US20210175063A1 - Axial ci source - off-axis electron beam - Google Patents
Axial ci source - off-axis electron beam Download PDFInfo
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- US20210175063A1 US20210175063A1 US16/709,845 US201916709845A US2021175063A1 US 20210175063 A1 US20210175063 A1 US 20210175063A1 US 201916709845 A US201916709845 A US 201916709845A US 2021175063 A1 US2021175063 A1 US 2021175063A1
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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
- H01J49/14—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
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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
- H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
- H01J49/145—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using chemical ionisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/067—Ion lenses, apertures, skimmers
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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
Definitions
- the present disclosure generally relates to the field of mass spectrometry including axial chemical ionization sources with an off-axis electron beam.
- Mass spectrometry can be used to perform detailed analyses on samples. Furthermore, mass spectrometry can provide both qualitative (is compound X present in the sample) and quantitative (how much of compound X is present in the sample) data for a large number of compounds in a sample. These capabilities have been used for a wide variety of analyses, such as to test for drug use, determine pesticide residues in food, monitor water quality, and the like.
- Sensitivity of a mass spectrometer can be limited by the efficiency of the ion source, ion losses through the mass spectrometer and in the mass analyzer, and sensitivity of the detector.
- Increasing the efficiency of the ion source, the number of ions produced per unit sample or per unit time can significantly improve the detection limits of the mass spectrometer, enabling the detection of lower concentrations of compounds or the use of smaller amounts of sample.
- increasing the stability of the ion source, number of ions produced as a function of time is important for quantitative comparisons between runs and samples. As such, there is a need for improved ion sources.
- an ion source can include an electron generator, an ionization chamber, a magnetic field, and an ion optic.
- the electron generator can be configured to produce electrons.
- the ionization chamber can have an electron entrance aperture through a first wall, an ion exit aperture through a second wall, and an axis.
- the ionization chamber can be configured to produce ions.
- the magnetic field can be arranged to confine electrons in a beam directed through the electron entrance aperture, in a direction within 45 degrees of parallel to the axis, and towards a location displaced from the ion exit aperture.
- the ion optic can be configured to direct ions exiting the ion exit aperture in an ion beam along the axis.
- the ionization chamber can be configured to produce ions by chemical ionization.
- the location can be on the second wall.
- the electron beam can be parallel to the axis but offset from the ion beam in a direction orthogonal to the axis.
- the electron beam can intersect a line along the direction of the ion beam.
- the ionization chamber can further includes a recess on the second wall and displaced from the ion exit aperture, and the electron beam can be directed towards the recess.
- a mass spectrometer can include an ion source of the first aspect, and a mass analyzer.
- a method can include generating electrons; directing electrons in a beam through an electron entrance aperture through a first wall of an ionization chamber and towards a location displaced from an ion exit aperture through a second wall of the ionization chamber, and in a direction within 45 degrees of parallel to an axis of the ionization chamber; producing ions within the ionization chamber; and directing ions as a beam through the ion exit aperture and in a direction parallel to the axis of the ionization chamber.
- producing ions within the ionization chamber can include producing ions by chemical ionization.
- the location can be on the second wall.
- directing the electron beam can include directing the electron beam in a direction parallel to the axis but offset from the ion beam in a direction orthogonal to the axis.
- directing the electron beam can include directing the electron beam to intersect a line along the direction of the ion beam.
- directing the electron beam can include directing the electron beam towards a recess on the second wall of the ionization chamber and displaced from the ion exit aperture.
- an ion source can include an electron generator, an ionization chamber, a magnetic field, and an electron dispersive mechanism.
- the electron generator can be configured to produce electrons.
- the ionization chamber can have an electron entrance aperture through a first wall and an ion exit aperture through a second wall.
- the ionization chamber can be configured to produce ions.
- the magnetic field can be arranged to confine electrons in a beam directed through the electron entrance aperture.
- the electron dispersive mechanism can be configured to disperse the electrons within the ionization chamber.
- the ionization chamber can be configured to produce ions by chemical ionization.
- first wall and the second wall can be opposite from one another.
- the electron dispersive mechanism can include a magnetic shielding configured to reduce the magnetic fields within at least a portion of the ionization chamber.
- the electron dispersive mechanism can include one or more additional magnets oriented to disrupt the magnetic field within at least one part of the ionization chamber.
- the electron dispersive mechanism can include an electrostatic lens can be configured to direct electrons away from the ion exit aperture without substantially affecting the ion beam.
- a mass spectrometer can include an ion source of third aspect and a mass analyzer.
- a method can include generating electrons; directing electrons in a beam through an electron entrance aperture of an ionization chamber; dispersing the electrons within the ionization chamber; producing ions within the ionization chamber; and directing the ions as a beam through the ion exit aperture.
- producing ions within the ionization chamber can includes producing ions by chemical ionization.
- FIG. 1 is a block diagram of an exemplary mass spectrometry system, in accordance with various embodiments.
- FIGS. 2A and 2B are diagrams illustrating an exemplary ion source, in accordance with various embodiments.
- FIGS. 3A and 3B are diagrams illustrating simulations of electrons in an ion source, in accordance with various embodiments.
- FIG. 4 is a diagram illustrating simulations of electrons in an ion source with an off axis magnetic field, in accordance with various embodiments.
- FIGS. 5A and 5B are diagrams illustrating electron impact density at the ion exit aperture, in accordance with various embodiments.
- FIG. 6 is a diagram illustrating a simulation of electrons in an ion source with an off axis magnetic field and a pocket for the electron beam, in accordance with various embodiments.
- FIG. 7 is a diagram illustrating a simulation of electrons in an ion source with an off axis magnetic field and an extended ionization chamber, in accordance with various embodiments.
- FIG. 8 is a diagram illustrating electron impact density at the ion exit aperture, in accordance with various embodiments.
