CN115901913A - Isotope separation and enrichment method using multipole rod mass analyzer - Google Patents
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Abstract
The invention discloses an isotope separation enrichment method by utilizing a multipole rod mass analyzer, which comprises the steps of injecting a high-concentration solution into a first chamber, and ionizing the high-concentration solution by using an ICP (inductively coupled plasma) ion source component in the first chamber to form plasma; the plasma vacuum chamber formed by the first chamber enters an ion extraction system, and the extracted ions are guided into a subsequent multipole rod mass analyzer; adjusting the voltage applied to the multipole rod mass analyzer according to different elements in the element sample to be enriched, so that a specific isotope to be separated passes through the multipole rod mass analyzer and enters a subsequent receiver; the invention can improve the ionization efficiency of the prior art, reduce the construction cost of the device and reduce the maintenance difficulty.
Description
Technical Field
The invention belongs to the technical field of analysis and test, and particularly relates to an isotope separation and enrichment method.
Background
Most elements in the periodic table have various isotopes, and in the fields of modern industry, medicine, and biology, geochemistry, specific isotopes of the elements need to be highly enriched. For example, natural U has two isotopes, 235U and 238U, with abundances of 0.7% and 99.3%, respectively, while nuclear fuel can only use 235U with high purity, so that the 235U with low abundance in nature needs to be purified and highly enriched to produce nuclear fuel; for another example, in the medical field, the condition of metabolic abnormality is often determined by enriched isotope, one of the routine items of physical examination is helicobacter pylori infection, the item is detected by carbon 13 urea breath test, and carbon 13 enriched raw material is used; in various environmental and chemical analysis fields, isotopes of various metal and non-metal elements are often used to trace migration or chemical reaction processes of pollutants, and these trace species are also highly enriched isotopes.
Isotope separation and enrichment technologies are various, and for the enrichment of gas isotopes, a thermal diffusion or low-temperature rectification method is generally adopted; for the enrichment of 235U, a gas centrifuge and a specific wavelength laser ionization method can be utilized; for some isotopes of specific elements, such as 6Li, ion exchange methods can be used. However, these methods are all dedicated methods, and dedicated apparatuses and methods must be used to separate and enrich specific elements and isotopes, but these dedicated apparatuses and methods cannot be applied to other types of isotopic enrichment, so that apparatuses and methods with certain versatility need to be found.
The existing general isotope separation and enrichment method is an electromagnetic separation method, the device thereof is similar to a large-scale magnetic mass spectrometer, the prior art implementation scheme is a magnetic isotope separation device, the structure and the schematic diagram of which are shown in figure 1: the key components of the ion source comprise an ion source, a fan-shaped magnetic field and an isotope receiving cup, the principle of the ion source is generally solid thermal surface ionization or gas electron bombardment ionization, elements ionized by the ion source are accelerated in a high-vacuum chamber through an electric field to form ion beam current which enters the fan-shaped magnetic field and is deflected under the action of a Lorentz effect under the magnetic field, the deflection radiuses of ions with different mass/charge ratios are different, and specific isotopes can be selected by adjusting the magnetic field intensity and are received by the isotope receiving cup after the fan-shaped magnetic field.
Through research and analysis of the applicant, the defects of the existing method comprise:
(1) The ionization efficiency is low: the ionization efficiency of the hot surface ionization is about 1 percent, and the gas electron bombardment ionization efficiency is only about 0.01 percent.
(2) The plants suitable for this method are costly to build: magnetic isotope separation devices are limited by the ionization efficiency of the ion source, and in order to obtain sufficient isotope enrichment in a given time, the physical size of the device must be increased to support a sufficiently strong isotope ion beam current. The large size of the high vacuum system and the magnetic sector are both prohibitively expensive. Commercial magnetic mass spectrometers (the same basic principle as magnetic isotope separation devices) with a radius of 300mm are priced in millions of RMB, can support ion beam currents of the order of 10-9A, and cannot achieve meaningful isotope enrichment. The magnetic isotope separation device with industrial enrichment capacity is almost built for national financial fund transfer, for example, a calalutron device in a national laboratory of oak ridge, a Lanzhou heavy ion device in China and the like, and the construction and operation costs are extremely high, and the device can be supported only by special fund transfer of a central government.
(3) The equipment formed by the method has high maintenance difficulty: because the large-scale magnetic isotope separation device is a special facility and the ion source is also in the vacuum cavity, professional operation and maintenance are needed.
Therefore, new devices and new methods are needed to solve the corresponding technical problems.
