EP1220285A2 - Source d' ions dans laquelle une source de lumière UV/VUV est utilisée pour l' ionisation - Google Patents

Source d' ions dans laquelle une source de lumière UV/VUV est utilisée pour l' ionisation Download PDF

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Publication number
EP1220285A2
EP1220285A2 EP01120299A EP01120299A EP1220285A2 EP 1220285 A2 EP1220285 A2 EP 1220285A2 EP 01120299 A EP01120299 A EP 01120299A EP 01120299 A EP01120299 A EP 01120299A EP 1220285 A2 EP1220285 A2 EP 1220285A2
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EP
European Patent Office
Prior art keywords
vuv
ionization
gas
ion source
light
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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.)
Granted
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EP01120299A
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German (de)
English (en)
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EP1220285B1 (fr
EP1220285A3 (fr
Inventor
Andreas Ulrich
Fabian Mühlberger
Ralf Dr. Zimmermann
Antonius Prof. Dr. Kettrup
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Helmholtz Zentrum Muenchen Deutsches F
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Helmholtz Zentrum Muenchen Deutsches Forschungszentrum fuer Gesundheit und Umwelt GmbH
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Publication of EP1220285A3 publication Critical patent/EP1220285A3/fr
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    • 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
    • H01J49/161—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
    • H01J49/162—Direct photo-ionisation, e.g. single photon or multi-photon ionisation