- FIG. 9 is a diagram illustrating a simulation of electrons in an ion source with an electron dispersive mechanism, in accordance with various embodiments.
- FIG. 10 is a diagram illustrating electron impact density at the ion exit aperture, in accordance with various embodiments.
- FIGS. 11 and 12 are a diagrams illustrating ion sources with off-axis electron sources, in accordance with various embodiments.
- FIG. 13 is a flow diagram illustrating an exemplary method of operating an ion source, in accordance with various embodiments.
- a “system” sets forth a set of components, real or abstract, comprising a whole where each component interacts with or is related to at least one other component within the whole.
- mass spectrometry platform 100 can include components as displayed in the block diagram of FIG. 1 . In various embodiments, elements of FIG. 1 can be incorporated into mass spectrometry platform 100 . According to various embodiments, mass spectrometer 100 can include an ion source 102 , a mass analyzer 104 , an ion detector 106 , and a controller 108 .
- the ion source 102 generates a plurality of ions from a sample.
- the ion source can include, but is not limited to electron ionization source, chemical ionization (CI) source, or a combination thereof.
- the mass analyzer 104 can separate ions based on a mass to charge ratio of the ions.
- the mass analyzer 104 can include a quadrupole mass filter analyzer, a quadrupole ion trap analyzer, a time-of-flight (TOF) analyzer, an electrostatic trap (e.g., ORBITRAP) mass analyzer, Fourier transform ion cyclotron resonance (FT-ICR) mass analyzer, and the like.
- the mass analyzer 104 can also be configured to fragment the ions using collision induced dissociation (CID) electron transfer dissociation (ETD), electron capture dissociation (ECD), photo induced dissociation (PID), surface induced dissociation (SID), and the like, and further separate the fragmented ions based on the mass-to-charge ratio.
- CID collision induced dissociation
- ETD electron transfer dissociation
- ECD electron capture dissociation
- PID photo induced dissociation
- SID surface induced dissociation
- the ion detector 106 can detect ions.
- the ion detector 106 can include an electron multiplier, a photo multiplier, an avalanche diode, a silicon photomultiplier, a Faraday cup, and the like. Ions leaving the mass analyzer can be detected by the ion detector.
- the ion detector can be quantitative, such that an accurate count of the ions can be determined.
- the functions of mass analyzer 104 and ion detector 106 can be performed by the same component.
- the controller 108 can communicate with the ion source 102 , the mass analyzer 104 , and the ion detector 106 .
- the controller 108 can configure the ion source or enable/disable the ion source.
- the controller 108 can configure the mass analyzer 104 to select a particular mass range to detect.
- the controller 108 can adjust the sensitivity of the ion detector 106 , such as by adjusting the gain.
- the controller 108 can adjust the polarity of the ion detector 106 based on the polarity of the ions being detected.
- the ion detector 106 can be configured to detect positive ions or be configured to detected negative ions.
- FIGS. 2A and 2B are diagrams illustrating an ion source 200 , which can be used as ion source 102 of mass spectrometry platform 100 .
- Ion source 200 can include an electron source 202 , an electron lens 204 , an ionization chamber 206 , lens elements 208 , 210 , and 212 , and RF ion guide 214 . Additionally, ion source 200 can include a body 216 , insulator 218 , spacers 220 and 222 , and retaining clip 224 .
- the ionization chamber 206 , lens elements 208 , 210 , and 212 , and RF ion guide 214 can be aligned such that ions produced by the ion source form an ion beam.
- the alignment of the ionization chamber 206 , lens elements 208 , 210 , and 212 , and RF ion guide 214 and the direction of the ion beam defines an axis 250 of the ion source.
- Electron source 202 can include a thermionic filament 226 for the generation of electrons. In various embodiments, electron source 202 can include more additional thermionic filaments for redundancy or increased electron production. In alternate embodiments, electron source 202 can include a field emitter, electron multiplier, photoelectric effect emitter, or other source of electrons. The electrons can travel axially along ion source 200 into ionization chamber 206 to ionize gas molecules. Electron lens 204 can serve to prevent the ions from traveling back towards the electron source.
- Ionization chamber 206 can include gas inlet 228 for directing a gas sample into an ionization volume 230 defined by the ionization chamber 206 .
- Gas molecules within the ionization volume 230 can be ionized by the electrons from the thermionic filament 226 .
- Lenses 208 and 210 can define a lens volume 232 .
- Lens volume 232 can include regions of the lenses where some electrons may be present. In various embodiments, it may also include areas outside of the ionization volume and the lenses.
- Wall 234 can restrict the flow of gas from ionization volume 230 to the lens volume 232 , creating a substantial pressure difference between the ionization volume 230 and lens volume 232 .
- Ion exit aperture 236 can provide a path through wall 234 for ions to exit the ionization chamber 206 .
- the ionization chamber 206 and lens element 208 can be joined to create an extended ionization element 240 defining the ionization volume 230 and at least a portion of the lens volume 232 .
- lens element 208 can be electrically coupled to ionization chamber 206 .
- the joined ionization chamber 206 and lens element 208 can be electrically isolated, such that different voltage potentials can be applied to the ionization chamber 206 and the lens element 208 .
- Lens 210 and 212 and RF ion guide 214 can assist in the axial movement of ions from the ionization volume 230 to additional ion optical elements and mass analyzer 104 of mass spectrometry platform 100 .
- ion guide assembly 238 can include lens 212 and RF ion guide 214 .
- Ion guide assembly 238 can include additional insulating portions to electrically isolate lens 212 from RF ion guide 214 . Additionally, the insulating portions can include standoffs to prevent electrical contact between lens 210 and lens 212 .
- insulator 218 When assembled into body 216 , insulator 218 can prevent electrical contact between lens 208 (or extended ionization element 240 ) and lens 210 .
- Spacer 220 can prevent electrical contact between electron lens 204 and ionization chamber 208 (or extended ionization element 240 ).