Disclosure of Invention
In view of the above, there is a need to overcome at least one of the above-mentioned deficiencies in the prior art. The invention provides an isotope separation and enrichment method by utilizing a multipole rod mass analyzer, which comprises the following steps:
s1, preprocessing:
preparing a high-concentration solution containing an element sample to be enriched, converting the high-concentration solution into aerosol through an atomizing device, and introducing the aerosol into a high-efficiency ion source (ICP);
s2, ionizing the high-concentration solution of the element sample to be enriched
Ionizing the high concentration solution in the first chamber using an ICP ion source assembly comprising a rectangular tube to form a plasma;
or an isotope collection apparatus.
In the technical scheme, an ICP ion source component ionizes high-concentration solution containing elements to be detected through plasma formed by inductive coupling and generates ions, the ions enter an ion extraction system in a vacuum chamber through a vacuum interface, the ions generated by the ICP ion source component are extracted and guided into a multipole rod mass analyzer on the rear side, the multipole rod mass analyzer is controlled through an electronic control system, a specific isotope is specified to pass through the analyzer, other isotopes are shunted to other places, the isotope passing through the analyzer is received by a receiver and is subjected to signal amplification through an amplifier to form analysis-recognizable information or is received by an isotope collection device and redundant charges are led out, so that the ions are deposited on the surface of the isotope collection device, and after enough isotopes are collected, the isotope collection device is taken out and the isotopes are extracted by a chemical method such as acid soaking to obtain analyzable data.
The technical scheme provides a new design scheme, and the problems of low ionization efficiency, high construction cost and high operation and maintenance difficulty of a large-scale magnetic isotope separation device related to the existing method can be solved by adopting an ion source for ionizing a high-concentration solution to form a certain concentration and obtaining a specified isotope through a multipole rod mass analyzer, so that the method is utilized to construct a high-efficiency, low-cost and universal isotope enrichment device.
In addition, the isotope separation and enrichment method by using the multipole rod mass analyzer disclosed by the invention also has the following additional technical characteristics:
further, the receiver is a pluggable receiver for receiving the isotope screened and separated by the multipole rod mass analyzer.
Further, the receiver is a faraday cup which can be disassembled and replaced, and after enough isotopes are collected, the faraday cup is taken out and the isotopes are extracted by a chemical method.
Still further, the chemical process is an acid soak process.
Furthermore, the Faraday cup adopts a cup body structure made of simple substance graphite or inert metal materials.
Further, the Faraday cup is grounded
Further, the ICP ion source assembly further comprises a high-concentration solution container and an inductive coupling component which interacts with the high-concentration solution container to generate plasma.
Further, the multipole rod mass analyzer is a quadrupole rod mass analyzer or a hexapole rod mass analyzer.
Further, the vacuum chamber has a vacuum chamber top cover for facilitating disassembly, assembly, maintenance of the ion extraction system, the multipole rod mass analyzer.
Further, the concentration of the high concentration solution is greater than or equal to 1000ppm or 0.1wt%.
Further, the receiver and the bore of the vacuum interface and the ion source are in an unobstructed line, i.e., a straight-through ion-optical configuration.
Further, adopt short multipole pole, so combine together with other structures of this device, further promote the ion through rate, also can further reduce this device volume and cost simultaneously, the length of short multipole pole can be calculated and experimental the confirming according to expected value. The short multipole rods can be short quadrupole rods or short hexapole rods, etc.
Further, the electronic control system comprises an ICP radio frequency power supply for exciting plasma, a quadrupole radio frequency power supply for screening and separating isotopes, and an electronic software, hardware and firmware control system for correspondingly controlling all functional devices, such as a vacuum pump and other units to normally work.
The firmware control system mainly comprises a power distribution module: the 220V AC power supply is converted into a 12V/24V/48V DC power supply. 2. An instrument control module: the sensor data reading module is used for controlling the vacuum system control module, the ICP radio frequency power supply module, the quadrupole radio frequency power supply module, the signal amplifier module, the pneumatic solenoid valve control module and the sensor data reading of each module unit. And 3.ICP radio frequency power supply module. 4. Quadrupole pole radio frequency power module. 5. A vacuum system control module. 6. And a signal amplifier module. 7. The pneumatic solenoid valve control module: ICP gas path control and vacuum interface closing control. 8. A communication module: data transmission and analog-digital control between the data processing system and the instrument control module are realized by using Ethernet or optical fiber communication.
Furthermore, the vacuum interface adopts a salt-tolerant large-aperture cone structure. During operation, high-concentration single element solution is introduced, so that the general isotope separation device based on the quadrupole rod adopts salt-tolerant design (such as low-cost consumables and large-aperture cones) at the ICP and the vacuum interface part (corresponding to the sampling cone and the intercepting cone of the multipole rod).
The method has the following characteristics.
(1) The ionization efficiency is high. Ionization is realized by utilizing an ICP principle, and 100 percent ionization can be realized for almost all metal elements. Can realize continuous sample introduction under the laboratory condition and does not need to open the vacuum cavity frequently.