Definitions

  • the invention relates to an ion source in the UV / VUV light is used for ionization, according to the generic term of Claim 1, and their use.
  • VUV light can be generated by so-called micro hollow cathode lamps become.
  • One or more burning at the same time Discharges in small (typically 100 ⁇ m diameter) openings in constricted in a dielectric.
  • gas discharge parameters with can scale the product of diameter and gas pressure with the arrangement in turn, because of the small diameter with high Gas pressure maintain a stable glow discharge and VUV excimer light is generated in the dense gas [1].
  • Another alternative variant for generating brilliant UV / VUV radiation is a discharge in dense noble gases between pointed metal electrodes or a pointed metal electrode and a metal surface. These varinates of the corona discharge are operated with both high frequency and direct voltage [D. E. Murnick, M. Salvermoser, private communication, Gaseous Electronics Conference “GEC” 2000, 24.-27. October, Houston, Texas, USA, accepted for publication].
  • a particularly suitable for ion sources UV / VUV light source is the electron beam pumped structure described below.
  • Vacuum ultraviolet light generation in the light source which generates the ions in the ion source by photoionization, is carried out by exciting a dense gas with an electron beam [2, 3].
  • the gas usually consists of one of the noble gases He, Ne, Ar, Kr or Xe or a noble gas and the admixture of another gas, such as hydrogen.
  • VUV generation process in a gas cell is very inefficient. Therefore, powerful and therefore very expensive, large solid-state lasers are used (mostly Nd: YAG lasers with 355 nm). In operation, high additional costs arise from flash lamps (needed to pump the laser medium) and maintenance. Farther can generally only be a single one with a solid-state laser VUV wavelength can be generated (118 nm when using 355 nm laser radiation). Tunable solid-state lasers are extreme complex and cannot be used for practical analytical tasks. Frequency tripling is a very sensitive one nonlinear process, its VUV yield with the third power the primary radiation is scaled. This leads to a high one System instability and fluctuations in VUV yield. Furthermore, there is a complex separation of the primary radiation 355 nm necessary for fragmentation by VUV absorption to prevent ions formed.
  • Deuterium lamps based on a gas discharge in a deuterium gas can also be used and if they have a window that is transparent to vacuum ultraviolet light, e.g. B consisting of MgF 2 or LiF, emit continuum radiation and the so-called Lyman and Werner molecular bands around 160 and 130 nm, respectively.
  • Deuterium lamps are commercially available from various manufacturers.
  • VUV can light with so-called dielectrically disabled Discharges are generated, with a gas discharge at least one of the electrodes with a non-conductive layer is provided. [9].
  • a gas discharge at least one of the electrodes with a non-conductive layer is provided.
  • the object of the invention is an ion source with a light source to provide high useful photon density as well indicate an advantageous use
  • FIG. 1 shows an example of the configuration of the ionization region of a time-of-flight mass spectrometer with VUV Eximer lamp ionization.
  • FIG. 2 shows a section of the beam coupling and
  • FIG. 3 shows the entire mass spectrometer with the VUV Eximerlampe.
  • Figure 4 shows different options for coupling the UV / VUV light into the ionization chamber 14 or to the ionization site 23.
  • FIGS. 5 and 6 show examples Application results with the developed prototype.
  • the VUV Eximer lamp unit is e.g. via a flange to the Ionization chamber 14 coupled.
  • the upper part of the lamp serves for generating an electron beam 8 with the electron gun 1 and has a vacuum.
  • the electron tube 2 is about a getter pump 4 or a pump nozzle 5 is evacuated.
  • the Electron beam 8 is focused on the film 3.
  • the foil e.g. made of ceramic silicon nitride and separates that High vacuum of the electron tube 2 from the gas space 9.
  • the gas room 9 there is a gas mixture that is pumped over the electron beam Excimer process in the UV / VUV spectral range lights up (radiative Decay of the excimers).
  • the gas space 9 is a Getter 10 cleaned.
  • the lens 12 consists of UV / VUV transparent material (e.g. made of MgF2 or LiF) and separates the Gas space 9 from the ionization space 14 of the time-of-flight mass spectrometer (TOFMS).
  • TOFMS time-of-flight mass spectrometer
  • a multimicrochannel light guide 24 or 25 can be used.
  • a multi-micro-channel light guide 24 consists of a bundle with a large number of narrow capillaries (analogous to a micro-channel plate).
  • the UV / VUV light that falls through the capillaries can reach the ionization chamber 14, which has a vacuum. If the capillaries are sufficiently long and thin, the gas flow from the gas space 9 through the multimicrochannel light guide 24 into the ionization space 14 is very low (ie the vacuum in 14 is not overloaded too much).
  • the UV / VUV light either falls directly through the clear width of the capillary or is guided through one or more total reflections through the capillaries of the multimicrochannel light guide 24.
  • a multimicrochannel light guide 25 can be used, which allows the transmitted UV / VUV light beam 22 to be focused on the ionization site 23 by a conical taper of the capillary bundle.
  • the main advantage of using multimicrochannel light guides 24 or 25 is that they can transmit VUV light with wavelengths less than 110 nm.
  • Optical lenses 12 or windows for decoupling can only be used up to approximately this wavelength due to the self-absorption of the material (LiF, MgF 2 ).
  • Other sample gas inlet techniques such as pulsed [11] or continuous supersonic molecular beams [12] can also be used.
  • FIG. 3 shows a schematic illustration of a time-of-flight mass spectrometer (TOFMS, without representation of the vacuum pumps, of the reflectron ion mirror and other details) with electron beam pumped Excimer-ionization.
  • TOFMS time-of-flight mass spectrometer
  • the UV / VUV light from the electron beam pumped excimer lamp 20 becomes the optical elements described above in the from the inlet needle 15 emerging effusive molecular beam focused.
  • the Voltages in the ion source (simplified here with the electrodes 18, 16 and 17) are chosen so that the ionization space is field free.
  • the by single-photon absorption of VUV photons are not formed by electrical ions Fields affected.
  • the ions formed are thus enriched at and around the ionization site 23.
  • This ion enrichment can be operated for about a few ⁇ s, then leave the Ions due to space charge effects and airspeed the particles from the effusive molecular beam again the acceptance volume of the time-of-flight mass spectrometer (i.e. the Volume that can be imaged on the ion detector 21).
  • the controlled, pulsable high-voltage supply 19 suddenly suitable Potentials applied to the electrodes 18, 16 and 17.
  • the Rising edges of the voltage pulses are usually in the range of a few ns.
  • the ions are accelerated to the detector 21. in the field-free drift space (space between aperture 17 and detector 21) the ions separate according to their mass.