- Spacer 222 can be indexed to prevent rotation of the electron source 202 , and retaining clip 224 can hold the other components within body 216 .
- FIG. 3A is an illustration of a simulation of electrons in ion source 200 using positive chemical ionization (CI). Potentials used for the simulation are shown in FIG. 3A and Table 1.
- positive CI the ionizing electrons form reagent ions in the ionization volume. These reagent ions then interact with the analyte neutrals to form positive analyte ions.
- electrons can be on axis 250 with the ion beam. This can have the advantage of using the negative space charge from the electron beam to focus positive ions to the center axis 250 . Additionally, a negatively charged ion exit aperture can help extract positive ions. These features can also be beneficial when used for positive CI.
- FIG. 3B is an illustration of a simulation of electrons in ion source 200 performing negative CI. Potentials used for the simulation are shown in FIG. 3B and Table 2.
- the ionizing electrons can form reagent ions in the ionization volume.
- the outer shell electrons released during this ionization can be at thermal energies.
- the ionizing electrons can also lose kinetic energy as they collide with the reagent gas.
- the ionizing electrons can lose kinetic and reach thermal energies. These various thermal energy electrons can then interact with the analyte neutrals and can be captured to produce negative analyte ions.
- Electrons striking the area around ion exit aperture 236 can result in the accumulation of an insulating layer around the ion exit aperture, changing the potential to close to that of the electrons, ⁇ 70 V.
- neutral molecules from the analyte of matrix can temporarily land on the surfaces of the ionization chamber 206 . The molecules will generally leave the surface. However, if electrons strike the neutral molecules while on the surface, they can become attached to the surface in the form of inorganic carbon, silicon dioxide, or other insulating material depending on the composition of the molecule. This can form an insulating layer on the surface of the metal.
- the ion exit aperture can become a barrier to the electrons and the negative ions. This reduces the number of negative ions which leave the ionization volume 230 and travel to the ion detector 106 to be detected.
- FIG. 4 is an illustration of a simulation of electrons in ion source 400 performing negative ion chemical ionization.
- the magnetic field is shifted off-axis which directs the electron beam at an angle relative to the axis 450 of the ion 400 source.
- the magnetic field can be produced by a magnet, such as permanent magnet or an electromagnet, placed at one end of ion source, by a solenoid oriented around the ion source 400 , or other known techniques known for producing magnetic fields.
- the electron entrance aperture 452 can be shifted to align with the electron beam 454 rather than the ion source axis 450 .
- shifting the magnetic field by 4 mm and the aperture by 0.4 mm can direct the electrons away from the ion exit aperture 436 .
- shifting the electron entrance aperture 452 nearly the same number of electrons are able to reach the ionization volume.
- FIG. 5A illustrates the distribution of electrons striking the surface around the ion exit aperture 536 with the electron beam aligned with the ion source axis.
- the highest density of electrons 502 (indicated by the darkest color) is in the immediate vicinity of the ion exit aperture 536 .
- FIG. 5B illustrates the distribution of electrons when the magnetic field and electron entrance aperture are shifted to direct the electrons away from the ion exit aperture 536 .
- the highest density of electrons 506 is displaced from the ion exit aperture 536 , and the accumulation of an insulating layer around the ion exit aperture 536 can be reduced. This reduces the amount of charging near the ion exit aperture 536 and increases the number of analyte ions which are able to exit the ionization chamber 206 .
- FIG. 6 is an illustration of an ion source 600 for performing negative ion chemical ionization.
- the magnetic field is shifted off-axis which directs the electron beam 654 at an angle relative to the axis 650 of the ion source 600 .
- the electron entrance aperture 652 can be shifted to align with the electron beam 654 rather than the ion source axis 650 .
- a dimple, well, or pocket 656 is formed in wall 634 allowing the electron beam a greater distance of travel and moving the region of on highest electron impact density further away from the ion exit aperture 636 .
- FIG. 7 is an illustration of an ion source 700 for performing negative ion chemical ionization.
- the magnetic field is shifted off-axis which directs the electron beam 754 at an angle relative to the axis 750 of the ion source 700 .
- the electron entrance aperture 752 can be shifted to align with the electron beam 754 rather than the ion source axis 750 .
- the length of the ionization chamber 706 is extended by an additional 5.8 mm, allowing the electron beam 754 a greater distance of travel and moving the region of on highest electron impact density further away from the ion exit aperture 736 .
- the length of the ionization chamber 706 can be extended by more or less than 5.8 mm to achieve sufficient separation between the region of highest electron impact density and the ion exit aperture 736 .
- FIG. 8A illustrates the distribution of electrons when the magnetic field and electron entrance aperture are shifted to direct the electrons away from the ion exit aperture 836 and the ionization volume length is extended. Comparing to FIG. 5B , the highest density of electrons 802 is even further displaced from the ion exit aperture 836 and the electrons are distributed over a larger area, and further reducing the accumulation of an insulating layer around the ion exit aperture 836 .
- FIG. 9 is an illustration of an ion source 900 for performing negative ion chemical ionization.
- the electrons can be dispersed using an electron dispersive mechanism.
- the electron dispersive mechanism can include reducing or eliminating the magnetic field inside the ionization chamber 906 , such as by making the ionization chamber 906 from MuMetal or adding a layer of MuMetal between the electron source and the ionization chamber 906 , such as the wall shown by 958 .
- the simulation shows an ideal scenario where there is no magnetic field inside the ionization chamber 906 . Without the magnetic field to contain the electrons, electron to electron space charge can make the electrons spread out.
- additional magnets can be positioned to cancel out the magnetic fields within the ionization chamber or to make the magnetic fields dispersive to electrons rather than containing the electrons.
- the electrons can be dispersed electrostatically, such as by using a lens to direct electrons away from the ion exit aperture without substantially affecting the ion beam.
- FIG. 10 illustrates the distribution of electrons when the magnetic field inside the ionization chamber is reduced.