(2) The universality is good, and the enrichment of various isotopes can be realized. Separation and enrichment of isotopes of all metals ranging from the lightest metal, li, to the heaviest metal, U, can be achieved using quadrupole rod technology.
(3) The method involves a low construction cost of the device. The device can be modified based on a commercial quadrupole ICP mass spectrometer. Commercial quadrupole ICP mass spectrometers are currently available in the range of 50-100 million renminbi. Compared with a magnetic isotope separation device, the device is extremely economical.
(4) The operation and maintenance are simple. The operations of opening the vacuum cavity and replacing the faraday cup can be performed by related personnel only through basic training.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic view illustrating a construction principle of a conventional magnetic isotope separation apparatus of the present invention;
fig. 2 is a schematic diagram of an embodiment of the isotope separation enrichment apparatus with a multipole rod mass analyzer of the present invention.
The device comprises a torch tube 1, a torch tube 2, a vacuum interface 3, a quadrupole rod mass analyzer 4, a turbo molecular vacuum pump 5, a plug-in isotope collector 6, a resistance amplifier 7, an RF coil 8, a vacuum chamber 9, a sealing ring 10, a detachable upper cover and a first chamber 11.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative only and should not be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "bottom", "top", "front", "rear", "inner", "outer", "lateral", "vertical", and the like, indicate orientations and positional relationships based on the orientations and positional relationships shown in the drawings, are used only for convenience in describing the present invention and for simplification of description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise specifically stated or limited, the terms "coupled," "communicating," "connected," "coupled," and "engaged" are to be construed broadly and may include, for example, a fixed coupling, an integral coupling, and a detachable coupling; may be communication within two elements; can be directly connected or indirectly connected through an intermediate medium; "mating" may be a surface-to-surface mating, a point-to-surface or line-to-surface mating, and also includes a hole axis mating, and it is obvious to those skilled in the art that the above terms have specific meanings in the present invention.
A multi-robot scheduling method for an inspection robot and a fire-extinguishing robot system according to the present invention will be described with reference to the accompanying drawings, in which fig. 1 is a schematic view of the construction principle of the conventional magnetic isotope separation apparatus according to the present invention; fig. 2 is a schematic diagram of an embodiment of the isotope separation enrichment method using a multipole rod mass analyzer in accordance with the present invention.
As shown in fig. 2, according to an embodiment of the present invention, an isotope separation enrichment method using a multipole rod mass analyzer includes:
s1, preprocessing:
preparing a high-concentration solution containing an element sample to be enriched, converting the high-concentration solution into aerosol through an atomizing device, and introducing the aerosol into a high-efficiency ion source;
meanwhile, a molecular pump is used for vacuumizing a vacuum chamber internally provided with a multipole rod mass analyzer, a plug-in receiver and a signal amplification circuit;
s2, ionizing the high-concentration solution of the element sample to be enriched
Ionizing the high concentration solution in the first chamber using an ICP ion source assembly comprising a rectangular tube to form a plasma;
s3, ion splitting in the vacuum chamber
The ions formed in the first chamber in S2 enter the vacuum chamber through a vacuum interface between the first chamber and the vacuum chamber, and enter an ion extraction system, and the extracted ions are guided into a subsequent multipole mass analyzer; and adjusting the voltage applied to the multipole rod mass analyzer according to different elements in the element sample to be enriched, so that the required separated isotopes pass through the multipole rod mass analyzer and enter a subsequent receiver.
In addition, the isotope separation and enrichment method by using the multipole rod mass analyzer disclosed by the invention also has the following additional technical characteristics:
according to some embodiments of the invention, the receiver is a pluggable receiver for receiving the screened isotopes from the multipole rod mass analyser.
According to some embodiments of the invention, the receiver is a faraday cup that is removably replaceable and, after sufficient isotope has been collected, is removed and the isotope extracted chemically.
Further, the chemical method is an acid soaking method.
Further, the Faraday cup adopts a cup body structure made of simple substance graphite or inert metal materials.
Further, the faraday cup is grounded.
According to an embodiment of the present invention, the ICP ion source assembly further includes a high concentration solution container, and an inductive coupling part that interacts with the high concentration solution container to generate plasma.
According to some embodiments of the invention, the multipole rod mass analyser is a quadrupole rod mass analyser or a hexapole rod mass analyser.
According to an embodiment of the invention, the vacuum chamber has a vacuum chamber top cover for facilitating disassembly, assembly, maintenance of the ion extraction system, the multipole rod mass analyser. The top cover can be conveniently disassembled, the maintenance of the ion extraction system and the quadrupole rod is carried out, and the Faraday cup is replaced to collect isotopes.
The control function device comprises an electronic software, hardware and firmware control system for normal operation of units such as a vacuum pump.
According to an embodiment of the invention, the high concentration solution has a concentration of 1000ppm or more or 0.1wt%.
