber is covered with a microstructured plate having slots, holes, pores, or other shaped microscale openings.
  • the microstructured plate has the function of preventing a short circuit between the input of the evaporation chamber and the input of the next functional unit.
  • the microstructures mix the vapor components in order to counteract fractionation into the individual components and to stabilize the steam temperature b to the next functional unit.
  • the micro-evaporator can be heated.
  • heating elements and associated temperature sensors are connected.
  • a control circuit ensures the necessary temperature stability.
  • the temperature of the vaporized sample is kept constant above the boiling point of the exit fluid.
  • the filter means for biasing the vaporized fluid sample out of the micro-evaporator cavity is arranged in a filter plate.
  • the filter is preferably made of stainless steel and depending on the vaporized sample pore diameter of ⁇ 200 ⁇ , preferably ⁇ 20 ⁇ m, more preferably ⁇ 2 lim.
  • the filter plate is placed on the micro-evaporator base, so that the filter plate forms a unit with the micro-evaporator core.
  • the tempera ture applied to the microcontrollable lock is also transferred to the filter on the printer.
  • the filter is adapted to the fluid and easy to replace or clean. Analyzers generally need very low gas or vapor streams. The vapor surplus must be drained off and condensed. For this, the vaporized fluid sample is passed over a pressure drop and exhaust inlet.
  • the pressure-drop and discharge unit has a functional element for the Pressure drop and a drain line on.
  • the drain unit has the function of keeping the outlet for the drain at a high temperature, ie above the boiling point of the fluid, to avoid condensation in the drain line. Even small amounts of condensate cause a slight, not measurable pressure increase in the system, which leads to unwanted noise in the measuring signal, even if the condensate does not block the line.
  • the connection for the drainage pipe must be aligned so that the condensate can flow off easily. Therefore, a vertical or slightly inclined orientation, but in any case ⁇ 90 ° according to the angle between the vertical and the actual discharge line, is preferred.
  • the drain connection is provided with a discharge line, which is dimensioned so that the liquid droplets that condense in its cold part, the line cross-section, can not sleep and drain easily by the grav itations force. The connection of the drain line is heated.
  • the operating element for the pressure drop and the discharge line is arranged on in a separate Plattenelcment.
  • this functional unit can also be easily disassembled, replaced and cleaned separately.
  • the drainage line is connected via a connection to the compressor core.
  • the vacuum of the connected analyzer is conducted to the pressure drop unit, where a suitable functional element provides for the pressure drop.
  • This functional element is preferably a thin capillary, nozzle or filter and dimensioned accordingly, i. The length and diameter of the capillary, or the pore size and thickness of the filter is chosen accordingly. Since the temperature of the discharge pressure drop unit is at the working temperature of the evaporator and vacuum is present after the discharge pressure drop to the analyzer, there is no condensation in the line to the analyzer, which in turn operates at room temperature. A screw for the capillary to the analyzer is also provided. If the analysis is not performed under vacuum, the line to the analyzer must also be heated.
  • the ikro sampling system is completed with the lid.
  • the cover has a connection possibility for a connection element for connection to the capillary to the analysis unit.
  • the functional units of the device are held together with screws passing through the lid. Seals may be present between the units.
  • the micro-sampling system can additionally be covered with insulation from the outside.
  • the functional units are made of corrosion-resistant metal len. Depending on the location and the fluids to be examined stainless steel is used for this purpose. However, individual functional units can also consist of suitable plastics.
  • the bypass block and the cover are made of chemically inert and temperature-resistant plastic.
  • the present invention relates to the use of the micro-sampling system for continuously sampling small amounts of fluid in combination with or as an integral part of a vapor phase low fluid volume analyzer.
  • analyzers mass spectrometers are preferably used.
  • the sample fluid used is water.
  • the working temperature is 180 ° C
  • the opening of the aperture has a diameter of 150 ⁇
  • the pressure in the bypass is 1, 4 bar.
  • the reaction time (T90 time) of the micro-sampling system is about 3 s. This is the transit time of the mass flow from the bypass input to the capillary inlet into the screw connection to the analyzer. This reaction time is achieved with a liquid flow of about 100 ⁇ I min in the direction of micro-evaporator.
