CN117457471A - Mass spectrometer of hydrogen isotope accelerator - Google Patents
Mass spectrometer of hydrogen isotope accelerator Download PDFInfo
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- CN117457471A CN117457471A CN202311107621.5A CN202311107621A CN117457471A CN 117457471 A CN117457471 A CN 117457471A CN 202311107621 A CN202311107621 A CN 202311107621A CN 117457471 A CN117457471 A CN 117457471A
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- ion
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- hydrogen isotope
- mass spectrometer
- ecr
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000001257 hydrogen Substances 0.000 title claims abstract description 33
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 33
- 150000002500 ions Chemical class 0.000 claims abstract description 80
- 239000007789 gas Substances 0.000 claims abstract description 59
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 40
- 238000002347 injection Methods 0.000 claims abstract description 9
- 239000007924 injection Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 230000001133 acceleration Effects 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 7
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 230000005686 electrostatic field Effects 0.000 description 3
- 238000004949 mass spectrometry Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001793 charged compounds Chemical class 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- TVEXGJYMHHTVKP-UHFFFAOYSA-N 6-oxabicyclo[3.2.1]oct-3-en-7-one Chemical compound C1C2C(=O)OC1C=CC2 TVEXGJYMHHTVKP-UHFFFAOYSA-N 0.000 description 1
- 238000004760 accelerator mass spectrometry Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005040 ion trap Methods 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006467 substitution reaction 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
- H01J49/105—Ion sources; Ion guns using high-frequency excitation, e.g. microwave excitation, Inductively Coupled Plasma [ICP]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
- H01J49/34—Dynamic spectrometers
- H01J49/36—Radio frequency spectrometers, e.g. Bennett-type spectrometers, Redhead-type spectrometers
- H01J49/38—Omegatrons ; using ion cyclotron resonance
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H13/00—Magnetic resonance accelerators; Cyclotrons
- H05H13/005—Cyclotrons
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a mass spectrometer of a hydrogen isotope accelerator, which comprises a sample injection assembly, an electron cyclotron resonance ECR ion source, an accelerating tube, a mass analyzer, a flow intensity detector and a detector system, wherein the ECR ion source is used for ionizing mixed gas to generate mixed ion beams comprising a plurality of ion beams; under the action of the extraction voltage of the ECR ion source and the acceleration voltage of the acceleration tube, the accelerated mixed ion beam enters a mass analyzer connected with the acceleration tube; the mass analyzer separates ion beams with different mass-to-charge ratios in the mixed ion beam and enters the flow intensity detector; the flow intensity detector is used for determining the ion signal intensity of the separated ion beam; the detector system is used for identifying ions with the same mass number in the separated ion beam. The embodiment greatly improves the measurement sensitivity and the measurement precision by adopting the ECR ion source and the accelerating tube to enable the mixed ion beam to have higher energy. In addition, ions of the same mass number can be identified by the detector system.
Description
Technical Field
The invention relates to the technical field of isotope analysis, in particular to a hydrogen isotope accelerator mass spectrometer.
Background
In nature, hydrogen always exists in the form of diatomic molecules, which presents great difficulties in measuring the abundance of hydrogen isotopes. Hydrogen has three isotopes, naturally forming six isotopic molecules: h 2 、HD、D 2 、HT、DT、T 2 。
Ion sources of mass spectrometers for hydrogen isotope analysis currently related are mostly electron bombardment, naturally generating monovalent ions of six hydrogen isotope diatomic molecules: h 2 + 、HD + 、D 2 + 、HT + 、DT + 、T 2 + 。
The associated mass spectrometer cannot measure D 2 + 、HT + Molecular ions of the same mass number are distinguished. Therefore, it is necessary to measure HT by gas chromatography or the like + The content is then corrected for the mass spectrometry measurement, i.e. the combined determination of gas chromatography and mass spectrometry. The measurement apparatus has a problem of high design cost.
Disclosure of Invention
The summary of the invention is provided to introduce a selection of concepts in a simplified form that are further described below in the detailed description. The disclosure is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
Some embodiments of the present invention provide a hydrogen isotope accelerator mass spectrometer that solves the technical problems noted in the background section above.
