US20130077943A1 - Liquid evaporator - Google Patents

Liquid evaporator Download PDF

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Publication number
US20130077943A1
US20130077943A1 US13/643,514 US201113643514A US2013077943A1 US 20130077943 A1 US20130077943 A1 US 20130077943A1 US 201113643514 A US201113643514 A US 201113643514A US 2013077943 A1 US2013077943 A1 US 2013077943A1
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US
United States
Prior art keywords
liquid
chamber
opening
channel
evaporation
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.)
Abandoned
Application number
US13/643,514
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English (en)
Inventor
Jörg Müller
Winfred Kuipers
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.)
Krohne Messtechnik GmbH and Co KG
Bayer Intellectual Property GmbH
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 US20130077943A1 publication Critical patent/US20130077943A1/en
Assigned to KROHNE MESSTECHNIK GMBH & CO. KG, BAYER INTELLECTUAL PROPERTY GMBH reassignment KROHNE MESSTECHNIK GMBH & CO. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MUELLER, JOERG, DR., Kuipers, Winfred
Abandoned legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24H—FLUID HEATERS, e.g. WATER OR AIR HEATERS, HAVING HEAT-GENERATING MEANS, e.g. HEAT PUMPS, IN GENERAL
    • F24H9/00—Details
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01B—BOILING; BOILING APPARATUS ; EVAPORATION; EVAPORATION APPARATUS
    • B01B1/00—Boiling; Boiling apparatus for physical or chemical purposes ; Evaporation in general
    • B01B1/005—Evaporation for physical or chemical purposes; Evaporation apparatus therefor, e.g. evaporation of liquids for gas phase reactions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
    • H01J49/049—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample with means for applying heat to desorb the sample; Evaporation
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • H05B6/80—Apparatus for specific applications
    • H05B6/802—Apparatus for specific applications for heating fluids
    • H05B6/804—Water heaters, water boilers
    • 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
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes

