WO2013002683A1 - Analyseur de masse d'ions statique - Google Patents

Analyseur de masse d'ions statique Download PDF

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Publication number
WO2013002683A1
WO2013002683A1 PCT/RU2012/000550 RU2012000550W WO2013002683A1 WO 2013002683 A1 WO2013002683 A1 WO 2013002683A1 RU 2012000550 W RU2012000550 W RU 2012000550W WO 2013002683 A1 WO2013002683 A1 WO 2013002683A1
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sector
energy
plane
ion
mass analyzer
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PCT/RU2012/000550
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English (en)
Russian (ru)
Inventor
Вячеслав Данилович САЧЕНКО
Original Assignee
Sachenko Viacheslav Danilovich
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Publication of WO2013002683A1 publication Critical patent/WO2013002683A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/28—Static spectrometers
    • H01J49/32—Static spectrometers using double focusing

Definitions

  • the invention relates to analytical instrumentation, and in particular to static instruments and devices for analyzing the mass spectral composition of substances.
  • Static ion mass analyzers are based on the principle of spatial separation of ions by momenta in the static magnetic sector (MS), where each monopulse ion group has its own optical axis.
  • MS static magnetic sector
  • the optical axes of monopulse groups are arcs of circles, the radii of which, in the case of an insignificant spread of ion energies, depend on their mass, which makes it possible to carry out a precision mass analysis of ions .
  • the resolving power of SMA deteriorates due to 1st order chromatic aberration (MS energy dispersion).
  • Known single-focus mass spectrometer with dual focusing see patent US 4766314, IPC H01J 49/32, publ. 08.23.1988, including an ion source (AI), a focusing system (FS), an exit slit (VSC), which object slit (OS) of the mass analyzer, aperture diaphragm (HELL), sequentially arranged static magnetic sector (MS), an intermediate electrostatic lens (EL) for electrical adjustment of the spectrometer, electrostatic sector (ES) and a single-collector mass spectrum detector .
  • the ES is set relative to the MS in such a way that the direction of rotation of its optical axis in the ES is preserved in the MS.
  • the well-known mass spectrometer does not allow simultaneously recording the entire mass spectrum or its part, which is due to both the order of the MS and the ES (the ES is installed behind the MS) and the fact that double focusing takes place only for one monomass ion group, which is deduced by the parameter sweeps to a fixed axial orbit a priori.
  • the detection of the lines of the mass spectrum is carried out by varying the sweep parameter with the consequent orbiting of all monomass ion groups into the orbit and registration of the mass spectrum by a single-collector detector, which is associated with a low mass spectrometer performance.
  • the disadvantages of the known mass spectrometer are its low resolution and low productivity due to the single-collector method for detecting the mass spectrum.
  • Known tandem mass spectrometer type MS / MS the second stage of which is made in the form of a two-stage dual focusing SMA (see patent US 4866267, IPC H0U 49/32, published 08.23.1988), including a source of "daughter” ions from the selected at the first stage of the mass spectrometer of monomass “parent” ions, and sequentially arranged Wien filter, MS and a spatially extended detector (PPD) of daughter ions.
  • PPD spatially extended detector
  • a disadvantage of the known mass spectrometer is that double focusing over the range of orbits of the detected ions takes place only in a narrow range of approximately equal initial velocities, which accounts for the relatively narrow scope of this analogue.
  • a multi-collector mass spectrometer must a) provide double focusing for all registered monomass groups of ions simultaneously, b) ensure equality of rotation angles optical axes of monomass ion groups in the MS, c) have a straight line of the focus lines of the MS.
  • the specified conditions are satisfied by the Mattauch-Herzog type MCA, in which the ES and MS are located in the S-scheme, the object gap (OS) is located in the front focal plane of the ES, and the geometric place of the optical foci of the MS forms a straight line.
  • Mattau-Herzog (MG) type SMA is the design of the MC made by a two-pole with a constant gap between the pole pieces, the output boundary of which is flat, made in such a way that the effective boundaries of the magnetic field and the input optical axis intersect at one point .
  • This special construction first described by Mattauch and Herzog (CMJ. Mattauch and RJ, Herzog. - Phys., 89, p. 789.1934, J. Mattauch and RJ, Herzog), ensures that the ion rotation angle in the MS field is independent of their mass .
  • the indicated construction will be called below the “MG construction”. Practically all SMAs made according to the Mattauch-Herzog type include MC structures of the MG in their composition.
  • a multi-collector magnetic mass spectrometer with double focusing is known, the MCA of which is made according to the Mattauch-Herzog type (see High-performance mass spectrometer with double focus. Instruments for scientific research, N? 2, pp. 37-44, 1985, A. O. Nir et al.), Including AI, FS, OSh, ES in the form of a sector of a cylindrical capacitor, MS of the MG design and a multi-collector detector, the receiving slits of which are installed along the focal line of the MS.