- the electrons are less focused and more evenly distributed over a larger area. Although many electrons still strike the area around the ion exit aperture 1036 , they are more spread out and accumulation of an insulating layer around the ion exit aperture 1036 can be reduced.
- FIG. 11 is an illustration of an ion source 1100 for performing negative ion chemical ionization.
- the electron source 1102 and magnetic field can be shifted relative to the axis 1150 of ion source 1100 .
- the electron beam 1154 can be parallel but offset from the axis 1150 of the ion source 1100 . In other embodiments, the electron beam 1154 may not be parallel but can be generally offset from the axis 1150 .
- FIG. 12 is an illustration of an ion source 1200 for performing negative ion chemical ionization.
- the electron source 1202 and magnetic field can be shifted relative to the axis 1250 of ion source 1200 and can be angled to align with the electron beam 1254 .
- the electron beam 1254 can be angled relative to the axis 1250 of the ion source 1200 , such as by less than 45°.
- the electron beam 1254 can intersect the axis 1250 or the electron beam 1254 and the axis 1250 can be skew.
- FIG. 13 illustrates a method 1300 of generating negative ions using chemical ionization.
- a reactant gas can be supplied into the ionization chamber of the ion source.
- electrons can be introduced into the ionization chamber to ionize the reactant gas and produce thermalized electrons.
- the thermalized electrons can include electrons ejected from outer electron shell when the reactant gas (or carrier gas) is ionized and electrons from the electron beam that are slowed or cooled by collisions with the reactant gas (and the carrier gas).
- the neutral analyte can be introduced into the ionization chamber.
- the thermalized electrons can react with and be captured by the neutral analyte to produce negative analyte ions.
- the ions can be extracted from the ionization chamber, and at 1313 , the ions can be analyzed.
- the specification may have presented a method and/or process as a particular sequence of steps.
- the method or process should not be limited to the particular sequence of steps described.
- other sequences of steps may be possible. Therefore, the particular order of the steps set forth in the specification should not be construed as limitations on the claims.
- the claims directed to the method and/or process should not be limited to the performance of their steps in the order written, and one skilled in the art can readily appreciate that the sequences may be varied and still remain within the spirit and scope of the various embodiments.
- the embodiments described herein can be practiced with other computer system configurations including hand-held devices, microprocessor systems, microprocessor-based or programmable consumer electronics, minicomputers, mainframe computers and the like.
- the embodiments can also be practiced in distributing computing environments where tasks are performed by remote processing devices that are linked through a network.
- any of the operations that form part of the embodiments described herein are useful machine operations.
- the embodiments, described herein also relate to a device or an apparatus for performing these operations.
- the systems and methods described herein can be specially constructed for the required purposes or it may be a general purpose computer selectively activated or configured by a computer program stored in the computer.
- various general purpose machines may be used with computer programs written in accordance with the teachings herein, or it may be more convenient to construct a more specialized apparatus to perform the required operations.
- Certain embodiments can also be embodied as computer readable code on a computer readable medium.
- the computer readable medium is any data storage device that can store data, which can thereafter be read by a computer system. Examples of the computer readable medium include hard drives, network attached storage (NAS), read-only memory, random-access memory, CD-ROMs, CD-Rs, CD-RWs, magnetic tapes, and other optical and non-optical data storage devices.
- the computer readable medium can also be distributed over a network coupled computer systems so that the computer readable code is stored and executed in a distributed fashion.
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Abstract
Description
- The present disclosure generally relates to the field of mass spectrometry including axial chemical ionization sources with an off-axis electron beam.
- Mass spectrometry can be used to perform detailed analyses on samples. Furthermore, mass spectrometry can provide both qualitative (is compound X present in the sample) and quantitative (how much of compound X is present in the sample) data for a large number of compounds in a sample. These capabilities have been used for a wide variety of analyses, such as to test for drug use, determine pesticide residues in food, monitor water quality, and the like.
- Sensitivity of a mass spectrometer can be limited by the efficiency of the ion source, ion losses through the mass spectrometer and in the mass analyzer, and sensitivity of the detector. Increasing the efficiency of the ion source, the number of ions produced per unit sample or per unit time, can significantly improve the detection limits of the mass spectrometer, enabling the detection of lower concentrations of compounds or the use of smaller amounts of sample. Additionally, increasing the stability of the ion source, number of ions produced as a function of time, is important for quantitative comparisons between runs and samples. As such, there is a need for improved ion sources.
- In a first aspect, an ion source can include an electron generator, an ionization chamber, a magnetic field, and an ion optic. The electron generator can be configured to produce electrons. The ionization chamber can have an electron entrance aperture through a first wall, an ion exit aperture through a second wall, and an axis. The ionization chamber can be configured to produce ions. The magnetic field can be arranged to confine electrons in a beam directed through the electron entrance aperture, in a direction within 45 degrees of parallel to the axis, and towards a location displaced from the ion exit aperture. The ion optic can be configured to direct ions exiting the ion exit aperture in an ion beam along the axis.
- In various embodiments of the first aspect, the ionization chamber can be configured to produce ions by chemical ionization.
- In various embodiments of the first aspect, the location can be on the second wall.
- In various embodiments of the first aspect, the electron beam can be parallel to the axis but offset from the ion beam in a direction orthogonal to the axis.
- In various embodiments of the first aspect, the electron beam can intersect a line along the direction of the ion beam.
- In various embodiments of the first aspect, the ionization chamber can further includes a recess on the second wall and displaced from the ion exit aperture, and the electron beam can be directed towards the recess.
- In various embodiments of the first aspect, a mass spectrometer can include an ion source of the first aspect, and a mass analyzer.
- In a second aspect, a method can include generating electrons; directing electrons in a beam through an electron entrance aperture through a first wall of an ionization chamber and towards a location displaced from an ion exit aperture through a second wall of the ionization chamber, and in a direction within 45 degrees of parallel to an axis of the ionization chamber; producing ions within the ionization chamber; and directing ions as a beam through the ion exit aperture and in a direction parallel to the axis of the ionization chamber.