Definitions

  • the present invention relates to a liquid evaporator and to a method for evaporating liquids.
  • Liquid evaporators are used for converting liquids into the gas phase and are employed in various applications.
  • U.S. Pat. No. 7,618,027B2 discloses, for example, a liquid evaporator for generating a highly pure gas with a low vapour pressure, the gas being used in the field of microelectronics.
  • WO05/016512A1 discloses, for example, a liquid evaporator which can be used in a method for removing a volatile compound from a substance mixture.
  • Liquid evaporators also have widespread use in analysis, where a sample quantity of a liquid to be analysed is first converted into the gas phase in order to make it accessible for an analysis method.
  • U.S. Pat. No. 7,309,859B2 discloses, for example, a liquid evaporator which can be used in an ion source for mass spectrometers.
  • liquid evaporators have preferably been configured as constantly heated systems to which liquid samples are supplied continuously in small quantities.
  • a high heat capacity of the evaporator is generally necessary, together with a high thermal mass. This entails a high energy demand and—owing to the in general spatially extended structure of the evaporator—a correspondingly high power demand and concomitantly sometimes also long dead times between sampling and evaporation.
  • micro mass spectrometers are known (see for example WO08/101669A1) which can function with minimal sample quantities.
  • sample quantity is on the one hand advantageous. Smaller sample quantities mean, for example, a shorter evaporation time and therefore a higher temporal resolution with which changes in sample composition can be recorded.
  • the liquid evaporator needs to be adapted to the small sample quantity in order to be able to fully exploit the advantages of a smaller sample quantity.
  • the sample volume to be evaporated is in this context preferably less than 100 ⁇ l, particularly preferably less than 10 ⁇ l, more particularly preferably less than 1 ⁇ l.
  • the sample quantity evaporated should be representative of the liquid from which it is taken.
  • the liquid evaporator should be economical to manufacture and operate, have a low energy demand for the evaporation and ensure rapid evaporation.
  • the liquid evaporator should either have self-cleaning capabilities, so that it is even possible to evaporate liquids which contain dissolved substances that may possibly leave a deposit, or be configured as a disposable article.
  • this object is achieved by a method for evaporating at least a part of a liquid according to Claim 1 , and by a liquid evaporator according to Claim 4 , which is formed in order to carry out the method.
  • a method for evaporating at least a part of a liquid according to Claim 1 and by a liquid evaporator according to Claim 4 , which is formed in order to carry out the method.
  • Preferred embodiments may be found in the dependent claims.
  • the present invention therefore firstly provides a method for evaporating at least a part of a liquid, characterized in that a liquid is fed through a channel past an opening, the opening leading to a vapour chamber which is maintained at a temperature above the evaporation temperature of the liquid, and the liquid is heated in the region of the opening by electromagnetic radiation so that at least a part of the liquid evaporates and the vapour enters the heated vapour chamber.
  • the present invention secondly provides a liquid evaporator comprising at least
  • the method according to the invention and the evaporator according to the invention use the energy of electromagnetic radiation in order to evaporate a sample quantity of a liquid by local heating.
  • a liquid is passed through a channel which leads past an opening into a chamber.
  • the region of the opening is accessible for electromagnetic radiation, i.e. it can be irradiated with electromagnetic radiation.
  • the liquid is locally heated by means of electromagnetic radiation to such an extent that a sample quantity evaporates.
  • the evaporated sample quantity passes through the opening into a chamber—also referred to below as the vapour chamber—which can be heated to a temperature above the evaporation temperature of the liquid, so that the vapour does not condense in the chamber.
  • the electromagnetic radiation is preferably supplied to the evaporation site from outside the liquid evaporator.
  • the evaporation site is therefore preferably provided with a cover which is at least partially transparent for the electromagnetic radiation being used.
  • An at least partially transparent cover is intended to mean a cover which preferably transmits a majority of the electromagnetic radiation and absorbs and/or reflects only a small part, so that a majority of the incident energy reaches the evaporation site and is available there for heating a sample quantity.
  • a high transparency and therefore low absorption of the cover also have the effect that the cover itself is not heated.
  • the evaporation region is configured so that it absorbs a high proportion of the electromagnetic radiation and converts it into heat.
  • the inner walls of the channel may consist of a material which absorbs a majority of the incident energy and converts it into heat. It is likewise conceivable for the inner walls of the channel to be coated in the evaporation region with a material which has a high absorption coefficient for the radiation being used. In both of these cases, by means of the evaporator it is even possible to evaporate liquids which themselves have only a low absorption coefficient for the radiation being used; the heating takes place indirectly.
