EP3118886A1 - Spectromètre de masse et procédé de spectrométrie de masse - Google Patents
Spectromètre de masse et procédé de spectrométrie de masse Download PDFInfo
- Publication number
- EP3118886A1 EP3118886A1 EP15177079.9A EP15177079A EP3118886A1 EP 3118886 A1 EP3118886 A1 EP 3118886A1 EP 15177079 A EP15177079 A EP 15177079A EP 3118886 A1 EP3118886 A1 EP 3118886A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- hollow body
- vacuum
- vacuum chamber
- spectrometer
- 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.)
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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
- H01J49/10—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
-
- 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 is aimed to in situ analysis of complex gaseous samples using optical means.
- the invention is directed to a mass spectrometer device capable to work without the isolation of the sample from the surrounding medium, and a method for mass spectrometry that uses the said mass spectrometer.
- laser filamentation can be considered a paradigm that clearly gathers both interests mentioned before. Filamentation has its origin in the balance between two different phenomena: self focusing of the laser pulse when it propagates through a possitive Kerr medium and defocusing due to the properties of the plasma created by the concentration of energy in space and time. It was not until the development of intense femtosecond pulsed lasers that filamentation was observed in the atmosphere. Laser filaments have some applications like the control of lighting and rainfalls, the guiding of high power microwaves using the ionization channel created by the filament, or the remote sensing of pollutants in air using molecular fluorescence and LIDAR (Laser Illuminated Detection And Ranging).
- LIDAR Laser Illuminated Detection And Ranging
- a mass spectrometer is provided, more specifically a TOF (Time of Flight) spectrometer.
- TOF Time of Flight
- the ionization process and the detection of the ionized particles take place in high vacuum conditions. This is so because on one hand the most usual ionization techniques in this field like electron impact ionization have low efficiency, being this proportional to the vacuum level. On the other hand the typical ions detectors require high vacuum conditions for their correct operation.
- the ionization is produced by a laser. In this way a much higher ionization yield is obtained making it possible to work at atmospheric pressure.
- the use of lasers allows a possible selective ionization of a certain species from a complex sample. Another advantage is the possibility to study a sample without isolating it from the surrounding medium. This is extremely important for different applications like the biological ones.
- a second aspect of the invention embraces a spectrometry method using the spectrometer of the first aspect of the invention.
- an ionization source is provided.
- Said ionization source must fulfil the requirement of providing at least 10 9 W / cm 2 ; in a preferred embodiment of the second aspect of the invention the ionization source is a laser system.
- the spectrometer of the invention is able to work at atmospheric pressure conditions and, in a preferred embodiment, it comprises a preferably cylinder shaped vacuum chamber which provides the required differential vacuum between the atmospheric pressure of the ionization region and the body of the spectrometer.
- the spectrometer comprises at least two, preferably cylinder shaped; vacuum chambers that means two stages of differential vacuum.
- a high vacuum chamber and a low vacuum chamber are provided.
- the vacuum chambers are respectively connected to vacuum systems and when more than one vacuum chamber is provided they are duly separated by pierced vacuum membranes (pierced standing for provided with an orifice for differential vacuum).
- a second pierced vacuum membrane is also provided with an orifice for differential vacuum, said second vacuum membrane being provided as a closing wall of the low vacuum chamber whilst the high vacuum chamber is closed by a base comprising a charged particles detector.
- a repeller for positive ions is provided opposite to the second vacuum membrane and separated thereof by a distance defining a passage through which the laser beam will flow; being a portion of said passage, that closer to the repeller, the ionization region under a pressure of 1013 mbar approximately, namely at atmospheric conditions.
- Said repeller may be a plate at a positive high voltage, which drives the ionized particles inside the hollow body into the detection region.
- the detection region is separated from the ionization region by one or several orifices, those of the membranes that allow differential pumping. This is of critical importance because charged particle detectors need to operate in high vacuum conditions.
- electrostatic lenses can be also incorporated. These spectrometer electrostatic lenses are arranged inside the vacuum chamber, although their exact position will depend on their number and the applied voltages, nonetheless and regardless of their position, said electrostatic lenses may have voltages in the range of hundreds of Volts.
- a mass spectrometer (1) depicted in figure 1 where it is shown the hollow body (2) of the mass spectrometer (1) with a vacuum chamber (3, 31, 32) therein.
- said vacuum chamber (3, 31, 32) is defined by a base (21), which comprises a charged particle detector (22) arranged at distal end of the hollow body (21), the inner wall of the hollow body (2) and a vacuum membrane (23) provided with a first pinhole (231) and arranged at the proximal end of the hollow body (2).
- the vacuum chamber (3, 31, 32) is connected to a vacuum generation system by means of at least one orifice (5, 51, 52).
