EP1746631B1 - Mikromechanisches Nano-Elektrodensystem - Google Patents
Mikromechanisches Nano-Elektrodensystem Download PDFInfo
- Publication number
- EP1746631B1 EP1746631B1 EP06117211.0A EP06117211A EP1746631B1 EP 1746631 B1 EP1746631 B1 EP 1746631B1 EP 06117211 A EP06117211 A EP 06117211A EP 1746631 B1 EP1746631 B1 EP 1746631B1
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- EP
- European Patent Office
- Prior art keywords
- capillary
- substrate
- electrode
- nanospray
- input
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- 150000002500 ions Chemical class 0.000 claims description 26
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/165—Electrospray ionisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0013—Miniaturised spectrometers, e.g. having smaller than usual scale, integrated conventional components
- H01J49/0018—Microminiaturised spectrometers, e.g. chip-integrated devices, Micro-Electro-Mechanical Systems [MEMS]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/067—Ion lenses, apertures, skimmers
Definitions
- This invention relates to mass spectrometry, and in particular to the use of mass spectrometry in conjunction with liquid chromatography or capillary electrophoresis.
- the invention particularly relates to a system and method that is implemented in a microengineered configuration.
- the spray is passed from atmospheric pressure via a chamber held at an intermediate pressure.
- Several vacuum interfaces that use differential pumping to match flow rates to achievable pressures have been developed [Duffin 1992].
- the ion optics normally consist of input and output orifices such as capillaries, capillary arrays and skimmer electrodes, and occasionally also a quadrupole lens operating as an ion guide in all-pass mode. These components are used to maximise the ratio of coupled ions to neutrals, which would otherwise swamp the chamber.
- US 5,386,115 discloses a solid state mass spectrograph that includes an inlet, a gas ionizer, a mass filter and a detector array all formed within a cavity in a semiconductor substrate.
- WO 2005/019804 A2 discloses a microfluidic chip formed with multiple fluid channels terminating at a tapered electrospray ionization tip for mass spectrometric analysis.
- the fluid channels may be formed onto a channel plate that are in fluid communication with corresponding reservoirs.
- the electrospray tip can be formed along a defined distal portion of the channel plate that can include a single or multiple tapered surfaces.
- the fluid channels may terminate at an open-tip region of the electrospray tip.
- a covering plate may substantially enclose most portions of the fluid channels formed on the channel plate except for the open-tip region.
- Another aspect of the invention provides methods for conducting mass spectrometric analysis of multiple samples flowing through individual fluid channels in a single micro fluidic chip that is formed with a tapered electrospray tip having an open-tip region.
- MEMS technology could be used to provide nanospray devices.
- the device must typically operate with high voltages, in a wet environment, so that electrical isolation and drainage are both required.
- the substrate material most commonly used in MEMS, silicon is therefore not appropriate; however, other insulating materials such as glasses are difficult to micromachine.
- an electrode containing an axially aligned orifice is typically required.
- electrostatic deflection or focusing is required.
- further electrodes containing aligned orifices are needed. If the ion path is itself in the plane of a substrate, such orifices are extremely difficult to form by in plane patterning alone.
- FIG. 1 illustrates the concept of a microengineered nanospray electrode system.
- a mass spectrometer 101 is provided in a high-vacuum enclosure 102 pumped (for example) by a turbomolecular pump 103. Ions are channelled into this chamber via a further chamber 104 held at an intermediate pressure and pumped (again, for example) by a rotary pump 105.
- the inlet to the vacuum system is assumed to be a capillary 106.
- the filter element of the mass spectrometer could be an ion trap, a quadrupole, a magnetic sector, a crossed-field or a time of flight device.
- the intermediate vacuum chamber could contain a range of components including further capillaries and skimmer electrodes.
- the overall input to the system is provided by a nanospray capillary 107.
- Alignment between the nanospray capillary 107 and the capillary input to the mass spectrometer 106 is provided by a microengineered chip 108.
- the chip contains a first set of mechanical alignment features 109 for the nanospray capillary and a second set of alignment features 110 for the capillary input to the mass spectrometer.