  • the time-of-flight mass spectrum is on the detector 21 with suitable electronics (not shown) registered.
  • Apertures 16 and 17 can be made of perforated screens with or without nets or just consist of networks.
  • the mass resolution and sensitivity in the operation of the TOFMS with ionization described above is limited by continuously shining VUV excimer lamps, because of the continuous operation of the lamp new ions are also formed during the ion withdrawal. These "subsequently" formed ions reach the detector later than ions formed during the enrichment period Mass (i.e. there are peak broadenings and an increased background signal on).
  • VUV excimer lamp can operate through the pulsed mode the VUV excimer lamp can be avoided.
  • the electron beam 8 is pulsed (e.g. by pulsed Aperture in the electron gun or through baffles) the film 3 steered.
  • the electron density can be increased thermally without the film 3 to overload.
  • VUV light emission 22 breaks within 500 to 1000 ns together. This can be exploited to get the ions from the ion source with already significantly reduced VUV light intensity deducted.
  • FIG. 5 shows measured parameters of the VUV excimer lamp ionization TOFMS (prototype) in pulsed operation. The upper trace shows the light pulse from the excimer lamp measured with a photodetector.
  • the middle track shows that Withdrawal pulse from the ion source and the lower trace shows the ion detector signal.
  • Piperidine (85 m / z) and Toluene (92 m / z) the corresponding mass peaks are in the lower one Trace visible.
  • VUV excimer lamp ionization is that by the choice of gas in the gas space 9 different wavelengths can be adjusted.
  • the selectivity of single-photon ionization is based on that only molecules whose ionization energy can be ionized below the photon energy of the incident VUV light is. This allows the ionization to be suppressed of compounds such as oxygen, nitrogen or noble gases, which have very high ionization energies. Hence the VUV ionization very good for on-line analysis of trace compounds from air or process gases (exhaust gases) because the main components the gas mixture cannot be ionized. Farther can also be a by using different wavelengths more precise statement about the composition of the observed Peaks in the mass spectrum can be achieved. For example with photon energies of about 9 eV, an involvement of aliphatic organic compounds excluded on the mass spectrum become.
  • Table 1 shows different gases or Gas mixtures with the corresponding emission wavelengths (maximum values) given.
  • Figure 6 shows the emission profiles of the VUV excimer lamp for argon (left, top) and krypton (left, below). The ionization energies of are also shown Benzene and toluene. On the right are the related ones measured TOFMS mass spectra of a mixture of benzene (92 m / z) and toluene.
  • the argon excimer emission (top) is 128 nm (9.7 eV). Both benzene and toluene are therefore efficiently ionized.
  • the Krypton Excimer Emission (Bottom) is 150 nm (8.2 eV).
  • toluene is right in the center the emission curve, while benzene only from a "shoulder emission" is detected on the high-energy side.
  • the toluene peak is therefore orders of magnitude more intense than the benzene peak.
  • Exhaust gas was released via an on-line sampling system a motorcycle (TYPE 43F) via the inlet needle 15 into the mass spectrum admitted.
  • the lamp was operated with argon (128 nm).
  • the figure shows a 3D plot of the mass spectrometric Information (mass, time, intensity) recorded during a starting process of the motorcycle.
  • Different aromatic compounds Benzene and methylated benzenes
  • Mass spectrometer with VUV excimer lamp ionization can advantageous for fast time-resolved online analysis of Process gases or used for headspace analysis.
  • Possible Fields of application are, for example, in the food industry (Monitoring of roasting, baking, cooking or Maturation processes etc.) of the chemical industry (monitoring of Syntheses, waste streams, mineral oil processing etc.), in the monitoring of combustion processes and other production processes.
  • VUV excimer lamp ionization can also be used with other types of mass spectrometers, that don't work pulsed like TOFMS, be used.
  • FIG. 8 shows one according to the invention built-up VUV excimer lamp with optical elements for focusing of the VUV light onto the ionization region of a Quadrupole mass spectrometer.
  • the ion source 29 is generated a continuous ion beam.
  • the Andes Quadruplolstäben 27 applied alternating electric fields (from control 28) only allow ions of one mass at a time pass from the ion beam to the detector 30.
  • Quadrupole mass spectrometer By changing the alternating fields by means of the controller 28 can be Quadrupole mass spectrometer in succession on a transmission different masses and so can a mass spectrum be included. Possible fields of application of the Quadrupole mass spectrometry with VUV excimer lamp ionization are, for example, in the area of the food industry (monitoring of roasting, baking, cooking or ripening processes etc.) chemical industry (monitoring of syntheses, waste streams, mineral oil processing, etc.) during monitoring of combustion processes and other production processes.
  • GC-MS is a standard technique of organic trace analysis.
  • VUV light for ionization for mass spectrometry in gas chromatography mass spectrometry Coupling brings another level of selectivity to the Mass spectrometry.
  • Certain connections with higher levels Ionization energies can be excluded from ionization become.
  • a fragmentation-free ionization is compared achieved the standard technique of electron impact ionization (EI).
  • EI electron impact ionization
  • Different types of mass spectrometers ion trap MS, Sector field MS, Qudrupol MS, Flight time MS can be used for this Purpose.
  • FIG. 9 shows the schematic structure an ionization cell detector with the VUV excimer lamp 20 of the generic type.
  • the ionization cell i.e. the ionization space 14
  • a suitable trigger voltage is applied.
  • the sample gas passes between electrodes 31 and 32 via an inlet 15 to the ionization zone.
  • an ammeter 34 can the photocurrent (photo ion current and photo electron current) be detected.
  • Such a detector has roughly the properties of a flame ionization detector, so it responds to most organic Compounds and on some inorganic species.
  • a VUV excimer lamp ionization cell detector can be beneficial for different Applications are used. For example, he can can be used as a detector for gas chromatography.
  • a Another possible application is the use as a sensor for the Occurrence of organic compounds in gas mixtures.
  • Figure 10 shows an example of the structure of an excimer VUV lamp in which one of the two excimer light sources is used by means of an electron gun 1 36 of the generic type depending on the adjacent electric field pumped between the deflection electrodes 35 and is thus brought to light.
  • the gas spaces 9 are filled of the two excimer light sources with different gases or Gas mixtures (see Tab. 1), the photons have the generated Light of the two excimer light sources is different Photon energy.