- a repeller (4) is arranged opposite to the vacuum membrane (23) at a distance thereof defining a passage through which a laser beam will flow generating a plasma producing ions, as depicted either in figure 1 or 2 .
- the mass spectrometer (1) comprises more than one vacuum chamber (3), for example, and not being a limitative number, two.
- This is achieved by adding separation elements, like equipping the hollow body (2) with at least an additional vacuum membrane (24) which is provided with a second pinhole and arranged inside the hollow body (2) so that said additional vacuum membrane (24) splits the vacuum chamber (3) into a high vacuum chamber (31) and a low vacuum chamber (32); hence the high vacuum chamber (31) is defined by the base (21), which comprises a charged particle detector (22) arranged at distal end of the hollow body (21), the inner wall of the hollow body (2) and the additional vacuum membrane (24), whereas the low vacuum chamber (32) is defined by the additional vacuum membrane (24) which is pinholed, the inner wall of the hollow body (2) and the vacuum membrane (23).
- the mass spectrometer of either the preferred or the alternative embodiment earlier described may be furnished with one or more electrostatic lenses inside the hollow body (2) for guiding electrons throught the hollow body (2), said electrostatic lenses are meant to be charged with a voltage up to 100 Volts.
- a second aspect of the invention is that of a mass spectrometry method using the mass spectrometer (1) of the first aspect of the invention.
- a possible ionization source (5) may be one of the three different exits, with peak powers of 20 TW, 200 TW and 1 PW respectively, of a Ti-Saphire laser system.
- the used 200 TW exit delivers pulses of 30 fs, up to 6 J of energy per pulse, 800 nm of central wavelength, a beam diameter of 10 cm, and a repetition rate of 10 Hz was used.
- an attenuation of the energy per pulse to 30 mJ could be made in order to work at atmospheric pressure conditions after laser compression.
- any ionization system providing sufficient intensity may be used as an ionization source (5), for example: an 800 nm wavelength laser beam with a cross section of 3 cm of diameter, delivering pulses of 120 fs with a repetition rate of 1 kHz being the energy per pulse of 2.2 mJ, furnished with a 50 cm focal lens.
- the laser pulses generated were focused by the combination of a spherical mirror and a plano-convex lens with focal lengths of 1 m and 20 cm respectively.
- the effective focal length of the whole system was 28 cm.
- a filament (61) is created in the vicinity of the focal plane.
- Any other focalization system that provides the required peak intensity (larger than 10 9 W/cm 2 ) can be used.
- This invention was designed and constructed in order to have access to the plasma dynamics and the different species generated once the laser-matter interaction ceased.
- the interaction region at atmospheric pressure, and the body (2) of the spectrometer (1) at a vacuum level lower than 10 -4 mbar are separated by a first pinhole (231) with diameter in the order of tens of microns, and a thickness of around 10 microns.
- the ions generated in an ionization zone (61) generated by the ionization source (6) are directed towards the first pinhole (231) by the repeller (4) plate at a positive voltage of the order of 1kV.
- the ionization zone (61), directed from the ionization source (6), is separated at a distance comprised between 0.5 mm and 20 mm from first pinhole (231) and a distance comprised between 0.5 mm and 10 cm from the repeller (4).
- the ions Once the ions enter in the spectrometer (1) they travel freely, i.e., there are no further acceleration stages, towards the charged particle detector (22). To avoid a charge accumulation in the body of the spectrometer (1), the outer structure must be properly connected to ground. The signal from the charged particle detector (22) is collected and integrated in an oscilloscope triggered by the laser.
- the integration time was approximately five minutes due to the small size of the first pinhole (231) and the low repetition rate of the laser.
- a larger first pinhole (231), with sizes up to 25 microns may be used, although a larger first pinhole (231) would make measurements faster, it would decrease the vacuum level to a non-safe value for the correct function of the spectrometer (1), producing unwanted sparks in the charged particle detector (22) that would ruin any useful data, and could risk the integrity of the detector.
- new steps of differential vacuum must be added to the spectrometer or to correctly remodel the vacuum pumping system.
- the alignment of the ionization zone (61) with respect to the first pinhole (231) was carried out maximizing the UV light detected by the the charged particle detector (22) of the spectrometer (1), which is a MCP that is sensitive to UV, at time zero.
- the ionization zone (61) is arranged at a distance comprised between 0.5 mm and 20 mm from the pinhole of the second vacuum membrane (24) and at a distance comprised between 0.5 mm and 10 cm to the repeller (4).