  • the volume flow in the bypass can be set independently of this value and varies in the range from approx. 20 ⁇ / min to 2 ml / min.
  • FIG. 1 Schematic representation of the stacked functional units of the micro-sampling system according to the invention
  • FIG. 2 Schematic representation of the micro evaporator block in Stapeiholz au
  • FIG. 3 Schematic representation of the block-built functional units of the micro-sampling system according to the invention
  • FIG. 4 Schematic representation of the micro evaporator block in block construction
  • Figure 1 shows the individual functional units of the micro-sampling system in the exploded state.
  • the device has a plurality of functional units, which are stacked on each other and are pressed together with screws 10.
  • the micro- Sampling system consists of the functional units bypass block 1, micro-evaporator block 2, filter element 3a, pressure drop and discharge unit 4 and lid 5.
  • bypass block 1 For the rapid feeding of small amounts of sample to the micro-evaporator block 2, the fluid volume flow through capillaries, which are bolted to the bypass (screw 6a and 6b), passed through the bypass, in the bypass, the mass flow can be arbitrarily large.
  • the desired small amount of sample through a diaphragm 1 a in the direction of micro-evaporator block 2 is derived.
  • the arrows illustrate the flow direction of the sample.
  • the orifice la is located directly at the entrance of the micro-evaporator block 2.
  • the amount of the fluid sample to be evaporated can be controlled by the pressure in the bypass flow.
  • the microevaporator block 2 also has connections for heating elements 8 and a temperature sensor 9.
  • a microstructured plate 2a at the outlet of the micro-evaporator block 2 prevents a short circuit between the input of the evaporation chamber 2b and the input of the next functional unit. In addition, the vapor components are mixed and thus prevented fractionation.
  • the filter element 3a is made of stainless steel and has pore diameter ⁇ 2 lim.
  • the filter element 3a is integrated in a filter plate 3, which is pressed against the micro-evaporator block 2 and is thereby kept at the same temperature level as the micro-evaporator block 2.
  • the steam feed is discharged via the pressure drop and discharge unit 4 and condensed.
  • the vacuum of the analyzer, a mass spectrometer, is passed to the pressure drop unit 4, where a suitable means for determining the pressure drop 4a.
  • the functional element for the Druckabfa l 4a is inserted in a 4e Lemente 4d.
  • the stack construction of the micro-sampling system is completed with a cover 5 and the functional units of the device are pressed together with screws 10.
  • the cover 5 also has a connection element 7 for the capillary to the mass spectrometer. Sealing rings can be arranged between the individual units.
  • FIG. 2 shows the Mikroverdampferblock 2 in Stapelauibau.
  • the micro-evaporator block 2 has a small evaporation chamber 2b whose volume is ⁇ 100 ⁇ .
  • the only element between the evaporation chamber 2b and the bypass block I is the aperture 1 a. Therefore, the path between the two functional units is reduced to a minimum, preferably ⁇ 0.5 mm.
  • the small amount of fluid sample introduced into the evaporation chamber 2b becomes in a very short time evaporated.
  • the vapor volume is significantly above the liquid volume. This causes a very fast vapor flow at the exit of the evaporation chamber 2b.
  • At the outlet of the evaporation chamber 2b is followed by a microstructured plate 2a.
  • FIG. 3 shows an alternative design of the micro-sampling system as a block.
  • the individual functional units are arranged as block elements around the microevaporator block 2.
  • the operating principle of the device is identical to that in the stacked version in Figure 1.
  • the reference numerals of the components are also identical. This concept focuses on the dismantling of the individual functional elements.
  • the flow direction of the steam in the micro-evaporator block 2 is deflected by 90 °.
  • the path of the steam is sketched with open arrows. The steam is directed against the microstructured plate 2a, which initially deflects the flow upwards and then downwards.
  • the flow direction of the steam is deflected again (not shown) and guided in the direction of filter element 3a.
  • the filter element 3a Through the filter element 3a, the steam flows back into the micro-evaporator block 2. From there it is steered to the pressure drop unit 4 after a further detachment.
  • the drain is via ei ne capillary 4b, which here is fastened with the screw 4c on the micro-evaporator block 2. Due to the modular construction with deflected flow path for the steam, all functional units can be disassembled, exchanged and cleaned individually.
  • FIG. 4 shows the micro-evaporator block 2 in block construction. The operating principle is identical to that in Figure 3.