  • a disadvantage of the known mass spectrometer is its low resolution under conditions of significant energy dispersion of ions.
  • a multi-collector magnetic mass spectrometer with double focusing is known, the MCA of which is made according to the Mattauh-Herzog geometry (see Development of a miniaturized gas chromatograph-mass spectrometer with a microbore capillary columns and array detector. Analytical Chemistry, vol. 63, No. 18, p.2012-2016,1991, MP Sinha et al.), Including AI, FS, OSh, ES in the form of a sector of a cylindrical capacitor, MS design MG, electro-optical detector with a microchannel plate, installed along the focal line of the MS, and an automated mass spectrometer control system.
  • SMA static mass analyzer of ions with double focusing
  • IPC N IPC N (49/26, published June 20, 2004)
  • SMA is made according to the geometry of Mattauch -Herzog and includes AI, FS, OSh, aperture diaphragm, energy dispersive electrostatic sector (ES) and magnetic sector (MS) in the form of a bipolar magnet with a constant gap between the poles.
  • the ES is made in the form of a sector of a cylindrical capacitor.
  • the SMA also includes a system for simultaneously recording mass spectral lines in the form of a multi-collector detector, the receiving slits of which are installed along the line of the MS foci, a mass spectrometer control system and an automated computer-based data collection system for cyclically recording and storing mass spectra.
  • the disadvantage of the prototype is the lack of an ion-beam energy filtration system and the fundamental impossibility of its installation, which significantly limits the level of resolution of the prototype in conditions where the ion beam to be mass spectrally analyzed is not uniform in energy.
  • An object of the present invention is to increase the resolving power of SMA in the mode of simultaneous recording of the ion mass spectrum under conditions of an ion beam that is not uniform in energy.
  • the static mass analyzer of ions includes an ion source (AI), a focusing system, an object slit, an aperture diaphragm, an energy dispersive electrostatic sector (ES), and a magnetic sector (MS) in the form of a bipolar magnet with a constant gap between the poles, and a system for the simultaneous registration of mass spectral lines.
  • the output boundary of the MS is flat and made in such a way that the effective boundaries of the magnetic field and the input optical axis intersect at one point.
  • the ES is set relative to the MS so that the directions of rotation of the optical axes in the ES and the MS coincide, and relative to the AI so that the plane of the optical image OS is located between ES and MS.
  • An energy-filtering diaphragm (ED) is installed in the plane of the optical image of the OS.
  • a collimating lens (CR) is installed between the ED and the MS, the front focal plane of which is located in the ED plane at the CL optical power ; satisfying the ratio:
  • P L is the optical power of the CL, mm "1 ;
  • D e is the dispersion coefficient for ES energy in the ED plane, mm;
  • C m is the dimensionless coefficient determined by the design of the magnetic sector, numerically equal to the product of the mass dispersion coefficient and the optical power of the MS, the same for all axial orbits of monomass ion groups in the MS field.
  • a system for simultaneously recording mass spectral lines can be implemented as a multi-collector ion detector with electrical registration of ion currents, receiving slits of which are installed in the focal planes of the MS corresponding to the axial orbits of the recorded monomass components of the ion beam.
  • the system for simultaneously recording mass spectral lines can be made in the form of a spatially extended detector, the receiving surface of which is mounted on the focal line of the static mass analyzer.
  • At least one lens can be installed between the object gap and the ES for the electrical adjustment of the SMA.
  • ES can be made in the form of a sector of an electrostatic capacitor with an equipotential optical axis, angle ⁇ ⁇ and radius r e of rotation of the optical axis, axial radius a e of curvature of its equipotential, and set at a distance L 'from OS to ES and at a distance L " from ES 5 to ED 10, the values of which are related to the coefficient D e of the energy dispersion of ES 5, as it is easy to show, with a parametric dependence:
  • the ES and MS are installed according to the C-scheme, which allows focusing of ions according to the angular spread between the ES and MS and installing the ED in front of the MS.
  • the ES is installed relative to the AI in such a way that an optical image of the SMA object slit is formed between the ES and the MS (in the prototype, the ES is installed relative to the AI so that the exit slit of the AI is located in the front focal plane of the ES); in the plane of the intermediate image of the OS is installed ED; a CR was installed in front of the MS, the design and position of which with respect to the ED was calculated so that its front focal plane is located in the ED plane at the optical power of the CR depending on the dispersion coefficient of the ES in the ED plane according to the equality
  • P L is the optical power of CL
  • D e is the dispersion coefficient for ES energy in the ED plane, mm;
  • C m is the dimensionless coefficient determined by the design of the magnetic sector, numerically equal to the product of the mass dispersion coefficient and the optical power of the MS, the same for all axial orbits of monomass ion groups in the MS field.