- the chip also contains a set of electrodes 111 set up perpendicular to the ion path, which may (for example, but not exclusively) consist of diaphragm electrodes. Other features may be integrated on the chip, including holes for drainage and gas inlet.
- the second substrate again consists of a base 208 formed in insulating material, and carrying a further set of electrodes corresponding to a further part of the features 111 in Figure 1 and consisting of grooves 209 etched into upright plates of conducting or semiconducting material 210.
- the partial electrode sets combine to form complete diaphragm electrodes with closed pupils 211.
- Figure 8 shows a mode of thermal operation.
- a current I is passed through one or more of the electrodes 801 to provide local heating, which may preferentially evaporate more volatile components in the spray such as a carrier solvent, thus enriching the analyte ion stream.
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Claims (32)
- Mikrotechnische Nanosprüh-Ionisationsvorrichtung, die auf einem einzelnen Chip (108) vorgesehen ist, der zur Kopplung zwischen einer Nano-Spray-Quelle und einem Massenspektrometer (106) konfiguriert ist, wobei die Vorrichtung ein erstes Ausrichtmittel (109) aufweist, das für ein Zusammenwirkten mit einem Kapillar-Eingang bestimmt ist, ein zweites Ausrichtmittel (110), dass zum Zusammenwirken mit einem Kapillar-Ausgang und einer öffnung bestimmt ist, die einen Ionenweg zwischen dem Kapillar-Eingang und dem Kapillar-Ausgang definiert, wobei die Vorrichtung weiters mindestens eine leilende Elektrode (111) aufweist, die in einer Orientierung von im Wesentlichen senkrechter Richtung zum Ionenweg vorgesehen ist, und wobei sowohl das erste Ausrichtmittel (109), das zweite Ausrichtmittel (110), die Öffnung und die mindestens eine Elektrode (111) in integral in dem Chip (108) gebildet sind.
- Vorrichtung nach Anspruch 1, wobei der Chip (208) aus zwei Substraten konstruiert ist, wobei die Substrate in einer Stapelkonfiguration kombiniert sind, um so den Chip (108) zu bilden.
- Vorrichtung nach Anspruch 2, wobei jedes der zwei Substrate mit einer Isolierbasis (201) versehen ist, wobei die Substrate relativ zueinander gestapelt sind, derart, dass der resultierende Chip (108) einen Isolationsabschnitt auf einer Außenfläche hiervon halt.
- Vorrichtung nach Anspruch 2 oder 3, wobei jedes der beiden Substrate mit individuellen Mitteln gebildet ist, welche Mitte derart konfiguriert sind, dass die resultierende Kombinatin der Mittel das Ausrichtmittel (109), das zweite Ausrichtmittel (110), die Öffnung und die mindestens eine Elektrode (111) definieren, wenn die zwei Substrate zusammengebracht werden.
- Vorrichtung nach Anspruch 4, wobei ein erstes Substrat ein erstes gerilltes Ausrichtmittel (204) für den Kapillar-Eingang und ein zweites gerilltes Ausrichtmittel (206) für den Kapillar-Ausgang definiert, wobei das Substrat zusätzlich hierauf die mindestens eine leitende Elektrode mit einem gerillten aufrechten Rand hat, der normal zum Substrat angeordnet ist.
- Vorrichtung nach Anspruch 5, wobei das zweite Substrat darauf mindestens eine leitende Elektrode (111) mit einem gerillten aufrechten Rand hat, der normal zum Substrat angeordnet ist.
- Vorrichtung nach Anspruch 6, wobei dem Stapeln des ersten und zweiten Substrates relativ zueinander die mindestens einen Elektroden (111), die auf dem ersten und zweiten Substrat vorgesehen sind, eine zusammenhängende Elektrode bilden, und die Elektrodenrillen sich zur Bildung von Öffnungen kombinieren.
- Vorrichtung nach einem der vorangehenden Ansprüche, wobei der Kapillar-Eingang eine Nano-Spray-Kapillare (106) ist.