- In various embodiments of the second aspect, producing ions within the ionization chamber can include producing ions by chemical ionization.
- In various embodiments of the second aspect, the location can be on the second wall.
- In various embodiments of the second aspect, directing the electron beam can include directing the electron beam in a direction parallel to the axis but offset from the ion beam in a direction orthogonal to the axis.
- In various embodiments of the second aspect, directing the electron beam can include directing the electron beam to intersect a line along the direction of the ion beam.
- In various embodiments of the second aspect, directing the electron beam can include directing the electron beam towards a recess on the second wall of the ionization chamber and displaced from the ion exit aperture.
- In a third aspect, an ion source can include an electron generator, an ionization chamber, a magnetic field, and an electron dispersive mechanism. The electron generator can be configured to produce electrons. The ionization chamber can have an electron entrance aperture through a first wall and an ion exit aperture through a second wall. The ionization chamber can be configured to produce ions. The magnetic field can be arranged to confine electrons in a beam directed through the electron entrance aperture. The electron dispersive mechanism can be configured to disperse the electrons within the ionization chamber.
- In various embodiments of the third aspect, the ionization chamber can be configured to produce ions by chemical ionization.
- In various embodiments of the third aspect, the first wall and the second wall can be opposite from one another.
- In various embodiments of the third aspect, the electron dispersive mechanism can include a magnetic shielding configured to reduce the magnetic fields within at least a portion of the ionization chamber.
- In various embodiments of the third aspect, the electron dispersive mechanism can include one or more additional magnets oriented to disrupt the magnetic field within at least one part of the ionization chamber.
- In various embodiments of the third aspect, the electron dispersive mechanism can include an electrostatic lens can be configured to direct electrons away from the ion exit aperture without substantially affecting the ion beam.
- In various embodiments of the third aspect, a mass spectrometer can include an ion source of third aspect and a mass analyzer.
- In a fourth aspect, a method can include generating electrons; directing electrons in a beam through an electron entrance aperture of an ionization chamber; dispersing the electrons within the ionization chamber; producing ions within the ionization chamber; and directing the ions as a beam through the ion exit aperture.
- In various embodiments of the fourth aspect, producing ions within the ionization chamber can includes producing ions by chemical ionization.
- For a more complete understanding of the principles disclosed herein, and the advantages thereof, reference is now made to the following descriptions taken in conjunction with the accompanying drawings and exhibits, in which:
-
FIG. 1 is a block diagram of an exemplary mass spectrometry system, in accordance with various embodiments. -
FIGS. 2A and 2B are diagrams illustrating an exemplary ion source, in accordance with various embodiments. -
FIGS. 3A and 3B are diagrams illustrating simulations of electrons in an ion source, in accordance with various embodiments. -
FIG. 4 is a diagram illustrating simulations of electrons in an ion source with an off axis magnetic field, in accordance with various embodiments. -
FIGS. 5A and 5B are diagrams illustrating electron impact density at the ion exit aperture, in accordance with various embodiments. -
FIG. 6 is a diagram illustrating a simulation of electrons in an ion source with an off axis magnetic field and a pocket for the electron beam, in accordance with various embodiments. -
FIG. 7 is a diagram illustrating a simulation of electrons in an ion source with an off axis magnetic field and an extended ionization chamber, in accordance with various embodiments. -
FIG. 8 is a diagram illustrating electron impact density at the ion exit aperture, in accordance with various embodiments. -
FIG. 9 is a diagram illustrating a simulation of electrons in an ion source with an electron dispersive mechanism, in accordance with various embodiments. -
FIG. 10 is a diagram illustrating electron impact density at the ion exit aperture, in accordance with various embodiments. -
FIGS. 11 and 12 are a diagrams illustrating ion sources with off-axis electron sources, in accordance with various embodiments. -
FIG. 13 is a flow diagram illustrating an exemplary method of operating an ion source, in accordance with various embodiments. - It is to be understood that the figures are not necessarily drawn to scale, nor are the objects in the figures necessarily drawn to scale in relationship to one another. The figures are depictions that are intended to bring clarity and understanding to various embodiments of apparatuses, systems, and methods disclosed herein. Wherever possible, the same reference numbers will be used throughout the drawings to refer to the same or like parts. Moreover, it should be appreciated that the drawings are not intended to limit the scope of the present teachings in any way.
- Embodiments of systems and methods for ion isolation are described herein and in the accompanying exhibits.
- The section headings used herein are for organizational purposes only and are not to be construed as limiting the described subject matter in any way.
- In this detailed description of the various embodiments, for purposes of explanation, numerous specific details are set forth to provide a thorough understanding of the embodiments disclosed. One skilled in the art will appreciate, however, that these various embodiments may be practiced with or without these specific details. In other instances, structures and devices are shown in block diagram form. Furthermore, one skilled in the art can readily appreciate that the specific sequences in which methods are presented and performed are illustrative and it is contemplated that the sequences can be varied and still remain within the spirit and scope of the various embodiments disclosed herein.
- All literature and similar materials cited in this application, including but not limited to, patents, patent applications, articles, books, treatises, and internet web pages are expressly incorporated by reference in their entirety for any purpose. Unless described otherwise, all technical and scientific terms used herein have a meaning as is commonly understood by one of ordinary skill in the art to which the various embodiments described herein belongs.
- It will be appreciated that there is an implied “about” prior to the temperatures, concentrations, times, pressures, flow rates, cross-sectional areas, etc. discussed in the present teachings, such that slight and insubstantial deviations are within the scope of the present teachings. In this application, the use of the singular includes the plural unless specifically stated otherwise. Also, the use of “comprise”, “comprises”, “comprising”, “contain”, “contains”, “containing”, “include”, “includes”, and “including” are not intended to be limiting. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the present teachings.