  • the problem is solved within the framework of C-schemes, since they create conditions for double focusing of ions while ensuring their intermediate focusing (due to opposite signs of the dispersion coefficients of ES and MS), and it is possible to set the ED.
  • a mass spectrometric mode receiving slot mnogokollektor- Nogo detector should be installed at the focal planes of the MS, The corresponding axial orbits monomassovyh groups of ions; in the mass spectrographic mode of the MCA using a spatially extended detector (PDD), the receiving surface of the PDA should be located on the focus line.
  • PDA spatially extended detector
  • the values of the dispersion coefficient of the MS and its optical power, therefore, and the coefficient C t in the right-hand side of (1) are uniquely determined MC structure (see G. Volnik. Optics of charged particles, Energoizdat, 1987).
  • the analysis shows that, in the case of the MG of the MG design, the specified coefficient is dimensionless, i.e. its value does not depend on the radius of the axial orbit of any monomass group.
  • Fig. 1 shows the optical part of the SMA prototype
  • Fig. 2 shows the CMA of the present invention.
  • ion source 1 exit slit 2
  • aperture diaphragm 3 optical axis 4 in the energy dispersive electrostatic sector (ES)
  • optical axis b in the energy dispersive magnetic sector (MS) 7 having an input boundary of 8 and output boundary 9 (effective boundaries of the magnetic field MS 7 are indicated).
  • ion source 1 exit slit 2
  • aperture diaphragm 3 optical axis 4 in the energy dispersive electrostatic sector (ES) 5
  • optical axis b in the dispersive energy magnetic sector (MS) 7 having an input boundary of 8 and an output boundary of 9 (the effective boundaries of the magnetic field of MS 7 are indicated)
  • the SMA prototype (see Fig. 1) is made according to the Mattauch-Herzog geometry.
  • the exit slit 2, in the plane of which the focusing system (not shown) of the ion source 1 focuses the ion beam, is located in the front focal plane of ES 5.
  • the directions of rotation of the optical axis 4 in ES 5 and optical axis b in MS 7 are opposite (S diagram).
  • MS 7 is made according to the MG design, according to which the output boundary 9 intersects the optical axis b and the input boundary 8 at point 12.
  • the ion beam formed in the source 1 is focused on the plane of the output slit 2 by a focusing system (not shown), is limited according to the size of the exit slit 2 and the divergence angle of the aperture diaphragm 3, then near the axis 4 ions follow in the direction of the electrostatic sector 5, where they are spatially separated by energy.
  • ions move in the direction of MS 7, enter it through border 8, exit from it through rectilinear border 9, being separated by mass and assembled into monomass groups moving near the corresponding axial orbits 13.
  • axial orbits 13 are shown, corresponding to three lines of the mass spectrum .
  • each monomassic group of ions is focused at points designated, respectively, Di, D 2 , D 3 , which form a focus line 14, on which, for example, a microchannel plate of a spatially extended detector (PPD) can be mounted or receiving slots of a multi-collector detector (not shown in the drawing).
  • PPD spatially extended detector
  • ED 10 is installed in the plane of the optical image of slit 2
  • CL 11 is installed so that the plane its front focus with optical power CR, corresponding to equation (1), is located in the plane of ED 10.
  • ES 5 and MS 7 are installed according to the C-scheme.
  • MS 7 is made by the design of MG similarly to Fig. 1.
  • the input boundary 8 is non-orthogonal to the optical axis and is located at an angle ⁇ to the normal to the boundary, which ensures that the focus line is removed from the output boundary 9.
  • the ion beam formed in AI 1 focuses on the plane of the exit slit 2 by the focusing system (in Fig. .2), is limited by the size of the exit slit 2 and by the divergence angle of the aperture diaphragm 3, then near the axis 4 the ions follow in the direction of ES 5, where they are spatially separated into monoenergetic groups, each of which focuses in angular scatter in the plane ED 10. Ions passing through ED 10 are focused near point 15. Next, they follow the axis b in the direction of CR 11 and further, to MS 7, exit it, being formed into spatially separated monomass groups, move near the corresponding axial orbits 13.
  • each monomassic group of ions is focused at the corresponding points, denoted by Di, D 2 / D 3 , which form the focus line 14, on which, for example, a microchannel plate PPD (mass spectrograph mode) or receiving slots of a multi-collector detector (multi-collector mass spectrometer).
  • Di denoted by Di, D 2 / D 3 , which form the focus line 14, on which, for example, a microchannel plate PPD (mass spectrograph mode) or receiving slots of a multi-collector detector (multi-collector mass spectrometer).
  • An electrostatic lens or a lens system (not shown in Fig. 2) can be installed between AI 1 and ES 5 to enable the electrical adjustment of the mass spectral resolution of the SMA.
  • ES 5 can be made in the form of a sector of an electrostatic capacitor with an equipotential optical axis, angle ⁇ ⁇ and radius r e of rotation of the optical axis, the axial radius a e of curvature of its equipotential, and is set to the distance L 'from OSH to ES and at a distance L "from ES 5 to ED 10, the values of which are associated with the coefficient D e of the energy dispersion of ES 5 with a parametric dependence:

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

Un analyseur d'ions de masse statique comprend une source d'ions (1), un système de mise au point, une fente pour objet (2), un diaphragme à ouverture (3), un secteur électrostatique (5) et un secteur magnétique (7) à dispersion d'énergie. Le secteur électrostatique (5) est monté par rapport au secteur magnétique (7) de manière à ce que le sens de rotation des axes optiques (4), (6) dans le secteur électrostatique (5) et le secteur magnétique (7) coïncident. Le secteur électrostatique (5) est monté par rapport à la source d'ions (1) de manière à ce que le plan de l'image optique de la fente pour objet (2) se situe entre le secteur électrostatique (5) et le secteur magnétique (7). Dans le plan de l'image optique de la fente pour objet (2) on a monté un diaphragme à filtrage d'énergie (10). Entre le secteur électrostatique (5) et le secteur magnétique (7) on a monté une lentille de collimation (11). L'analyseur d'ions en masse statique possède une résolution plus élevée dans un mode d'enregistrement simultané de spectre d'ions pour un faisceau d'énergie d'ions inégal en termes d'énergie.
PCT/RU2012/000550 2011-06-30 2012-06-29 Analyseur de masse d'ions statique WO2013002683A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2011128285 2011-06-30
RU2011128285/07A RU2456700C1 (ru) 2011-06-30 2011-06-30 Статический масс-анализатор ионов

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WO2013002683A1 true WO2013002683A1 (fr) 2013-01-03

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Publication number Priority date Publication date Assignee Title
RU2533383C1 (ru) * 2013-06-06 2014-11-20 Вячеслав Иванович Козловский Способ разделения заряженных частиц по удельному заряду
WO2015057042A2 (fr) * 2013-10-18 2015-04-23 Алдан Асанович САПАРГАЛИЕВ Spectromètre de masse et éléments pour celui-ci

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4300044A (en) * 1980-05-07 1981-11-10 Iribarne Julio V Method and apparatus for the analysis of chemical compounds in aqueous solution by mass spectroscopy of evaporating ions
EP0475674A2 (fr) * 1990-09-07 1992-03-18 FISONS plc Méthode et dispositif pour la spectrométrie de masse
RU2017143C1 (ru) * 1991-04-23 1994-07-30 Физико-технический институт им.А.Ф.Иоффе РАН Способ определения элементарного состава твердого тела
RU2231165C2 (ru) * 2002-03-04 2004-06-20 Трошков Михаил Львович Многоколлекторный магнитный масс-спектрометр

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4423324A (en) * 1977-04-22 1983-12-27 Finnigan Corporation Apparatus for detecting negative ions

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4300044A (en) * 1980-05-07 1981-11-10 Iribarne Julio V Method and apparatus for the analysis of chemical compounds in aqueous solution by mass spectroscopy of evaporating ions
EP0475674A2 (fr) * 1990-09-07 1992-03-18 FISONS plc Méthode et dispositif pour la spectrométrie de masse
RU2017143C1 (ru) * 1991-04-23 1994-07-30 Физико-технический институт им.А.Ф.Иоффе РАН Способ определения элементарного состава твердого тела
RU2231165C2 (ru) * 2002-03-04 2004-06-20 Трошков Михаил Львович Многоколлекторный магнитный масс-спектрометр

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