EP2406811A1 - Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant - Google Patents
Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondantInfo
- Publication number
- EP2406811A1 EP2406811A1 EP10714937A EP10714937A EP2406811A1 EP 2406811 A1 EP2406811 A1 EP 2406811A1 EP 10714937 A EP10714937 A EP 10714937A EP 10714937 A EP10714937 A EP 10714937A EP 2406811 A1 EP2406811 A1 EP 2406811A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- ionization
- filament
- slot
- cage
- ionization cell
- 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.)
- Granted
Links
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000010894 electron beam technology Methods 0.000 claims abstract description 12
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 5
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 2
- 229910003452 thorium oxide Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims 1
- 239000007789 gas Substances 0.000 description 16
- 239000000700 radioactive tracer Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 229910052741 iridium Inorganic materials 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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
- H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
- H01J49/147—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers with electrons, e.g. electron impact ionisation, electron attachment
Definitions
- the present invention relates to an ionization cell for a mass spectrometer.
- the invention applies to mass spectrometers in which an electric heating filament emits electrons.
- the invention also relates to a leak detector comprising the ionization cell.
- a gas sample is analyzed by bombarding the sample paj a stream of electrons, then moving the ionized particles thus obtained to differentiate them for example according to their trajectory.
- the mass spectrometers of leak detectors measure and thus quantify a gas . irace ⁇ r, such as helium.
- The. spect.rometr . es mass comprise for example an ionization cell comprising an ionization cage and an electric heating filament emits electrons.
- the molecules of the gas to be analyzed are bombarded by the electron beam and a large part of the molecules of the gas to be analyzed is converted into ionized particles, ionized particles are then accelerated by an electric field. They arrive 1 then in one. zone subject to a magnetic field, which has the property of deflecting the trajectories of the ionized particles into. function of their mass.
- the stream of ionized particles of the gas. tracer is proportional to the partial pressure of the gas. in . the installation ;, and its measurement makes it possible to know the value of the flow rate of the leak detected.
- some ionization cells In order to make the. In operation of the mass spectrometer, some ionization cells have two filaments. A first working filament is supplied to produce the electron beam and a second backup filament is to be powered in case of failure of the first working filament.
- the object of the invention is therefore to reduce the waiting time required for the ionization cell to be operational again during the passage of the first working filament defaiant to the second spare connection.
- the subject of the invention is an ionization cell for a mass spectrometer comprising: an ionization cage comprising a first and a second electron input slot and one side of which has an exit slot for the passage of ionized particles, a first working filament disposed opposite said first electron input slot, intended to be fed to produce an electron beam, and a second emergency filament arranged opposite said second slot electron input and to be fed in case of failure of the first working filament to produce the electron beam,.
- said second entry slit being disposed outside a front region located vis-à-vis said first input slot.
- the inventors have found with surprise that with this arrangement of the ionization cell, the second emergency filament is not altered by the first working filament in operation.
- the longitudinal axes of said first and said second entrance slots are substantially parallel to each other and parallel to an edge of said ionization cags.
- said first and said second input slots are arranged on opposite sides of said ionization cage.
- said first and said second entrance slots define a plane substantially parallel to the plane defined by the side containing the exit slot for i ⁇ passage of the ionized particles, the first and second ends of said first and said second entrance slots are contained in two pans respectively parallel to each other and parallel to a side face of the ionization cage, said second entrance slot is decaiée of the frontal region, both along an axis parallel to the longitudinal axis of said first slot of at an entrance and along an axis perpendicular to the longitudinal axis of said first entrance slit, said second entrance slit is disposed at a distance of at least one millimeter from the perimeter of the screw-faced frontal region.
- the first working filament and the second emergency filament comprise an iridium wire covered with a deposit oxide, the oxide deposit is a layer of yttrium oxide or thorium oxide.
- the invention also relates to a mass spectrometer leak detector comprising an ionization cell as described above.
- FIG. 1 is a schematic view of a leak detector
- FIG. 2 is a schematic view of elements of a mass spectrometer according to a first embodiment
- FIG. 3 is a schematic perspective view of a cage of ionization
- FIG. 4 is a schematic side view of an ionization cell
- FIG. G is a schematic perspective view of an ionization cell according to a second embodiment
- FIG. 6 is a schematic perspective view of an ionization cell according to a third embodiment.
- FIG. 7 is a schematic perspective view of an ionization cell according to a fourth embodiment
- - ia Figure 8 is a schematic perspective view of a cell of ionization according to a fifth embodiment.
- the identical elements bear the same reference numbers.