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Electron Tubes For Measurement (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP15177079.9A EP3118886A1 (fr) | 2015-07-16 | 2015-07-16 | Spectromètre de masse et procédé de spectrométrie de masse |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP15177079.9A EP3118886A1 (fr) | 2015-07-16 | 2015-07-16 | Spectromètre de masse et procédé de spectrométrie de masse |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP3118886A1 true EP3118886A1 (fr) | 2017-01-18 |
Family
ID=53673804
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP15177079.9A Withdrawn EP3118886A1 (fr) | 2015-07-16 | 2015-07-16 | Spectromètre de masse et procédé de spectrométrie de masse |
Country Status (1)
| Country | Link |
|---|---|
| EP (1) | EP3118886A1 (fr) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1726945A1 (fr) * | 2004-03-16 | 2006-11-29 | Kabushiki Kaisha IDX Technologies | Spectroscope de masse a ionisation laser |
| US20070075240A1 (en) * | 2004-02-23 | 2007-04-05 | Gemio Technologies, Inc. | Methods and apparatus for ion sources, ion control and ion measurement for macromolecules |
| US20150008313A1 (en) * | 2011-12-29 | 2015-01-08 | Dh Technologies Development Pte. Ltd. | Ionization with femtosecond lasers at elevated pressure |
-
2015
- 2015-07-16 EP EP15177079.9A patent/EP3118886A1/fr not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070075240A1 (en) * | 2004-02-23 | 2007-04-05 | Gemio Technologies, Inc. | Methods and apparatus for ion sources, ion control and ion measurement for macromolecules |
| EP1726945A1 (fr) * | 2004-03-16 | 2006-11-29 | Kabushiki Kaisha IDX Technologies | Spectroscope de masse a ionisation laser |
| US20150008313A1 (en) * | 2011-12-29 | 2015-01-08 | Dh Technologies Development Pte. Ltd. | Ionization with femtosecond lasers at elevated pressure |
Non-Patent Citations (8)
| Title |
|---|
| A PERALTA CONDE ET AL: "An initial study on atmospheric pressure ion transport by laser ionization and electrostatic fields", 24 October 2014 (2014-10-24), pages 1 - 11, XP055222928, Retrieved from the Internet <URL:http://oa.upm.es/32321/1/AN%20INITIAL%20STUDY%20ON%20ATMOSPHERIC.pdf> [retrieved on 20151022] * |
| A PERALTA CONDE ET AL: "An initial study on atmospheric pressure ion transport by laser ionization and electrostatic fields", 24 October 2014 (2014-10-24), pages 1 - 11, XP055222930, Retrieved from the Internet <URL:http://oa.upm.es/32321/1/AN INITIAL STUDY ON ATMOSPHERIC.pdf> [retrieved on 20151022] * |
| A. TALEBPOUR; M. ABDEL-FATTAH; A. D. BANDRAUK; S.L. CHIN, LASER PHYS., vol. 11, no. 1, 2001, pages 68 - 76 |
| J. H. ODHNER; D. A. ROMANOV; R. J. LEVIS, PHYS. REV. LETT., vol. 103, 2009, pages 075005 |
| M. PLEWICKI; R. J. LEVIS, J. OPT. SOC. AM., vol. B 25, 2008, pages 1714 |
| MULLEN C ET AL: "Femtosecond Laser Photoionization Time-of-Flight Mass Spectrometry of Nitro-aromatic Explosives and Explosives Related Compounds", JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY, ELSEVIER SCIENCE INC, US, vol. 20, no. 3, 1 March 2009 (2009-03-01), pages 419 - 429, XP025990439, ISSN: 1044-0305, [retrieved on 20081106], DOI: 10.1016/J.JASMS.2008.10.022 * |
| OSER H ET AL: "DEVELOPMENT OF A JET-REMPI (RESONANTLY ENHANCED MULTIPHOTON IONIZATION) CONTINUOUS MONITOR FOR ENVIRONMENTAL APPLICATIONS", APPLIED OPTICS, OPTICAL SOCIETY OF AMERICA, WASHINGTON, DC; US, vol. 40, no. 6, 20 February 2001 (2001-02-20), pages 859 - 865, XP001017735, ISSN: 0003-6935, DOI: 10.1364/AO.40.000859 * |
| ROBERT J. LEVIS ET AL: "Photoexcitation, Ionization, and Dissociation of Molecules Using Intense Near-Infrared Radiation of Femtosecond Duration", JOURNAL OF PHYSICAL CHEMISTRY. A, MOLECULES, SPECTROSCOPY,KINETICS, ENVIRONMENT AND GENERAL THEORY, vol. 103, no. 33, 1 August 1999 (1999-08-01), US, pages 6493 - 6507, XP055223054, ISSN: 1089-5639, DOI: 10.1021/jp984543v * |
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