- As used herein, “a” or “an” also may refer to “at least one” or “one or more.” Also, the use of “or” is inclusive, such that the phrase “A or B” is true when “A” is true, “B” is true, or both “A” and “B” are true. Further, unless otherwise required by context, singular terms shall include pluralities and plural terms shall include the singular.
- A “system” sets forth a set of components, real or abstract, comprising a whole where each component interacts with or is related to at least one other component within the whole.
- Various embodiments of
mass spectrometry platform 100 can include components as displayed in the block diagram ofFIG. 1 . In various embodiments, elements ofFIG. 1 can be incorporated intomass spectrometry platform 100. According to various embodiments,mass spectrometer 100 can include anion source 102, amass analyzer 104, anion detector 106, and acontroller 108. - In various embodiments, the
ion source 102 generates a plurality of ions from a sample. The ion source can include, but is not limited to electron ionization source, chemical ionization (CI) source, or a combination thereof. - In various embodiments, the
mass analyzer 104 can separate ions based on a mass to charge ratio of the ions. For example, themass analyzer 104 can include a quadrupole mass filter analyzer, a quadrupole ion trap analyzer, a time-of-flight (TOF) analyzer, an electrostatic trap (e.g., ORBITRAP) mass analyzer, Fourier transform ion cyclotron resonance (FT-ICR) mass analyzer, and the like. In various embodiments, themass analyzer 104 can also be configured to fragment the ions using collision induced dissociation (CID) electron transfer dissociation (ETD), electron capture dissociation (ECD), photo induced dissociation (PID), surface induced dissociation (SID), and the like, and further separate the fragmented ions based on the mass-to-charge ratio. - In various embodiments, the
ion detector 106 can detect ions. For example, theion detector 106 can include an electron multiplier, a photo multiplier, an avalanche diode, a silicon photomultiplier, a Faraday cup, and the like. Ions leaving the mass analyzer can be detected by the ion detector. In various embodiments, the ion detector can be quantitative, such that an accurate count of the ions can be determined. In various embodiments, such as when using an electrostatic mass analyzer, the functions ofmass analyzer 104 andion detector 106 can be performed by the same component. - In various embodiments, the
controller 108 can communicate with theion source 102, themass analyzer 104, and theion detector 106. For example, thecontroller 108 can configure the ion source or enable/disable the ion source. Additionally, thecontroller 108 can configure themass analyzer 104 to select a particular mass range to detect. Further, thecontroller 108 can adjust the sensitivity of theion detector 106, such as by adjusting the gain. Additionally, thecontroller 108 can adjust the polarity of theion detector 106 based on the polarity of the ions being detected. For example, theion detector 106 can be configured to detect positive ions or be configured to detected negative ions. -
FIGS. 2A and 2B are diagrams illustrating anion source 200, which can be used asion source 102 ofmass spectrometry platform 100.Ion source 200 can include anelectron source 202, anelectron lens 204, anionization chamber 206,lens elements RF ion guide 214. Additionally,ion source 200 can include abody 216,insulator 218,spacers clip 224. In various embodiments, theionization chamber 206,lens elements RF ion guide 214 can be aligned such that ions produced by the ion source form an ion beam. The alignment of theionization chamber 206,lens elements RF ion guide 214 and the direction of the ion beam defines anaxis 250 of the ion source. -
Electron source 202 can include athermionic filament 226 for the generation of electrons. In various embodiments,electron source 202 can include more additional thermionic filaments for redundancy or increased electron production. In alternate embodiments,electron source 202 can include a field emitter, electron multiplier, photoelectric effect emitter, or other source of electrons. The electrons can travel axially alongion source 200 intoionization chamber 206 to ionize gas molecules.Electron lens 204 can serve to prevent the ions from traveling back towards the electron source. -
Ionization chamber 206 can includegas inlet 228 for directing a gas sample into anionization volume 230 defined by theionization chamber 206. Gas molecules within theionization volume 230 can be ionized by the electrons from thethermionic filament 226.Lenses lens volume 232.Lens volume 232 can include regions of the lenses where some electrons may be present. In various embodiments, it may also include areas outside of the ionization volume and the lenses.Wall 234 can restrict the flow of gas fromionization volume 230 to thelens volume 232, creating a substantial pressure difference between theionization volume 230 andlens volume 232.Ion exit aperture 236 can provide a path throughwall 234 for ions to exit theionization chamber 206. - In various embodiments, the
ionization chamber 206 andlens element 208 can be joined to create an extended ionization element 240 defining theionization volume 230 and at least a portion of thelens volume 232. In such embodiments,lens element 208 can be electrically coupled toionization chamber 206. In other embodiments, the joinedionization chamber 206 andlens element 208 can be electrically isolated, such that different voltage potentials can be applied to theionization chamber 206 and thelens element 208. -
Lens RF ion guide 214 can assist in the axial movement of ions from theionization volume 230 to additional ion optical elements andmass analyzer 104 ofmass spectrometry platform 100. In various embodiments,ion guide assembly 238 can includelens 212 andRF ion guide 214.Ion guide assembly 238 can include additional insulating portions to electrically isolatelens 212 fromRF ion guide 214. Additionally, the insulating portions can include standoffs to prevent electrical contact betweenlens 210 andlens 212. - When assembled into
body 216,insulator 218 can prevent electrical contact between lens 208 (or extended ionization element 240) andlens 210.Spacer 220 can prevent electrical contact betweenelectron lens 204 and ionization chamber 208 (or extended ionization element 240).Spacer 222 can be indexed to prevent rotation of theelectron source 202, and retainingclip 224 can hold the other components withinbody 216. -
FIG. 3A is an illustration of a simulation of electrons inion source 200 using positive chemical ionization (CI). Potentials used for the simulation are shown inFIG. 3A and Table 1. In positive CI, the ionizing electrons form reagent ions in the ionization volume. These reagent ions then interact with the analyte neutrals to form positive analyte ions. -
TABLE 1 Positive Chemical Ionization Simulation Filament 226 −70 V Electron Lens 204 5 V Ionization Chamber 206 0 V (grounded) Lens 2080 V (grounded) Lens 210−7 V Lens 212 −83 V RF Ion Guide 214−7 V - In