- Vorrichtung Anspruch 8, wobei der Nano-Spray-Kapillar-Eingang ein Fluid bereitstellt, welches Fluid aus einem Flüssigkeitschromatographen-System entstammen kann.
- Vorrichtung nach Anspruch 8, wobei der Nano-Spray-Kapillar-Eingang ein Fluid bereitstellt, welches Fluid aus einem kapillaren elektrophoresichen System stammen kann.
- Vorrichtung nach einem der vorangehenden Anspruche, wobei die Elektrode (111) nächst zu der Eingangskapillare an erster Stelle dazu konfiguriert ist, einen Taylor-Kegel zu schaffen und dann Ionen von der in der Eingangskapillare enthaltendem Flüssigkeit zu extrahieren.
- Vorrichtung nach einem der vorangehenden Ansprüche, wobei der Kapillar-Ausgang den Eingang für einen Massenspektrometer (106) bildet.
- Vorrichtung nach einem der vorangehenden Ansprüche, aufweisend zumindest zwei Elektroden (111) und wobei mindestens eine zweite Elektrode konfiguriert list, um Ionen auf die Ausgangskapillare zu fokussieren.
- Vorrichtung nach einem der vorangehenden Ansprüche, wobei mindestens eine Elektrode elektrisch geheizt und konfiguriert ist, um vorzugsweise ein Lösungsmittel zu entfernen.
- Vorrichtung nach einem der Ansprüche, 1 - 13, wobei mindestens eine Elektrode segmentiert und konfiguriert ist, um ein ablenkendes laterales elektrisches Feld zu schaffen, um zur Separation von Ionen von Neutralen zu verhelfen.
- Vorrichtung nach Anspruch 15, wobei das ablenkende laterale Feld zeitlich variiert und konfiguriert ist, um eine Zerstäubung zu unterstützen.
- Vorrichtung nach einem der vorangehenden Ansprüche, wobei der Chip mindestens ein Entleerungsloch für Fluide enthält.
- Vorrichtung nach Anspruch 3, wobei zumindest eine erste Substratbasis mindestens ein Einlassloch für Gase und eine Plenumkammer (410) beinhaltet, die den Kapillar-Eingang umschließt.
- Vorrichtung nach Anspruch 18, wobei die Plenumkammer (410) angeordnet ist, um eine axiale Strömung von Gas zu schaffen, die als eine Umhüllung zum Spray angeordnet ist.
- Vorrichtung nach Anspruch 3, wobei die Isolationsbasis in einem fotomusterbaren Polymer gebildet ist.
- Vorrichtung nach Anspruch 18, wobei der Substrat-Basis-(201)-Außenumfang, die Entleerungslöcher und die Gaseinlässe durch Fotomusterung definiert sind.
- Vorrichtung nach einem der vorangehenden Ansprüche, wobei die Ausnchtmittel (109, 110) und Elektroden (111) in einem Halbleiter gebildet sind.
- Vorrichtung nach Anspruch 22, wobei der Halbleiter Silikon ist.
- Vorrichtung nach Anspruch 22, bei der der Halbleiter durch anisotrope Naßchemische Ätzung bis zu Kristallebenen verdrillt ist.
- Vorrichtung nach Anspruch 22, wobei der Halbleiter durch eine tiefenreaktive Ionenätzung (deep reactive ion etching) verrillt ist.
- Vorrichtung nach Anspruch 22, wobei entweder die Ausrichtmittel oder die Elektroden unter Anwendung einer tiefreaktiven Ionenätzung gebildet sind.
- Vorrichtung nach Anspruch 3, wobei die Elektroden, Rillen oder Substratbasen durch Sägen gebildet sind.
- Vorrichtung nach einem der vorangehenden Ansprüche, wobei die Ausrichtmittel (109, 110) und Elektroden (111) in einem Metall gebildet sind.
- Vorrichtung nach Anspruch 28, wobei das Metall durch Elektroplattierung abgesetzt ist.
- Vorrichtung nach Anspruch 3, wobei die Substratbasen in Glas geformt sind.
- Vorrichtung nach Anspruch 30, wobei das Glas fotomusterbar ist.
