CN113156032B - Mass spectrum system and method for simultaneously measuring isotope abundance and impurity content - Google Patents
Mass spectrum system and method for simultaneously measuring isotope abundance and impurity content Download PDFInfo
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Abstract
The invention provides a mass spectrum system and a method for simultaneously measuring isotope abundance and impurity content, wherein the mass spectrum system comprises: the ion source system is used for feeding and leading out multi-charge-state ion beam current; the acceleration subsystem is used for accelerating the multi-charge-state ions and simultaneously focusing and analyzing the energy and momentum of the multi-charge-state ions; and the detector subsystem is used for detecting the beam current of the isotope ions, distinguishing two isobaric elements with the same quantity and distinguishing two ions with the same mass-to-charge ratio. The invention can disintegrate all molecular ions by utilizing the electron cyclotron resonance ion source with multiple charge states, and can distinguish isobaric ions with the same quantity by utilizing the thin film absorption technology and the single particle energy detection technology, thereby obviously improving the sensitivity of measuring the isotopic abundance, reducing the lower limit of detection of each element, and realizing the simultaneous, accurate and rapid measurement of the isotopic abundance ratio and the impurity content in the material or the sample.
Description
Technical Field
The invention belongs to the technical field of mass spectrometry, and particularly relates to a mass spectrometry system and a mass spectrometry method for simultaneously measuring isotope abundance and impurity content.
Background
Mass spectrometry (also called Mass spectrometry, abbreviated as MS) is a spectroscopic method parallel to spectroscopy, and generally means a special technique widely applied in various subject fields for identifying compounds by preparing, separating, and detecting gas phase ions. The principle of mass spectrometry is to ionize the substance to be measured, separate according to the mass-to-charge ratio of the ions, measure the intensity of various ion spectral peaks, and realize the analysis.
Traditional MS includes inorganic MS, isotope MS and organic MS, wherein the inorganic MS is used for measuring the content of various elements and impurities in a sample; isotope MS is used to measure the ratio of abundance between different isotopes in an element in a sample.
Inorganic MS and isotope MS are two different MS, and simultaneous measurement of isotope abundance and impurity content cannot be achieved with one MS. The inorganic MS mainly includes inductively coupled plasma mass spectrometry (ICP-MS), time-of-flight mass spectrometry (TOF-MS), and the like. The isotope MS mainly comprises gas isotope MS, thermal surface ionization mass spectrum (TIMS), multi-receiving inductively coupled plasma mass spectrum ICP-MS, Accelerator Mass Spectrum (AMS) and the like. Inductively coupled plasma mass spectrometry ICP-MS (four-level rod) can be used for measuring isotope abundance ratio in some cases due to high measuring speed and simple sample pretreatment.
Because the existence of interfering ions such as molecular ions and isobaric ions influences the improvement of measurement sensitivity (or the reduction of the lower detection limit), the simultaneous, accurate and rapid measurement of the isotopic abundance ratio and the impurity content in the isotope material is difficult to realize in any MS. For example, calcium isotope materials including isotopes of 40Ca, 41Ca, 42Ca, 46Ca, 48Ca and the presence of impurities Be, Mg, Ar, K, Sc, etc. cannot achieve measurement of isobaric impurities 40Ar and 40K ions due to the presence of 40Ca ions, and cannot achieve measurement of 41Ca and 41K ions due to the presence of 40CaH molecular ions.
At present, measurement aiming at isotopic abundance and impurity content in materials and samples is carried out on two different MS in two steps, and the specific steps are as follows:
the first step is to measure the isotopic abundance ratio in the material by using isotopic MS;
and secondly, preparing a sample, removing main elements by using a chemical reaction, extracting impurity elements, and measuring by using an inorganic MS to obtain the content of impurities in the material. Thus, there are two problems, one is that the two-step measurement results in a long time, and the sample preparation is required, resulting in a decrease in the accuracy of the measurement.