ion source 200, electrons can be onaxis 250 with the ion beam. This can have the advantage of using the negative space charge from the electron beam to focus positive ions to thecenter axis 250. Additionally, a negatively charged ion exit aperture can help extract positive ions. These features can also be beneficial when used for positive CI. -
FIG. 3B is an illustration of a simulation of electrons inion source 200 performing negative CI. Potentials used for the simulation are shown inFIG. 3B and Table 2. In negative CI, the ionizing electrons can form reagent ions in the ionization volume. The outer shell electrons released during this ionization can be at thermal energies. The ionizing electrons can also lose kinetic energy as they collide with the reagent gas. Ultimately, the ionizing electrons can lose kinetic and reach thermal energies. These various thermal energy electrons can then interact with the analyte neutrals and can be captured to produce negative analyte ions. - Electrons striking the area around
ion exit aperture 236 can result in the accumulation of an insulating layer around the ion exit aperture, changing the potential to close to that of the electrons, −70 V. In various embodiments, neutral molecules from the analyte of matrix can temporarily land on the surfaces of theionization chamber 206. The molecules will generally leave the surface. However, if electrons strike the neutral molecules while on the surface, they can become attached to the surface in the form of inorganic carbon, silicon dioxide, or other insulating material depending on the composition of the molecule. This can form an insulating layer on the surface of the metal. As charged particles, such as electrons, strike the insulating layer, their charge cannot be quickly dissipated by the underlying metal and instead a charge can accumulate on the insulating layer. Once that occurs, the ion exit aperture can become a barrier to the electrons and the negative ions. This reduces the number of negative ions which leave theionization volume 230 and travel to theion detector 106 to be detected. -
TABLE 2 Negative Chemical Ionization Simulation Filament 226 −70 V Electron Lens 204 +5 V Ionization Chamber 206 0 V (grounded) Lens 2080 V (grounded) Lens 210+7 V Lens 212 +100 V RF Ion Guide 214+7 V - For CI, there is no inherent reason the electrons need to be on the same axis as the ions. By modifying the ion source geometry so the ion beam does not strike the exit aperture from the ionization chamber, charging near the aperture can be reduced.
-
FIG. 4 is an illustration of a simulation of electrons inion source 400 performing negative ion chemical ionization. Inion source 400, the magnetic field is shifted off-axis which directs the electron beam at an angle relative to theaxis 450 of theion 400 source. In various embodiments, the magnetic field can be produced by a magnet, such as permanent magnet or an electromagnet, placed at one end of ion source, by a solenoid oriented around theion source 400, or other known techniques known for producing magnetic fields. Additionally, theelectron entrance aperture 452 can be shifted to align with theelectron beam 454 rather than theion source axis 450. In an exemplary embodiment, shifting the magnetic field by 4 mm and the aperture by 0.4 mm can direct the electrons away from theion exit aperture 436. By also shifting theelectron entrance aperture 452, nearly the same number of electrons are able to reach the ionization volume. -
FIG. 5A illustrates the distribution of electrons striking the surface around theion exit aperture 536 with the electron beam aligned with the ion source axis. The highest density of electrons 502 (indicated by the darkest color) is in the immediate vicinity of theion exit aperture 536. In contrast,FIG. 5B illustrates the distribution of electrons when the magnetic field and electron entrance aperture are shifted to direct the electrons away from theion exit aperture 536. The highest density ofelectrons 506 is displaced from theion exit aperture 536, and the accumulation of an insulating layer around theion exit aperture 536 can be reduced. This reduces the amount of charging near theion exit aperture 536 and increases the number of analyte ions which are able to exit theionization chamber 206. -
FIG. 6 is an illustration of anion source 600 for performing negative ion chemical ionization. Inion source 600, the magnetic field is shifted off-axis which directs theelectron beam 654 at an angle relative to theaxis 650 of theion source 600. Additionally, theelectron entrance aperture 652 can be shifted to align with theelectron beam 654 rather than theion source axis 650. Additionally, a dimple, well, orpocket 656 is formed inwall 634 allowing the electron beam a greater distance of travel and moving the region of on highest electron impact density further away from theion exit aperture 636. -
FIG. 7 is an illustration of anion source 700 for performing negative ion chemical ionization. Inion source 700, the magnetic field is shifted off-axis which directs theelectron beam 754 at an angle relative to theaxis 750 of theion source 700. Additionally, theelectron entrance aperture 752 can be shifted to align with theelectron beam 754 rather than theion source axis 750. Additionally, the length of theionization chamber 706 is extended by an additional 5.8 mm, allowing the electron beam 754 a greater distance of travel and moving the region of on highest electron impact density further away from theion exit aperture 736. In various embodiments, the length of theionization chamber 706 can be extended by more or less than 5.8 mm to achieve sufficient separation between the region of highest electron impact density and theion exit aperture 736. -
FIG. 8A illustrates the distribution of electrons when the magnetic field and electron entrance aperture are shifted to direct the electrons away from theion exit aperture 836 and the ionization volume length is extended. Comparing toFIG. 5B , the highest density of electrons 802 is even further displaced from theion exit aperture 836 and the electrons are distributed over a larger area, and further reducing the accumulation of an insulating layer around theion exit aperture 836. -
FIG. 9 is an illustration of anion source 900 for performing negative ion chemical ionization. Inion source 900, the electrons can be dispersed using an electron dispersive mechanism. In various embodiments, the electron dispersive mechanism can include reducing or eliminating the magnetic field inside theionization chamber 906, such as by making theionization chamber 906 from MuMetal or adding a layer of MuMetal between the electron source and theionization chamber 906, such as the wall shown by 958. The simulation shows an ideal scenario where there is no magnetic field inside theionization chamber 906. Without the magnetic field to contain the electrons, electron to electron space charge can make the electrons spread out. In other embodiments, additional magnets can be positioned to cancel out the magnetic fields within the ionization chamber or to make the magnetic fields dispersive to electrons rather than containing the electrons. In yet other embodiments, the electrons can be dispersed electrostatically, such as by using a lens to direct electrons away from the ion exit aperture without substantially affecting the ion beam. -