- Integrierte Systemeinheit mit einer Nano-Spray-Quelle mit einer Kapillar-Nadel an einem Ausgang hiervon, einem Massenspektrometer mit einer Kapillar-Nadel an einem Eingang hiervon und einer Nano-Spray-Ionisationsvorrichtung nach einem der vorangehenden Ansprüche, vorgesehen zwischen der Quelle und dem .Massenspektrometer (101), wobei die Ausrichtmittel (109, 110) der Vorrichtung Anschlussstellen für die Kapillar-Nadeln schaffen, um so ein von der Quelle abstammendes Fluid ionisieren und an dem Massenspektrometer (101) führen zu können.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GBGB0514843.2A GB0514843D0 (en) | 2005-07-20 | 2005-07-20 | Microengineered nanospray electrode system |
GB0519439A GB2428514B (en) | 2005-07-20 | 2005-09-23 | Microengineered nanospray electrode system |
Publications (3)
Publication Number | Publication Date |
---|---|
EP1746631A2 EP1746631A2 (de) | 2007-01-24 |
EP1746631A3 EP1746631A3 (de) | 2009-02-25 |
EP1746631B1 true EP1746631B1 (de) | 2013-06-19 |
Family
ID=37305854
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP06117211.0A Active EP1746631B1 (de) | 2005-07-20 | 2006-07-14 | Mikromechanisches Nano-Elektrodensystem |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP1746631B1 (de) |
JP (1) | JP5265095B2 (de) |
CA (1) | CA2552086C (de) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1959476A1 (de) * | 2007-02-19 | 2008-08-20 | Technische Universität Hamburg-Harburg | Massenspektrometer |
US8242441B2 (en) * | 2009-12-18 | 2012-08-14 | Thermo Finnigan Llc | Apparatus and methods for pneumatically-assisted electrospray emitter array |
GB2527803B (en) * | 2014-07-02 | 2018-02-07 | Microsaic Systems Plc | A method and system for monitoring biomolecule separations by mass spectrometry |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005019804A2 (en) * | 2003-08-26 | 2005-03-03 | Predicant Biosciences, Inc. | Microfluidic chip with enhanced tip for stable electrospray ionization |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5386115A (en) * | 1993-09-22 | 1995-01-31 | Westinghouse Electric Corporation | Solid state micro-machined mass spectrograph universal gas detection sensor |
CN1312473C (zh) * | 1998-09-17 | 2007-04-25 | 阿德文生物科学公司 | 液相色谱*** |
US6633031B1 (en) * | 1999-03-02 | 2003-10-14 | Advion Biosciences, Inc. | Integrated monolithic microfabricated dispensing nozzle and liquid chromatography-electrospray system and method |
US6396057B1 (en) * | 2000-04-18 | 2002-05-28 | Waters Investments Limited | Electrospray and other LC/MS interfaces |
JP2002190272A (ja) * | 2000-12-21 | 2002-07-05 | Jeol Ltd | エレクトロスプレー・イオン源 |
GB2391694B (en) * | 2002-08-01 | 2006-03-01 | Microsaic Systems Ltd | Monolithic micro-engineered mass spectrometer |
GB2422951B (en) * | 2005-02-07 | 2010-07-28 | Microsaic Systems Ltd | Integrated analytical device |
-
2006
- 2006-07-14 EP EP06117211.0A patent/EP1746631B1/de active Active
- 2006-07-14 CA CA2552086A patent/CA2552086C/en active Active
- 2006-07-20 JP JP2006197964A patent/JP5265095B2/ja not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005019804A2 (en) * | 2003-08-26 | 2005-03-03 | Predicant Biosciences, Inc. | Microfluidic chip with enhanced tip for stable electrospray ionization |
Also Published As
Publication number | Publication date |
---|---|
JP2007027131A (ja) | 2007-02-01 |
EP1746631A2 (de) | 2007-01-24 |
CA2552086C (en) | 2014-09-09 |
JP5265095B2 (ja) | 2013-08-14 |
EP1746631A3 (de) | 2009-02-25 |
CA2552086A1 (en) | 2007-01-20 |
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