- FIG. 1 shows a mass spectrometer leak detector 1 with a tracer gas, such as rheium (He 3 or He 4 ) or hydrogen (H 2 ).
- a tracer gas such as rheium (He 3 or He 4 ) or hydrogen (H 2 ).
- Do the mass spectrometer 2 is connected to the suction of a secondary pump 3 whose delivery is connected to the suction of a primary pump 4 via a first isolation valve 5.
- gas 6, optionally containing the tracer gas revealing a leak are sucked into the intake of the secondary pump 3, 10 via a second isolation valve 7.
- Part of the gases to be analyzed 6 is then sampled by the spectrometer 2.
- the detector 1 may also include a pressure sensor 8 for determining the gas pressure at the connection line with the secondary pump 3, upstream of the second isolation valve 7.
- the magnetic deflection mass spectrometer 2 comprises an ionization cell 9 and means for deflecting and selecting the ionized particles 14a, 14b. 14c.
- the ionization cell 9 includes a cage ionization 10, box-shaped paralléî to divulgdiq ⁇ e having a first input slot 11 for passage of the electron beam 20 12.
- the ionization cell 9 also includes a first filament working 13 to form the electron beam 12 when it is powered.
- the first working filament 13 is arranged facing the first electron entry slot 1 1 of the ionization cage 10 so that a maximum of electrons enter the ionization cage 10.
- the ionization cell 9 thus makes it possible to ionize the gases to be analyzed 6 by bombarding them with the electron beam 12, obtaining a beam of ionized particles 14.
- the ionization cage 10 also has an outlet slot 15 on one side 16, which has a particular passivation of ⁇ 3 ionized 14a, 14b. 14c; formed in the cage In FIG. 2, the side 1.6 containing the exit slot 15 corresponds to the upper face of the ionization cage 10.
- the deflection and selection means comprise, for example, a means for generating an electric field (not shown) for accelerating the ionized particles 14a, 14b, 14c and means for generating a magnetic field (ho ⁇ shown) oriented substantially according to the arrow g, such as permanent magnets, to deflect the trajectory of the ionized particles 14a, 14b ,. 14c, according to radii of curvature Ra, Rb, Rc 1 function of the mass of the ionized particles.
- the beam of ionized particles 14, which contained ionized particles of different masses, is divided into several beams 14a, 14b, 14c, each beam containing only ionized particles of the same ratio m / e (ratio of the atomic mass of the particle on the number of electrons lost at the moment of ionization).
- the ionized particles of helium 14c are separated from the lighter ionized particles of hydrogen 14b whose radius of curvature Rb is smaller than the ionized particles heavier with nitrogen or oxygen 14c whose radius of curvature Rc is higher. great.
- the total pressure in the chamber of the mass spectrometer 2 must be kept below 10 -1 Pascal so that the trajectories of the electrons and the ionized particles are not disturbed by the residual molecules.
- the deflection and selection means may also comprise a triode electrode 17 for collecting the ionized particles 14a whose mass is higher than that of the tracer gas, as well as a diaphragm 18 for selecting the ionized particles of tracer gas 14c, and a braking electrode 19 for removing noise from other Ionized species.
- the leak detector 2 also has an acquisition chain including in particular a DC amplifier 20 downstream of a target 21 receiving the stream of ionized particles incident tracer gas 14c from the decelerating electrode 19 for transforming in electronic current.
- the ionization cell S further comprises a second back-up filament 22, intended to be powered in the event of failure of the first working filament 13 to produce an electronsis instead of the first working filament 13.
- the filament Relief 22 is disposed opposite a second entrance slit of éleclro ⁇ s disposed on one side of the ionization cage 10 (not visible in Figure 2).
- the ionization cell includes means for switching the power supply, making it possible selectively to power one of the two filaments in order to ensure the continuity of the work enabling it to. to switch the supply of the first working filament 13 to the second emergency filament 22 if the working filament 13 has a failure.
- the supply of the filaments 13. 22. is carried on the one hand by an electric current to carry the filament filament.
- the filaments 13, 22 are connected to a power supply 23a with a power of 14W at 3A.
- the filaments 13, 22 are supplied with voltage by a voltage supply 23b between 100V and 300V, connected to the filaments 13, 22 so that the potential of the ionization cage 10 is greater by at least 100V at the potential of enaque filament. 13, 22 (see Figure 2).
- the filaments 13, 22 may be in fi! of iridium covered with an oxide deposit.
- the oxide deposition is for example a layer of yttrium oxide (Y: Oa) or da thorium oxide (ThO 2).
