EP1274117A2 - Méthode et dispositif pour l' analyse de la composition chimique de particules d' aérosols - Google Patents

Méthode et dispositif pour l' analyse de la composition chimique de particules d' aérosols Download PDF

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Publication number
EP1274117A2
EP1274117A2 EP02013194A EP02013194A EP1274117A2 EP 1274117 A2 EP1274117 A2 EP 1274117A2 EP 02013194 A EP02013194 A EP 02013194A EP 02013194 A EP02013194 A EP 02013194A EP 1274117 A2 EP1274117 A2 EP 1274117A2
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EP
European Patent Office
Prior art keywords
ionization
aerosol
particles
heatable surface
mass spectrometer
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Withdrawn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
EP02013194A
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German (de)
English (en)
Other versions
EP1274117A3 (fr
Inventor
Ralf Prof. Dr. Zimmermann
Thomas Ferge
Antonius Prof. Dr. Kettrup
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.)
Helmholtz Zentrum Muenchen Deutsches F
Original Assignee
Helmholtz Zentrum Muenchen Deutsches Forschungszentrum fuer Gesundheit und Umwelt GmbH
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Publication date
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Publication of EP1274117A2 publication Critical patent/EP1274117A2/fr
Publication of EP1274117A3 publication Critical patent/EP1274117A3/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • 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
    • H01J49/0445—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 with means for introducing as a spray, a jet or an aerosol
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/40—Time-of-flight spectrometers