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  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Sources, Ion Sources (AREA)
EP01120299.1A 2000-09-09 2001-08-24 Source d' ions dans laquelle une source de lumière UV/VUV est utilisée pour l' ionisation Expired - Lifetime EP1220285B1 (fr)

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DE2000144655 DE10044655A1 (de) 2000-09-09 2000-09-09 Ionenquelle bei der UV-VUV-Licht zur Ionisation verwendet wird
DE10044655 2000-09-09

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102103971B (zh) * 2009-12-18 2012-11-07 中国科学院大连化学物理研究所 微型质谱仪中空心阴极放电真空紫外光电离源
CN111929354A (zh) * 2020-07-02 2020-11-13 东华理工大学 一种稀土矿样顺次电离分析仪器

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DE10236344B4 (de) 2002-08-08 2007-03-29 Bruker Daltonik Gmbh Ionisieren an Atmosphärendruck für massenspektrometrische Analysen
DE102005039269B4 (de) * 2005-08-19 2011-04-14 Helmholtz Zentrum München Deutsches Forschungszentrum Für Gesundheit Und Umwelt (Gmbh) Verfahren und Vorrichtung zum massenspektrometrischen Nachweis von Verbindungen
US8721836B2 (en) 2008-04-22 2014-05-13 Micron Technology, Inc. Plasma processing with preionized and predissociated tuning gases and associated systems and methods
DE102012209324A1 (de) * 2012-06-01 2013-12-05 Helmholtz Zentrum München Lichtleitervorrichtung für ein Ionisierungsgerät und Verfahren zum Ionisieren von Atomen und/oder Molekülen
CZ306584B6 (cs) 2015-11-16 2017-03-15 Univerzita Tomáše Bati ve Zlíně Zařízení pro generování UV záření a způsob generování tohoto záření
CN107014892B (zh) * 2017-05-15 2019-06-18 清华大学 一种基于真空紫外激光的微米级空间分辨质谱成像系统

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102103971B (zh) * 2009-12-18 2012-11-07 中国科学院大连化学物理研究所 微型质谱仪中空心阴极放电真空紫外光电离源
CN111929354A (zh) * 2020-07-02 2020-11-13 东华理工大学 一种稀土矿样顺次电离分析仪器
CN111929354B (zh) * 2020-07-02 2021-09-17 东华理工大学 一种稀土矿样顺次电离分析仪器

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EP1220285B1 (fr) 2014-08-20
EP1220285A3 (fr) 2005-03-16

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