The hydrogen isotope accelerator mass spectrometer comprises a sample injection assembly, an ECR ion source, an accelerating tube, a mass analyzer, a flow intensity detector and a detector system, wherein the ECR ion source is used for ionizing mixed gas entering from the sample injection assembly to generate mixed ion beams comprising a plurality of ion beams; the accelerating tube is connected with the ECR ion source, and the accelerated mixed ion beam enters a mass analyzer connected with the accelerating tube under the action of the extraction voltage of the ECR ion source and the accelerating voltage of the accelerating tube; the mass analyzer separates ion beams with different mass-to-charge ratios in the mixed ion beam and enters the intensity detector; the flow intensity detector is used for determining the ion signal intensity of the separated ion beam; the detector system is used for identifying ions with the same mass number in the separated ion beam.
Optionally, the sample injection assembly includes an air intake system, a sample air pipe, and an auxiliary support air pipe, where the sample air pipe is connected to the air intake system and is used to introduce hydrogen isotope gas into the air intake system; the auxiliary support gas pipeline is connected with the gas inlet system and is used for introducing auxiliary gas into the gas inlet system; the gas inlet system is connected with the ECR ion source, and mixed gas formed by mixing the hydrogen isotope gas in the gas inlet system and the auxiliary gas enters the ECR ion source.
Optionally, the flow intensity detector comprises 9 faraday cups, which correspondingly detect H + 、H 2 + /D + 、T + /HD + / 3 He + /H 3 + 、D 2 + 、DT + 、T + 、C + 、N + O and O + Is a function of the ion signal intensity of the ion source.
Optionally, the ions with the same mass number comprise H 2 + And D + Comprises T + 、 3 He + 、HD + And H 3 + Is a second ion group of (c).
Optionally, the first ion set is driven into a second faraday cup.
Optionally, the second ion set is driven into a third faraday cup.
Optionally, the detector system comprises two multi-anode gas ionization chambers.
Optionally, the two multi-anode gas ionization chambers are respectively connected to the second faraday cup and the third faraday cup for measuring each ion content in the first ion set and the second ion set.
Optionally, the mass analyzer comprises an electromagnet.
The above embodiment of the present invention has the following advantageous effects: according to the hydrogen isotope accelerator mass spectrometer, an ECR ion source (Electron Cyclotron Resonance Ion Source ) is adopted to generate an ion beam with a higher charge state than that of a traditional ion source, electrons on the outer layer of atoms can be almost completely stripped, so that single-atom ions can be mainly generated, and molecular ion interference is eliminated. Further, the accelerating tube can accelerate the mixed ion flow, so that the mixed ion beam has higher energy, and conditions are provided for discriminating the ion beam by the flow intensity detector and the detector system. In addition, the limitations of molecular background and isobaric background existing in the traditional mass spectrometry can be broken through, so that the measurement sensitivity and measurement accuracy are greatly improved. The mass analyzer can effectively separate the mixed ion beams according to the difference of deflection track radiuses of the ion beams with different mass-to-charge ratios in a magnetic field. And finally, identifying ions with the same mass number through a detector system.
The mass spectrometer of the hydrogen isotope accelerator also has the advantages of low instrument design and processing cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of one embodiment of a hydrogen isotope accelerator mass spectrometer of the present invention.
Reference numerals illustrate:
1: a sample gas conduit; 2: an auxiliary support gas duct; 3: an air intake system; 4: an ECR ion source; 5: an accelerating tube; 6: a mass analyzer; 7: a flow intensity detector.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more of the described features. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise. Furthermore, the terms "mounted," "connected," "coupled," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The present disclosure will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Referring to fig. 1, fig. 1 is a schematic diagram of a hydrogen isotope accelerator mass spectrometer according to an embodiment of the present invention. As shown in fig. 1, the hydrogen isotope accelerator mass spectrometer includes a sample injection assembly, an ECR (electron cyclotron resonance ) ion source 4, an acceleration tube 5, a mass analyzer 6, a flow intensity detector 7, and a detector system.
The sample introduction assembly is connected to an ECR ion source 4. Specifically, the sample injection assembly includes an air intake system 3, a sample gas conduit 1, and an auxiliary support gas conduit 2. The gas inlet system 3 corresponds to that of a conventional gas mass spectrometer and can be selected by a person skilled in the art based on common general knowledge. The sample gas pipe 1 is connected to a left side intake end (direction in fig. 1) of the intake system 3 for introducing a hydrogen isotope gas into the intake system 3. The auxiliary support gas duct 2 is connected to a left side intake end (direction in fig. 1) of the intake system 3 for introducing auxiliary gas into the intake system 3. The outlet end on the right side (direction in fig. 1) of the inlet system 3 is connected to the ECR ion source 4. In actual operation, the hydrogen isotope gas and the assist gas are sufficiently and uniformly mixed to form a mixed gas, and the mixed gas can enter the ECR ion source 4 at an air intake rate of 0.03 sccm. It should be noted that the air intake rate is not fixed, and the above 0.03sccm is merely exemplary, and those skilled in the art can adjust the air intake rate according to actual situations.