Definitions

  • the invention relates to a method and an apparatus for quantitative determination of the chemical composition of aerosol particles.
  • Methods for determining the chemical composition of aerosol particles are based on online methods such. B. on laser mass spectrometry. However, no quantifiable statements can be made with these methods. Quantifiable analysis methods are only available off-line, ie the chemical composition can only be determined quantitatively from a collected sample. Another elegant way of quantifying the chemical composition is the thermal evaporation of particles and particle components. The components are evaporated and ionized quantitatively by rapid heating of the particles to a certain preselected temperature and can thus be analyzed in a mass spectrometer.
  • Determination of the chemical composition of aerosol particles is carried out on collected samples using various analysis methods. These include extraction and separation of organic components by gas chromatography [1] or the determination of the elementary composition by means of PIXE [2].
  • the disadvantage of these methods is that they are off-line Character, because particle samples for long periods of time must be collected. But have such filter samples the disadvantage that during the analysis no statements about the Size distribution and possible distribution of the chemical components the particles hit over the measured size range can be. But important insights are straight about the morphology and the composition of individual or accessible to a few particles.
  • Off-line one-particle analysis is, for example, with laser microprobe mass spectrometry possible [2, 3]. It allows the chemical Characterization of individual particles.
  • One-particle laser mass spectrometry has been used in recent years successful for a number of studies on environmental aerosols or used on particles generated in the laboratory.
  • a Quadrupole mass spectrometers are only proof a single mass and therefore molecular species per unit of time possible.
  • the object of the invention is an apparatus and a method for quantitative on-line determination of the chemical composition of aerosol particles.
  • the measuring principle is based on the thermal evaporation of the particles on a heated surface and detection of the directly formed ions or ionization and subsequent detection of the gaseous molecules and molecular fragments formed using various ionization techniques. These include laser ionization with different wavelengths (266nm for REMPI - r esonance e nhanced m ulti p hoton i onisation, 118nm for V acuum- UV s ingle p hoton i onisation - VUV-SPI) as well as light-induced electron impact ionisation (LEI) [7, 8] ,
  • Time-of-flight mass spectrometry is particularly suitable for fast (to maintain online capability) and complete (to detect all ions formed) analysis.
  • the heated surface must be introduced into the ionization chamber in such a way that the fields required to accelerate the ions formed are disturbed as little as possible. This can be accomplished through the special geometric design and arrangement of this surface.
  • spatially small areas are suitable, such as the flattened tip of a thin needle.
  • the particles are now analyzed by detecting the ions formed.
  • their chemical composition is also determined quantitatively. The invention is explained in more detail below on the basis of exemplary embodiments with the aid of FIGS. 1 to 4.
  • FIG. 1 shows a typical bipolar aeroreol time-of-flight mass spectrometer.
  • the particles are suddenly separated from the gas phase by a skimmer system with differential vacuum pump stages and accelerated as a function of their mass and thus coupled size.
  • a particle beam 18 is formed.
  • 3 choppers 37 FIG. 4b
  • the increased requirements make the size range narrower, that is, the fractionation is finer.
  • the speed of the aerosol particles determined in this way can then be used, when the chopper position and circulation frequency are known, which can be determined and regulated via a light barrier system (not shown in the drawing for reasons of space), for calculating the flight time until it hits the heated baffle surface 1. This is necessary for triggering the ionization laser 17 and for triggering the pulsed ion extraction in the mass spectrometer. When they hit the heated surface, the components of the aerosol particle are thermally evaporated and ionized. The ions formed directly during evaporation and the components of the molecular cloud formed which have been subsequently ionized with a suitable wavelength of laser radiation are then detected by mass spectrometry.
  • the baffle As an elongated rectangular Baffle 1 can be reached.
  • a body a suitably arranged plate-shaped body 25 in question.
  • the heating of the elements 22, 23, 24, 25 can for example through thermal conduction (i.e. through contact with a body brought to temperatures of 30-2800 ° C) or by irradiating target region 1 with IR laser light respectively.
  • the stretched baffle by a heating tape 26, which is heated via the contact wires 27 will be formed.
  • the one formed by the heating tape 26 Area can also be pulsed briefly to the desired one Temperature can be brought up to one on the colder surface collected amount of particles (or their thermally evaporable Portion) to evaporate quantitatively and as described ionize and analyze.
  • One possibility for the improved heating of the stretched Impact surface by IR laser radiation is geometrical Formed as a wire-shaped body with a t-shaped Target region 28. Due to the constriction at the transition between Baffle 1 and wire can transfer heat from the area the area can be reduced, creating this geometry is especially suitable for use with IR laser pulses.
  • FIG 3a A possible version of an ionization finger is shown in FIG 3a.
  • a wire-shaped object 29 is made by contact with a heating element 32 to the desired temperature brought.
  • a heating element 32 For insulation, it is surrounded by ceramic sleeves 30, the surfaces of which are covered with a thin layer of metal, which can be connected to potential via a wire feed.
  • the heating of the target region 1, as in Figure 3b shown done only in a thin layer.
  • the baffle 1 as a thin high-resistance plate or Coating 33 executed, which with electrical leads 34 and leads 35, which is connected by a thin insulator layer 36 are separated.
  • a reactive gas for example ammonia, NH 3
  • This can be passed over the heated surface via a capillary inlet and react with the ions and molecules formed by impact on the impact surface 1 under the influence of electron bombardment (LEI).
  • LAI electron bombardment
  • a particle beam can be formed an alternate inlet can also be used to analyze fine and ultrafine particles.
  • the polydisperse aerosol first by means of an aerodynamic Focused lens [9] to a particle beam and then again through a system of 2 to 3 time-coupled choppers 37 selected a certain size fraction (FIG 4). Again, only those particles that have a have suitable speed and the correlated size pass freely through the rotating chopper 37 and hit the heated baffle 1. With this device can then be used in experiments with pulsed ion extraction the composition of fine particles can be determined.
  • the range of ultrafine particles can, however, be the chopper system described no longer in different Size intervals are fractional because of the speed of the different particles in this size range almost becomes identical.
  • a distinction between the different size fractions in this area with an electrostatic Classifiers possible. This selects based on the Mobility in an electric field a certain size fraction from the polydisperse aerosol, these particles become then focused into a beam by the aerodynamic lens and aimed at the heated surface.
  • a single one Chopper ( Figure 4c) enables this again, for example Impact of defined quantities of particles on the surface. Becomes the area pulsed heated can also with this device ultrafine particles can be analyzed quantitatively.
  • Double reflectron spectrometers can advantageously be used for the detection be used. These are suitable because of the possible simultaneous detection of both positive and negative ions very good for analysis of aerosol particles.
  • the use of a double TOFMS system and pulsed Voltages to withdraw the ions (“delayed extraction” technique) thus allows great variability in the detection of chemical particle composition and particle properties.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
EP02013194A 2001-07-05 2002-06-15 Méthode et dispositif pour l' analyse de la composition chimique de particules d' aérosols Withdrawn EP1274117A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10132735 2001-07-05
DE2001132735 DE10132735A1 (de) 2001-07-05 2001-07-05 Verfahren und Vorrichtung zum Nachweis der chemischen Zusammensetzung von Aerosolpartikeln