  • the evaporation region when it is adapted for indirect heating of the liquid, will also be referred to below as the absorber.
  • the radiation source used is matched to the liquid to be evaporated so as to allow direct heating of the liquid.
  • Direct heating has the advantage that the environment of the liquid is heated only slightly, and detrimental effects on the analysis due to a heated environment (lower temporal resolution, contamination, damage, etc.) are thus minimized.
  • a laser beam is preferably used for the irradiation.
  • a pulsed, focused laser beam is particularly preferably used.
  • the laser pulse length is preferably selected so that the thermal time constants of the absorber and/or the liquid to be evaporated are long compared with this pulse length. This means that even a single pulse is sufficient to evaporate a sample quantity.
  • the quantity of liquid evaporated may be varied by varying the length of the laser pulse and by varying its power.
  • a pulse sequence may also be used. Since the instant of the evaporation can be established very accurately, the vapour generation can be synchronized with sampling in an analyser so that a correlation measurement with increased measurement sensitivity is possible. Furthermore, this method allows segments of a sample flow to be evaporated and analysed in a controlled way, so that in particular even sample compositions which vary greatly as a function of time or, for example, unmixed or undissolved components carried by the liquid (emulsions, cells) can be recorded in a defined or selective way.
  • the laser beam is preferably supplied to the evaporation region through a cover, which is at least partially transparent for the laser beam, by means of free-beam or fibre optics.
  • the transition from the channel to the vapour chamber is configured so that, because of the capillary forces prevailing in the opening, the liquid cannot flow freely into the chamber. Suppression of the liquid egress is preferably achieved by a sufficiently large difference between the cross section of the chamber dimension at the position of the opening and the length of the interface with the channel and its cross section.
  • the inner walls of the channel and the chamber may be provided, at least in the opening region, with layers having different surface energies. If the liquid to be evaporated is an aqueous solution, for example, the opening region of the channel may be coated hydrophilically and that of the chamber may be coated hydrophobically.
  • the channel preferably has a curvature in the region of the evaporation.
  • the curvature leads to different flow rates in the inner and outer curve regions.
  • Dean vortices are generated, which lead to a flow perpendicular to the flow direction and convey liquid elements from the middle of the channel to the channel edge in the opening region.
  • the vapour chamber has a gas outlet, through which the vapour can leave the liquid evaporator according to the invention.
  • the chamber may be provided with further connections which, in particular, allow evacuation and optionally also flushing of the chamber between the sampling intervals, in order to avoid cross-contamination of samples from one evaporation process to the next.
  • this may also respectively be done in a controlled way after a plurality of evaporations, in order to increase the available gas quantity and/or its pressure for the injection or to permit averaging over a plurality of sample volumes directly before the analysis.
  • the vapour chamber may be heated by means of a heating element, which is preferably operated electrically.
  • lamellar structures made of a thermally conductive material may additionally extend through the vapour chamber, which preferably is locally heated by surface contact heating, these structures likewise being heated by the heating device via thermal conduction.
  • the structures are preferably applied so that they prevent particles from passing through the gas outlet (see FIG. 2 ), i.e. they preferably shield the opening and the gas outlet from one another.
  • the liquid evaporator according to the invention is configured as a disposable article.
  • the body of the liquid evaporator according to the invention in which the channel and chamber are formed, may be configured in one piece or a plurality of pieces. It is preferably configured in one piece.
  • the liquid evaporator is preferably a microsystem, the structures of which are produced by means of microfabrication techniques.
  • microsystems The production of structures in microsystems is known to the person skilled in the art of microsystem technology.
  • Microfabrication techniques are, for example, described and illustrated in the book “Fundamentals of Microfabrication” by Marc Madou, CRC Press Boca Raton Fla. 1997 or in the book “Mikrosystemtechnik für Ingenieure” [Microsystem technology for engineers] by W. Menz. J. Mohr and 0. Paul, Wiley-VCH, Weinheim 2005.
  • a more detailed description of silicon-on-silicon technology may for example be found in Q.-Y. Tong, U. Gösele: Semiconductor Wafer Bonding: Science and Technology; The Electrochemical Society Series, Wiley-Verlag, New York (1999).
  • Microsystem technologies are fundamentally based on the structuring of silicon and/or glass substrates with a high aspect ratio (for example narrow trenches ( ⁇ m) of great depth ( ⁇ 100 ⁇ m)) with structuring accuracies in the micrometre range using wet chemical, preferably plasma etching processes combined with sodium-containing glass substrates adapted in terms of their thermal expansion coefficient (for example Pyrex®), which are provided with simple etched structures and preferably connected to one another with a hermetic seal directly by so-called anodic bonding, or alternatively with a thin Au layer functioning as a solder alloy (AuSi).