FIG. 10 illustrates the distribution of electrons when the magnetic field inside the ionization chamber is reduced. The electrons are less focused and more evenly distributed over a larger area. Although many electrons still strike the area around theion exit aperture 1036, they are more spread out and accumulation of an insulating layer around theion exit aperture 1036 can be reduced. -
FIG. 11 is an illustration of anion source 1100 for performing negative ion chemical ionization. Inion source 1100, theelectron source 1102 and magnetic field can be shifted relative to theaxis 1150 ofion source 1100. In various embodiments, theelectron beam 1154 can be parallel but offset from theaxis 1150 of theion source 1100. In other embodiments, theelectron beam 1154 may not be parallel but can be generally offset from theaxis 1150. -
FIG. 12 is an illustration of anion source 1200 for performing negative ion chemical ionization. Inion source 1200, theelectron source 1202 and magnetic field can be shifted relative to theaxis 1250 ofion source 1200 and can be angled to align with theelectron beam 1254. In various embodiments, theelectron beam 1254 can be angled relative to theaxis 1250 of theion source 1200, such as by less than 45°. In various embodiments, theelectron beam 1254 can intersect theaxis 1250 or theelectron beam 1254 and theaxis 1250 can be skew. -
FIG. 13 illustrates amethod 1300 of generating negative ions using chemical ionization. At 1302, a reactant gas can be supplied into the ionization chamber of the ion source. At 1304, electrons can be introduced into the ionization chamber to ionize the reactant gas and produce thermalized electrons. The thermalized electrons can include electrons ejected from outer electron shell when the reactant gas (or carrier gas) is ionized and electrons from the electron beam that are slowed or cooled by collisions with the reactant gas (and the carrier gas). At 1306, the neutral analyte can be introduced into the ionization chamber. At 1308, the thermalized electrons can react with and be captured by the neutral analyte to produce negative analyte ions. At 1310, the ions can be extracted from the ionization chamber, and at 1313, the ions can be analyzed. - While the present teachings are described in conjunction with various embodiments, it is not intended that the present teachings be limited to such embodiments. On the contrary, the present teachings encompass various alternatives, modifications, and equivalents, as will be appreciated by those of skill in the art.
- Further, in describing various embodiments, the specification may have presented a method and/or process as a particular sequence of steps. However, to the extent that the method or process does not rely on the particular order of steps set forth herein, the method or process should not be limited to the particular sequence of steps described. As one of ordinary skill in the art would appreciate, other sequences of steps may be possible. Therefore, the particular order of the steps set forth in the specification should not be construed as limitations on the claims. In addition, the claims directed to the method and/or process should not be limited to the performance of their steps in the order written, and one skilled in the art can readily appreciate that the sequences may be varied and still remain within the spirit and scope of the various embodiments.
- The embodiments described herein, can be practiced with other computer system configurations including hand-held devices, microprocessor systems, microprocessor-based or programmable consumer electronics, minicomputers, mainframe computers and the like. The embodiments can also be practiced in distributing computing environments where tasks are performed by remote processing devices that are linked through a network.
- It should also be understood that the embodiments described herein can employ various computer-implemented operations involving data stored in computer systems. These operations are those requiring physical manipulation of physical quantities. Usually, though not necessarily, these quantities take the form of electrical or magnetic signals capable of being stored, transferred, combined, compared, and otherwise manipulated. Further, the manipulations performed are often referred to in terms, such as producing, identifying, determining, or comparing.
- Any of the operations that form part of the embodiments described herein are useful machine operations. The embodiments, described herein, also relate to a device or an apparatus for performing these operations. The systems and methods described herein can be specially constructed for the required purposes or it may be a general purpose computer selectively activated or configured by a computer program stored in the computer. In particular, various general purpose machines may be used with computer programs written in accordance with the teachings herein, or it may be more convenient to construct a more specialized apparatus to perform the required operations.
- Certain embodiments can also be embodied as computer readable code on a computer readable medium. The computer readable medium is any data storage device that can store data, which can thereafter be read by a computer system. Examples of the computer readable medium include hard drives, network attached storage (NAS), read-only memory, random-access memory, CD-ROMs, CD-Rs, CD-RWs, magnetic tapes, and other optical and non-optical data storage devices. The computer readable medium can also be distributed over a network coupled computer systems so that the computer readable code is stored and executed in a distributed fashion.
Claims (22)
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US18/182,176 US20230230826A1 (en) | 2019-12-10 | 2023-03-10 | Axial ci source - off-axis electron beam |
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CA1252581A (en) * | 1985-05-28 | 1989-04-11 | Yoshinobu Aoyagi | Electron beam-excited ion beam source |
US4742232A (en) * | 1987-03-03 | 1988-05-03 | United States Of America As Represented By The Adminstrator, National Aeronautics And Space Administration | Ion generator and ion application system |
US4933551A (en) * | 1989-06-05 | 1990-06-12 | The United State Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Reversal electron attachment ionizer for detection of trace species |
US5365070A (en) * | 1992-04-29 | 1994-11-15 | The Regents Of The University Of California | Negative ion beam injection apparatus with magnetic shield and electron removal means |
US7535329B2 (en) * | 2005-04-14 | 2009-05-19 | Makrochem, Ltd. | Permanent magnet structure with axial access for spectroscopy applications |
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