Publications (2)

Publication Number Publication Date
EP1274117A2 true EP1274117A2 (fr) 2003-01-08
EP1274117A3 EP1274117A3 (fr) 2006-01-25

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EP (1) EP1274117A3 (fr)
DE (1) DE10132735A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004025841A1 (de) * 2004-05-24 2005-12-15 Bergische Universität Wuppertal Verfahren und Vorrichtung zur massenspektroskopischen Untersuchung von Analyten
DE102008035773A1 (de) * 2008-07-31 2010-02-04 Eads Deutschland Gmbh Verfahren und Vorrichtung zur Ionisierung sowie damit versehene Gasdetektionsvorrichtung
GB2481883A (en) * 2010-06-08 2012-01-11 Micromass Ltd A mass spectrometer comprising a beam expander and a TOF mass analyser
CN109916510A (zh) * 2017-12-13 2019-06-21 中国科学院大连化学物理研究所 基于飞行时间谱真空紫外光横向分布在线测量装置及方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114994162B (zh) * 2022-06-01 2023-07-18 浙江大学 基于液滴辅助电离技术的气溶胶化学组分测量系统和方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999045362A1 (fr) * 1998-03-05 1999-09-10 Aerodyne Research, Inc. Analyseur de particules atmospheriques

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4383171A (en) * 1980-11-17 1983-05-10 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Particle analyzing method and apparatus
US5631462A (en) * 1995-01-17 1997-05-20 Lucent Technologies Inc. Laser-assisted particle analysis

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999045362A1 (fr) * 1998-03-05 1999-09-10 Aerodyne Research, Inc. Analyseur de particules atmospheriques

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
COPLEY, JRD, UDOVIC TJ: "Neutron time-of-flight spectroscopy", J. RES. NATL. INST. STAND. TECHNOL., vol. 98, no. 1, 1 January 1993 (1993-01-01) - 28 February 1993 (1993-02-28), Gaithersburg, pages 71q - 87 *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004025841A1 (de) * 2004-05-24 2005-12-15 Bergische Universität Wuppertal Verfahren und Vorrichtung zur massenspektroskopischen Untersuchung von Analyten
DE102004025841B4 (de) * 2004-05-24 2015-07-09 Bruker Daltonik Gmbh Verfahren und Vorrichtung zur massenspektroskopischen Untersuchung von Analyten
DE102008035773A1 (de) * 2008-07-31 2010-02-04 Eads Deutschland Gmbh Verfahren und Vorrichtung zur Ionisierung sowie damit versehene Gasdetektionsvorrichtung
GB2481883A (en) * 2010-06-08 2012-01-11 Micromass Ltd A mass spectrometer comprising a beam expander and a TOF mass analyser
GB2491305A (en) * 2010-06-08 2012-11-28 Micromass Ltd A mass spectrometer arranged to analyze positive and negative ions
GB2491305B (en) * 2010-06-08 2014-05-21 Micromass Ltd Mass spectrometer with beam expander
US8895920B2 (en) 2010-06-08 2014-11-25 Micromass Uk Limited Mass spectrometer with beam expander
US8916820B2 (en) 2010-06-08 2014-12-23 Micromass Uk Limited Mass spectrometer with beam expander
GB2481883B (en) * 2010-06-08 2015-03-04 Micromass Ltd Mass spectrometer with beam expander
US9053918B2 (en) 2010-06-08 2015-06-09 Micromass Uk Limited Mass spectrometer with beam expander
US9245728B2 (en) 2010-06-08 2016-01-26 Micromass Uk Limited Mass spectrometer with beam expander
CN109916510A (zh) * 2017-12-13 2019-06-21 中国科学院大连化学物理研究所 基于飞行时间谱真空紫外光横向分布在线测量装置及方法

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Publication number Publication date
DE10132735A1 (de) 2003-01-23
EP1274117A3 (fr) 2006-01-25

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