  • a high aspect ratio for example narrow trenches ( ⁇ m) of great depth ( ⁇ 100 ⁇ m)
  • structuring accuracies in the micrometre range using wet chemical, preferably plasma etching processes combined with sodium-containing glass substrates adapted in terms of their thermal expansion coefficient (for example Pyrex®), which are provided with simple etched structures and preferably connected to one another with a her
  • Metal structures with a high aspect ratio can be produced by electrolytic growth in thick photoresists (>100 ⁇ m) with comparable accuracy (UV-LIGA).
  • thin-film technologies such as high vacuum evaporation and sputtering, PVD processes or chemical vapour deposition (CVD processes) preferably in a plasma, in combination with photolithography and etching techniques, functional layers such as metallizations, hydrophobic or hydrophilic surfaces and functional elements such as valve seals and diaphragms, heating elements, temperature, pressure and flow sensors can be integrated on these substrates in a fully process-compatible technology.
  • the structures of the liquid evaporator according to the invention are preferably produced in a silicon-on-glass technology, silicon being used for the body and glass being used for the transparent cover.
  • This combination preferably connected hermetically by anodic bonding, allows highly accurate structuring of the various components of the system, particularly in silicon (photoetch technology, DRIE, coating).
  • Silicon is chemically and thermally stable like glass, and in contrast to glass it is a good thermal conductor with low heat capacity (heated chamber with uniform temperature) and a good optical absorber for conventional laser wavelengths. The heat losses by dissipation through the glass substrate are low.
  • the combination of silicon and glass makes it possible to achieve local input of the optical energy into the channel edge as well as thermal decoupling of the channel and the vapour chamber.
  • the vapour chamber and the liquid sample channel are preferably separated by horizontal and vertical incisions in the highly thermally conductive body.
  • Mechanical stability with low heat transfer is ensured by a transparent cover, for example made of glass or a polymer.
  • liquid evaporator from polymer materials, for example by means of injection moulding techniques.
  • a composite material is preferably used for the body, for example a polymer in which carbon (carbon black, carbon nanotubes) is dispersed in order to increase the absorption of electromagnetic radiation and the thermal conductivity.
  • a system produced in this way is also especially suitable for analysing or producing small sample volumes (nl liquid, ⁇ l in the gas phase).
  • the sample volume to be evaporated is preferably less than 100 ⁇ l, particularly preferably less than 10 ⁇ l, more particularly preferably less than 1 ⁇ l.
  • the liquid evaporator according to the invention is preferably suitable as a sample evaporator in a microanalysis system.
  • the present invention therefore also provides the use of the liquid evaporator according to the invention in a microanalysis system, particularly in a micro gas chromatograph or a micro mass spectrometer, as described for example in the article “ Complex MEMS: A fully integrated TOF micro mass spectrometer” published in Sensors and Actuators A: Physical, 138 (1) (2007), pages 22-27.
  • FIG. 1 shows a perspective representation of a liquid evaporator according to the invention from above.
  • the liquid evaporator comprises a body 6 , in which a channel 5 and a chamber 9 are formed.
  • the channel 5 and the chamber 9 are connected to one another through an opening 4 .
  • the channel 5 has a curvature 10 in the region of the opening 4 .
  • a liquid is fed through the channel 5 past the opening 4 .
  • the transition from the opening 4 to the chamber 9 is configured so that, because of the capillary forces prevailing in the opening, the liquid cannot flow into the directly adjacent region 9 .
  • the liquid In the region of the opening, the liquid is irradiated by means of electromagnetic radiation and therefore heated. In the present case, the irradiation takes place from the direction of the observer (from above).
  • the liquid is heated and a part of it evaporates, this part entering the chamber 9 through the opening 4 as a vapour stream.
  • a heating element by which the chamber can be heated (not shown in FIG. 1 ; see FIG. 3 ).
  • the vapour chamber 9 and liquid sample channel 5 are thermally decoupled by horizontal incisions 14 in the highly thermally conductive body 6 .
  • FIG. 2 shows the liquid evaporator of FIG. 1 , in the chamber 9 of which lamellar structures 12 are introduced.
  • the lamellar structures are preferably heated by the heating element below the chamber 9 (not shown in FIG. 2 ; see FIG. 3 ) via thermal conduction.
  • FIG. 3 shows the liquid evaporator according to the invention of FIG. 1 in cross section along a straight line from A to B. Besides the components already described above in relation to FIG. 1 , a transparent cover 2 can be seen in FIG. 3 which extends over the entire body 6 . A heating element 8 is furthermore installed below the vapour chamber. The irradiation of the liquid takes place through the transparent cover, preferably by means of a focused laser beam 1 .