Abstract

L'invention concerne un système de prélèvement de microéchantillons pour de petites quantités d'échantillons de fluide pour une analyse en phase vapeur. Ledit système comprend plusieurs unités fonctionnelles intégrées et est approprié pour de faibles quantités d'échantillons avec des temps de réaction rapides.
EP12762542.4A 2011-08-19 2012-08-14 Système de prélèvement de microéchantillons pour de petites quantités d'échantillons de fluide pour analyse en phase vapeur Withdrawn EP2745089A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011081287A DE102011081287A1 (de) 2011-08-19 2011-08-19 Mikro-Probenentnahmesystem für kleine Mengen an Fluidproben zur Analyse in der Dampfphase
PCT/EP2012/065881 WO2013026743A1 (fr) 2011-08-19 2012-08-14 Système de prélèvement de microéchantillons pour de petites quantités d'échantillons de fluide pour analyse en phase vapeur

Publications (1)

Publication Number Publication Date
EP2745089A1 true EP2745089A1 (fr) 2014-06-25

Family

ID=46924392

Family Applications (1)

Application Number Title Priority Date Filing Date
EP12762542.4A Withdrawn EP2745089A1 (fr) 2011-08-19 2012-08-14 Système de prélèvement de microéchantillons pour de petites quantités d'échantillons de fluide pour analyse en phase vapeur

Country Status (5)

Country Link
US (1) US20140329333A1 (fr)
EP (1) EP2745089A1 (fr)
CN (1) CN103765186A (fr)
DE (1) DE102011081287A1 (fr)
WO (1) WO2013026743A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6351540B2 (ja) * 2014-10-14 2018-07-04 三菱電機株式会社 ガス分析装置およびガス分析方法
EP3418714A1 (fr) * 2017-06-19 2018-12-26 V&F Analyse- und Messtechnik GmbH Dispositif et procédé d'acheminement partiel d'un échantillon de liquide comprenant plusieurs composants et procédé de détermination en ligne et d'analyse desdits composants

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US2826180A (en) * 1954-05-13 1958-03-11 Phillips Petroleum Co Vaporizer
GB1016461A (en) * 1963-12-24 1966-01-12 British Petroleum Co Chromatographic sampling apparatus
US3244152A (en) * 1964-03-10 1966-04-05 Beckman Instruments Inc Sample vaporizer
US3772909A (en) * 1971-08-02 1973-11-20 Varian Associates Apparatus for analyzing environmental gases
FR2227890B1 (fr) * 1973-05-04 1975-12-26 Erap
US4057997A (en) * 1976-03-31 1977-11-15 Phillips Petroleum Company Sample preparation
JPS61180136A (ja) 1985-02-06 1986-08-12 Mitsubishi Heavy Ind Ltd ガスクロマトグラフ試料導入装置
DE10035297A1 (de) 2000-07-18 2002-02-07 Volker Barkey Eindampfvorrichtung für Proben
CN2499819Y (zh) * 2001-09-18 2002-07-10 中国人民解放军总装备部后勤部军事医学研究所 动态标准气样制备装置
CN2667484Y (zh) 2004-01-05 2004-12-29 郑州易科电力技术有限责任公司 用于化学分析的液体样品自动蒸发浓缩装置
DE102005034574A1 (de) * 2005-01-07 2006-07-20 Merck Patent Gmbh Verfahren und Vorrichtung zur Entnahme und Analyse von Proben
GB2436075B (en) * 2006-03-17 2009-04-15 Genevac Ltd Evaporator and method of operation thereof
US8181544B2 (en) 2008-11-18 2012-05-22 Picarro, Inc. Liquid sample evaporator for vapor analysis

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Title
See references of WO2013026743A1 *

Also Published As

Publication number Publication date
CN103765186A (zh) 2014-04-30
WO2013026743A1 (fr) 2013-02-28
DE102011081287A1 (de) 2013-02-21
US20140329333A1 (en) 2014-11-06

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