The rf power of the ECR ion source 4 may be set to 100W, and further, since the auxiliary gas is introduced into the auxiliary support gas pipe 2 as a support body, H can be further generated after the ECR ion source 4 acts on the mixed gas + 、D + 、T + 、 3 He + 、H 2 + 、HD + 、H 3 + 、D 2 + 、DT + 、T 2 + 、Ar + And a small amount of C + 、N + 、O + Monoatomic ions. As an example, the auxiliary gas may be argon, which not only can effectively reduce H 2 + Is beneficial to the generation of H 2 Is (are) to collapse and promote H + Is generated. As another example, the auxiliary gas may also be helium. Specifically, the beam current drawn by the ECR ion source 4 may be in the range of 1nA to 1mA and continuously adjustable. The microwave frequency of ECR ion source 4 is in the range of 2-20 GHz. Likewise, although the above description is given by taking the setting of the rf power of the ECR ion source to 100W as an example, the rf power is not fixed, and the rf power may be adjusted by those skilled in the art according to the actual situation.
The accelerating tube 5 is connected to the outlet end of the ECR ion source 4, and the accelerating tube 5 may be an electric field accelerator. The accelerating tube 5 has its two ends connected to high voltage and ground, respectively. In this way, the mixed ion beam is accelerated by the high-voltage electrostatic field while passing through the accelerating tube 5, and thus a high energy is obtained.
In summary, the energy of the mixed ion beam is achieved by pre-acceleration of the extraction voltage of the ECR ion source 4 and high voltage electrostatic field acceleration of the accelerating tube 5. The extraction voltage of the ECR ion source 4 is set to be 20kV, the mixed ion beam has energy of 20keV after being extracted by the extraction voltage of the ECR ion source 4, the acceleration voltage of the accelerating tube 5 is set to be 160kV, and the mixed ion beam has energy of 180keV after being accelerated by the high-voltage electrostatic field of the accelerating tube 5. The ECR ion source 4 may be powered by a separate 30kV high voltage power supply and the accelerating tube 5 by another 200kV high voltage power supply. The mixed gas is ionized by adjusting the radio frequency power of the ECR ion source 4, the air inflow of the hydrogen isotope gas and the like.
The mass analyzer 6 is configured to separate ion beams of different mass to charge ratios in the mixed ion beam. As examples, the mass analyzer 6 described above may be a magnetic analyzer, a four-stage rod mass analyzer, an ion trap mass analyzer. The magnetic analyzer comprises an electromagnet, the electromagnetic field intensity of which is continuously adjustable between 0T and 1T, and the magnetic field current of the electromagnet can be 58.55A. The magnetic analyzer is capable of converting H in the mixed ion beam with energy of 180keV according to different deflection track radius of ion beam with different mass-to-charge ratio in magnetic field + 、H 2 + /D + 、T + /HD + / 3 He + /H 3 + 、D 2 + 、DT + 、T + 、C + 、N + O and O + The nine ion beams are separated and directed into a flow intensity detector.
The intensity detector is used to determine the ion signal intensities of the different ion beams. By way of example, the above-described flow intensity detector may be a faraday cup, an ion counter, or the like. Taking faraday cups as an example, the mass spectrometer comprises nine faraday cups 7 arranged at intervals, the nine ion beams are correspondingly driven into the nine faraday cups 7 one by one, and the faraday cups 7 can determine the ion signal intensity of the corresponding ion beams and further determine the number of incident ions. Thus, the faraday cup 7 can also be used for C + 、N + O and O + The ion beam quantity of the mass spectrometer can be used for measuring the impurity content, so that the versatility of the mass spectrometer is improved.
Due to H 2 + And D + The same mass numbers are all driven into a second faraday cup 7 (shown in fig. 1) to form a first ion set. T (T) + 、HD + 、 3 He + And H 3 + The same ion mass number is driven into a third faraday cup 7 (shown in fig. 1) to form a second ion set.