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electromagnetism (AREA)
  • Thermal Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Sampling And Sample Adjustment (AREA)
US13/643,514 2010-04-29 2011-04-26 Liquid evaporator Abandoned US20130077943A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102010018830A DE102010018830A1 (de) 2010-04-29 2010-04-29 Flüssigkeitsverdampfer
DE10201001830.1 2010-04-29
PCT/EP2011/056593 WO2011134968A1 (de) 2010-04-29 2011-04-26 Flüssigkeitsverdampfer

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US (1) US20130077943A1 (enrdf_load_stackoverflow)
EP (1) EP2563490A1 (enrdf_load_stackoverflow)
JP (1) JP2013527443A (enrdf_load_stackoverflow)
CN (1) CN103108682A (enrdf_load_stackoverflow)
CA (1) CA2797608A1 (enrdf_load_stackoverflow)
DE (1) DE102010018830A1 (enrdf_load_stackoverflow)
WO (1) WO2011134968A1 (enrdf_load_stackoverflow)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014222190A (ja) * 2013-05-14 2014-11-27 国立大学法人福井大学 試料溶液の質量分析方法及びその装置
NL2023927B1 (en) 2019-10-01 2021-06-01 Berkin Bv In-flow evaporator
US11938414B1 (en) * 2022-10-04 2024-03-26 Honeywell Federal Manufacturing & Technologies, Llc Microfluidic film evaporation with femtosecond laser-patterned surface

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CN103529149A (zh) * 2013-10-28 2014-01-22 徐继承 一种防堵塞的低压液化气体检验用进样蒸发器
CN103543228A (zh) * 2013-10-28 2014-01-29 徐继承 一种含有大气平衡装置的低压液化气体检验用进样蒸发器
CN104392883A (zh) * 2014-10-22 2015-03-04 常州博锐恒电子科技有限公司 一种注入机固体进料方法
CN116647901A (zh) 2017-12-22 2023-08-25 华为技术有限公司 无线唤醒包发送与接收方法与装置
CN109289948B (zh) * 2018-10-08 2020-02-18 重庆大学 一种光热定向操控液滴迁移聚合装置及其使用方法
CN109444248B (zh) * 2018-11-20 2020-10-30 中国地质大学（武汉） 一种基于激光的溶液剥蚀进样分析方法
CN115155077B (zh) * 2022-07-04 2023-08-18 枣庄学院 多组分液体微量蒸发装置

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JP2014222190A (ja) * 2013-05-14 2014-11-27 国立大学法人福井大学 試料溶液の質量分析方法及びその装置
NL2023927B1 (en) 2019-10-01 2021-06-01 Berkin Bv In-flow evaporator
US11938414B1 (en) * 2022-10-04 2024-03-26 Honeywell Federal Manufacturing & Technologies, Llc Microfluidic film evaporation with femtosecond laser-patterned surface
US20240109001A1 (en) * 2022-10-04 2024-04-04 Honeywell Federal Manufacturing & Technologies, Llc Microfluidic film evaporation with femtosecond laser-patterned surface

Also Published As

Publication number Publication date
WO2011134968A1 (de) 2011-11-03
JP2013527443A (ja) 2013-06-27
DE102010018830A1 (de) 2011-11-03
CN103108682A (zh) 2013-05-15
CA2797608A1 (en) 2011-11-03
EP2563490A1 (de) 2013-03-06

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Owner name: BAYER INTELLECTUAL PROPERTY GMBH, GERMANY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:MUELLER, JOERG, DR.;KUIPERS, WINFRED;SIGNING DATES FROM 20121025 TO 20121029;REEL/FRAME:031957/0138

STCB Information on status: application discontinuation

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