- tungsten filaments 13, 22 are provided.
- the tungsten filaments have a very low operating life at low pressure of the order of 10 -1 Pascal, compared to the yttria iridium filaments.
- yttria iridium filaments have better resistance to air entrances.
- the filaments 13, 22 are for example fixed at their ends 24 in a respective ceramic support 25.
- Each ceramic holder 25 is mounted in the cell ionization 9 of spectrometer 2, so that the filaments 13, 22, are arranged vis-à-vis their respective input slot bones ionization cage 10.
- the second inlet slot 26 is disposed on one face of the ionization cage, outside a front region F of the ionization cage 10 opposite the first inlet slot 11.
- frontal region F corresponds to the projection on the opposite face of the surface of the entrance slit 11 along the normal to the containing plane Ia.
- the second emergency filament 22 is arranged facing the second entrance slot 26, and therefore in a peripheral region distinct from the frontal region F situated opposite the first entrance slot 11.
- the second entry slot 26 is for example disposed in a peripheral region defined by a perimeter P to the gap by a distance of at least one millimeter around the perimeter of the frontal region F located vis-à-vis the first entrance slot 11 ⁇ see for example ia Figure 3).
- the emergency filament 22 is not altered by the first working filament 13.
- the time required for the tilting of the filament is thus significantly reduced because the interactions between the first working filament and the second back-up filament are reduced.
- each entrance slot 11, 26 are designed according to the disposition of the deflection and selection means. Taking the exemplary embodiment of the mass spectrometer of FIG. 2, the longitudinal axes L and L 'of the first and second inlet slits 11, 26 are substantially parallel to each other, and parallel to an edge of the ionisation cage 10.
- horizontal plane (X, y) is defined by the plane containing the exit slot 15.
- the first and the second input slots 11, 26 are, for example, arranged on opposite faces 27, 28 of the ionization cage 10. There is then sufficient space on either side of the cage. ionization 10 to arrange the filaments 13. 22 and their respective supports 25.
- Figures 2 to 4 illustrate a first embodiment in which the first and second ends of the first and second entrance slots 11, 26 are contained in two planes respectively parallel to each other and parallel to a lateral face 28 of Ea. ionisation cage 10.
- the second relief filament 22 is disposed in a peripheral region located below a front region F located vis-à-vis the first entrance slot 11.
- FIG. 3 shows the second input window 26 in dotted lines on an opposite face 28 of the ionization cage 10, shifted below the front region F 1 located opposite the first slot of FIG. entry 11.
- FIG. 4 there is a dashed line, ie second emergency filament 22 facing a second entrance slot 26, offset from a frontal region located opposite the first input slot 1 1 of an opposite side of the cage 10 ionization.
- FIG. 5 illustrates a second embodiment of the ionization cage 10.
- the longitudinal axes L and U of the first and second input slots 11, 26 are substantially parallel to each other, and parallel to a horizontal edge of the ionization cage 10.
- the first and second inlet slots 11, 26 are disposed on opposite side faces 27, 28 of the ionization cage 10.
- the first and second entrance slots 11, 26 define a plane substantially parallel to the plane defined by the side 16 of the ionization cage 10, containing the exit slot 15 for the passage of the particles. ionized.
- FIG. 6 illustrates a third embodiment similar to the two preceding examples, for which the peripheral region containing the second input slot 26 is shifted by the front region JF, at the same time along an axis Y parallel to I : ax longitudinal L the first entrance slot 11 and along an axis Z perpendicular to the longitudinal axis L of the first entry slot 11.
- the second input slot 26 is disposed on the opposite face 28 and is offset both horizontally along the horizontal axis Y, and vertically along the vertical axis Z, of the front region F located 5 vi ⁇ -i-vis the first entered slot 1 1.
- the first and the second inlet slit 11 * 26 are disposed on the same face 27 of the ionization cage 10.
- Figure 8 thus illustrates a fifth embodiment in which the longitudinal axes L and LJ slits input 11, 26 are respectively parallel to the vertical axis Z.
- the inlet slots 11, 26 may be disposed on the faces
- the first and second ends of the first and the second inlet slots 11, 26 are, for example, contained in two planes respectively parallel to one another.
- the ionization cell 9 thus makes it possible to shift the second back-up filament 22 from the front region F in which the interactions can take place, so that the waiting time required for the tilting of the first working filament 13 to fail is second spare fiord 22 is reduced.