The detector system may include two multi-anode gas ionization chambers connected to the bottoms of the second and third faraday cups, respectively, to measure the ion content of each of the first and second ion groups. Specifically, small holes can be formed at bottoms of the second Faraday cup and the third Faraday cup, so that the first ion group and the second ion group enter corresponding multi-anode gas ionization chambers.
The multi-anode gas ionization chamber can effectively measure the isobaric element based on an energy loss method, namely, the identification of the isobaric element is realized corresponding to the difference of the energy loss of ions in different anode areas. The person skilled in the art can choose multiple anode gas ionization chambers according to the actual situation. As an example, the multi-anode gas ionization chamber is described in detail on pages 80-83 of a book entitled "accelerator mass spectrometry technology and its applications" published by the university of Shanghai transportation press in 2020, wherein the structure and working principles of the feeding and gas ionization chamber developed by the national institute of atomic energy science are also illustrated.
In this way, by arranging the detector system, the content of each ion in the first ion combination second ion group can be measured, so that the accurate measurement of the hydrogen isotope abundance is realized.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. A mass spectrometer of a hydrogen isotope accelerator is characterized by comprising a sample injection assembly, an ECR ion source, an accelerating tube, a mass analyzer, a flow intensity detector and a detector system, wherein,
the ECR ion source is used for ionizing the mixed gas entering from the sample injection assembly to generate a mixed ion beam comprising a plurality of ion beams;
the accelerating tube is connected with the ECR ion source, and the accelerated mixed ion beam enters a mass analyzer connected with the accelerating tube under the action of the extraction voltage of the ECR ion source and the accelerating voltage of the accelerating tube;
the mass analyzer separates ion beams with different mass-to-charge ratios in the mixed ion beam and enters the intensity detector;
the flow intensity detector is used for determining the ion signal intensity of the separated ion beam;
the detector system is used for identifying ions with the same mass number in the separated ion beam.
2. The hydrogen isotope accelerator mass spectrometer of claim 1, wherein the sample injection assembly includes an air intake system, a sample gas conduit, and an auxiliary support gas conduit, wherein,
the sample gas pipeline is connected with the gas inlet system and is used for introducing hydrogen isotope gas into the gas inlet system; the auxiliary support gas pipeline is connected with the gas inlet system and is used for introducing auxiliary gas into the gas inlet system; the gas inlet system is connected with the ECR ion source, and mixed gas formed by mixing the hydrogen isotope gas in the gas inlet system and the auxiliary gas enters the ECR ion source.
3. A hydrogen isotope accelerator mass spectrometer as defined in claim 1, wherein the flow intensity detector includes 9 faraday cups for detecting H correspondingly + 、H 2 + /D + 、T + /HD + / 3 He + /H 3 + 、D 2 + 、DT + 、T + 、C + 、N + O and O + Is a function of the ion signal intensity of the ion source.
4. A hydrogen isotope accelerator mass spectrometer as defined in claim 3, wherein said ions of equal mass number include H 2 + And D + Comprises T + 、 3 He + 、HD + And H 3 + Is a second ion group of (c).
5. A hydrogen isotope accelerator mass spectrometer as defined in claim 4, wherein the first ion set is driven into a second faraday cup.
6. A hydrogen isotope accelerator mass spectrometer as defined in claim 4, wherein the second ion set is driven into a third faraday cup.
7. A hydrogen isotope accelerator mass spectrometer in accordance with claim 6 wherein said detector system includes two multi-anode gas ionization chambers.
8. A hydrogen isotope accelerator mass spectrometer as defined in claim 7, wherein the two multi-anode gas ionization chambers are respectively connected to the second faraday cup and the third faraday cup for measuring each ion content in the first ion set and the second ion set.
9. A hydrogen isotope accelerator mass spectrometer as defined in claim 1, wherein the mass analyzer includes an electromagnet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202311107621.5A CN117457471A (en) | 2023-08-30 | 2023-08-30 | Mass spectrometer of hydrogen isotope accelerator |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311107621.5A CN117457471A (en) | 2023-08-30 | 2023-08-30 | Mass spectrometer of hydrogen isotope accelerator |
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| CN117457471A true CN117457471A (en) | 2024-01-26 |
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| CN202311107621.5A Pending CN117457471A (en) | 2023-08-30 | 2023-08-30 | Mass spectrometer of hydrogen isotope accelerator |
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