According to an embodiment of the invention, the receiver and the cone of the vacuum interface and the ion source are in a line that is not blocked, i.e. a straight-through ion-optical configuration.
Further, adopt short multipole, so combine together with other structures of this device, further promote the ion through rate, also can further reduce this device volume and cost simultaneously, the length of short multipole can be calculated and experimental the confirming according to expected value. The short multipole rods can be short quadrupole rods or short hexapole rods, etc.
According to the embodiment of the invention, the electronic control system comprises an ICP radio frequency power supply for exciting plasma, a quadrupole radio frequency power supply for screening and separating isotopes and an electronic software, hardware and firmware control system for controlling the normal operation of various functional devices, such as a vacuum pump and other units.
The firmware control system mainly comprises a power distribution module: the 220V AC power supply is converted into a 12V/24V/48V DC power supply. 2. An instrument control module: the sensor data reading module is used for controlling the vacuum system control module, the ICP radio frequency power supply module, the quadrupole radio frequency power supply module, the signal amplifier module, the pneumatic solenoid valve control module and the sensor data reading of each module unit. And 3.ICP radio frequency power supply module. 4. Quadrupole pole radio frequency power module. 5. A vacuum system control module. 6. And a signal amplifier module. 7. The pneumatic solenoid valve control module: ICP gas path control and vacuum interface closing control. 8. A communication module: and the data processing system and the instrument control module are subjected to data transmission and analog-digital control by using Ethernet or optical fiber communication.
According to the embodiment of the invention, the vacuum interface adopts a salt-tolerant large-aperture cone structure. During operation, high-concentration single element solution is introduced, so that the general isotope separation device based on the quadrupole rod adopts salt-tolerant design (such as low-cost consumables and large-aperture cones) at the ICP and the vacuum interface part (corresponding to the sampling cone and the intercepting cone of the multipole rod).
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Any reference to "one embodiment," "an embodiment," "example embodiment," etc., means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. This schematic representation in various places throughout this specification does not necessarily refer to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the purview of one skilled in the art to effect such feature, structure, or characteristic in connection with other ones of the embodiments.
While specific embodiments of the invention have been described in detail with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this invention. In particular, reasonable variations and modifications are possible in the component parts and/or arrangements of the subject combination arrangement within the scope of the foregoing disclosure, the drawings and the appended claims without departing from the spirit of the invention. Except variations and modifications in the component parts and/or arrangements, the scope of which is defined by the appended claims and equivalents thereof.
Claims (11)
1. An isotope separation and enrichment method by utilizing a multipole rod mass analyzer is characterized by comprising the following steps of,
s1, preprocessing:
preparing a high-concentration solution containing an element sample to be enriched, converting the high-concentration solution into aerosol through an atomizing device, and introducing the aerosol into a high-efficiency ion source;
s2, ionizing the high-concentration solution of the element sample to be enriched
Ionizing the high concentration solution in the first chamber using an ICP ion source assembly comprising a rectangular tube to form a plasma;
s3, ion splitting in the vacuum chamber
The ions formed in the first chamber in S2 enter the vacuum chamber through a vacuum interface between the first chamber and the vacuum chamber, and enter an ion extraction system, and the extracted ions are guided into a subsequent multipole mass analyzer; and adjusting the voltage applied to the multipole rod mass analyzer according to different elements in the element sample to be enriched, so that the required separated isotopes pass through the multipole rod mass analyzer and enter a subsequent receiver.
2. The method of claim 1, wherein the receiver is a pluggable receiver configured to receive the screened isotopes from the multipole rod mass analyzer.
3. The method of claim 1, wherein the receiver is a faraday cup that can be removed and replaced, and after sufficient isotope has been collected, the faraday cup can be removed and the isotope can be chemically extracted.
4. The method of claim 3, wherein the chemical process is acid soaking.
5. The method of claim 3, wherein the Faraday cup is a cup made of elemental graphite or an inert metal material.
6. The method of claim 3, wherein the Faraday cup is grounded.
7. The isotope separation and enrichment apparatus with a multipole rod mass analyzer in accordance with claim 1, wherein the ICP ion source assembly further comprises a high concentration solution container, and an inductive coupling component that interacts with the high concentration solution container to generate a plasma.
8. The method of claim 1, wherein the multipole rod mass analyzer is a quadrupole rod mass analyzer or a hexapole rod mass analyzer.
9. The method of claim 1, wherein the vacuum chamber has a vacuum chamber lid for easy disassembly, assembly, and maintenance of the ion extraction system, the multipole rod mass analyzer.
10. The method of claim 1, wherein the high concentration solution has a concentration of 1000ppm or more or 0.1wt% or more.
11. The method of claim 1, wherein the receiver and the bore of the vacuum interface and the ion source are in an unobstructed line.
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