Landscapes
- Physics & Mathematics (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 Tubes For Measurement (AREA)
- Examining Or Testing Airtightness (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0901114A FR2943173B1 (fr) | 2009-03-11 | 2009-03-11 | Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant |
PCT/FR2010/050407 WO2010103235A1 (fr) | 2009-03-11 | 2010-03-10 | Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2406811A1 true EP2406811A1 (fr) | 2012-01-18 |
EP2406811B1 EP2406811B1 (fr) | 2017-11-08 |
Family
ID=41066492
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP10714937.9A Active EP2406811B1 (fr) | 2009-03-11 | 2010-03-10 | Cellule d'ionisation pour spectrometre de masse et detecteur de fuites correspondant |
Country Status (6)
Country | Link |
---|---|
US (1) | US8803104B2 (fr) |
EP (1) | EP2406811B1 (fr) |
JP (1) | JP5289589B2 (fr) |
CN (1) | CN102439686B (fr) |
FR (1) | FR2943173B1 (fr) |
WO (1) | WO2010103235A1 (fr) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9666422B2 (en) | 2013-08-30 | 2017-05-30 | Atonarp Inc. | Analyzer |
JP6320197B2 (ja) * | 2014-06-26 | 2018-05-09 | ヤマハファインテック株式会社 | イオン発生装置およびガス分析器 |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1516614A (fr) * | 1966-03-23 | 1968-03-08 | Varian Associates | Source d'ions à deux filaments pour spectromètre de masse |
GB1338213A (en) * | 1971-06-18 | 1973-11-21 | Scient Research Instr Corp | Dual mode chemical or electron impact ionization source for mass spectrometer |
JPS5719949A (en) * | 1980-07-09 | 1982-02-02 | Hitachi Ltd | Dual filament ion source |
JP2943226B2 (ja) * | 1990-03-29 | 1999-08-30 | 株式会社島津製作所 | ガスクロマトグラフ質量分析計のイオン源 |
JPH07169427A (ja) * | 1993-12-14 | 1995-07-04 | Nissin Electric Co Ltd | イオン源装置 |
US5600136A (en) * | 1995-06-07 | 1997-02-04 | Varian Associates, Inc. | Single potential ion source |
WO2001043160A1 (fr) * | 1999-12-10 | 2001-06-14 | Epion Corporation | Ionisateur pour formation de faisceau d'ions a amas gazeux |
US6686595B2 (en) * | 2002-06-26 | 2004-02-03 | Semequip Inc. | Electron impact ion source |
KR100505040B1 (ko) * | 2003-12-19 | 2005-07-29 | 삼성전자주식회사 | 이온 소스 및 이를 갖는 이온 주입 장치 |
US6974957B2 (en) * | 2004-02-18 | 2005-12-13 | Nanomat, Inc. | Ionization device for aerosol mass spectrometer and method of ionization |
US7173252B2 (en) * | 2004-10-25 | 2007-02-06 | Epion Corporation | Ionizer and method for gas-cluster ion-beam formation |
US7459677B2 (en) * | 2006-02-15 | 2008-12-02 | Varian, Inc. | Mass spectrometer for trace gas leak detection with suppression of undesired ions |
US7427751B2 (en) * | 2006-02-15 | 2008-09-23 | Varian, Inc. | High sensitivity slitless ion source mass spectrometer for trace gas leak detection |
-
2009
- 2009-03-11 FR FR0901114A patent/FR2943173B1/fr active Active
-
2010
- 2010-03-10 WO PCT/FR2010/050407 patent/WO2010103235A1/fr active Application Filing
- 2010-03-10 CN CN201080011241.6A patent/CN102439686B/zh active Active
- 2010-03-10 JP JP2011553494A patent/JP5289589B2/ja active Active
- 2010-03-10 US US13/255,383 patent/US8803104B2/en active Active
- 2010-03-10 EP EP10714937.9A patent/EP2406811B1/fr active Active
Non-Patent Citations (1)
Title |
---|
See references of WO2010103235A1 * |
Also Published As
Publication number | Publication date |
---|---|
CN102439686B (zh) | 2015-04-08 |
WO2010103235A1 (fr) | 2010-09-16 |
FR2943173B1 (fr) | 2016-03-18 |
US8803104B2 (en) | 2014-08-12 |
FR2943173A1 (fr) | 2010-09-17 |
JP2012520542A (ja) | 2012-09-06 |
EP2406811B1 (fr) | 2017-11-08 |
US20110315875A1 (en) | 2011-12-29 |
CN102439686A (zh) | 2012-05-02 |
WO2010103235A9 (fr) | 2010-11-18 |
JP5289589B2 (ja) | 2013-09-11 |
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