With the development of scientific technology, in many fields such as geology, geography, nuclear industry, biomedicine, semiconductors and metal materials, it is necessary to measure not only the isotopic abundance ratio but also the contents of impurities or other elements in the material or sample. Such samples and materials are: solid materials such as boron, lithium, calcium, iron, uranium, various mineral substances, semiconductor materials and the like; gaseous materials such as oxygen, hydrogen, helium, nitrogen, argon, and the like; and liquid isotope materials such as deuterium-depleted water, tritium water, various liquid materials and reagents, and the like. It is desirable to measure the isotopic abundance in a sample while also giving an accurate measure of the impurity (or dopant) content.
If a MS is used for simultaneously obtaining the data of the isotopic abundance and the impurity content in the sample, the following three conditions are required:
firstly, sample preparation cannot be carried out, and sample introduction is uniform;
secondly, the capability of removing background such as molecular ions and molecular fragment ions is required;
third, the ability to identify isobaric ion backgrounds of the same amount and mass-to-charge ratio. After the three conditions are met, the isotope abundance sensitivity of the instrument is remarkably improved, and the lower limit of the detection of impurity elements is greatly reduced.
Disclosure of Invention
The invention aims to provide a mass spectrum system and a mass spectrum method for simultaneously measuring the isotope abundance and the impurity content, which can break down all molecular ions and realize the simultaneous, accurate and rapid measurement of the isotope abundance ratio and the impurity content in materials or samples.
The invention provides a mass spectrum system for simultaneously measuring isotope abundance and impurity content, which comprises: the ion source subsystem is used for injecting and extracting multi-charge-state ion beam current and comprises a sample injector and a multi-charge-state electron cyclotron resonance ion source connected with the sample injector; the acceleration subsystem is used for accelerating multi-charge-state ions and simultaneously focusing and analyzing the energy and momentum of the multi-charge-state ions, and is connected with the electron cyclotron resonance ion source; and the detector subsystem is used for detecting the beam current of the isotope ions, distinguishing two isobaric elements with the same quantity and distinguishing two ions with the same mass-to-charge ratio, and comprises a group of multi-receiving Faraday cups connected with the acceleration subsystem, at least one path of energy absorption film connected with the multi-receiving Faraday cups and detectors which are the same in quantity with the energy absorption films and connected with the corresponding energy receiving films.
Preferably, the ion source system further comprises a first high pressure stage housing the injector and ion source.
Preferably, the acceleration subsystem comprises a pre-accelerator connected to an electron cyclotron resonance ion source of multiple charge states, an electrostatic analyser connected to the pre-accelerator and a magnetic analyser connected to the electrostatic analyser.
Preferably, the acceleration subsystem further comprises an accelerator connected between the electrostatic analyzer and the magnetic analyzer.
Preferably, the acceleration subsystem further comprises a second high voltage stage enclosing the ion source subsystem, pre-accelerator, and electrostatic analyzer.
Preferably, the number of faraday cups is equal to the sum of the number of isotopes to be measured and the number of impurity species.
Preferably, the detector is a single particle energy detector.
Preferably, the detector is a semiconductor detector, a gas detector or a liquid energy detector.
The invention also provides a mass spectrometry method for simultaneously measuring the isotope abundance and the impurity content, which comprises the following steps:
s1: the sample injector acts on the isotope sample to convert the isotope sample into a gas state or a fog state;
s2: the electron cyclotron resonance ion source with multiple charge states enables the isotope sample which becomes gaseous state or fog state to generate ions with multiple charge states;
s3: the pre-accelerator accelerates multi-charge-state ions;
s4: the electrostatic analyzer carries out energy focusing on the accelerated multi-charge-state ions;
s5: the magnetic analyzer performs momentum analysis on the multi-charge-state ions subjected to energy focusing, and distinguishes ions with different mass-to-charge ratios according to the size of the mass-to-charge ratio;
s6: measuring the ion beam current by a multi-receiving Faraday cup;
s7: the energy absorption film distinguishes isobaric ions;
s8: the detector records each isotope, each element, each isobaric ion beam current or single particle counting rate.
Preferably, for steps S7 and S8, when two isobaric elements with the same energy and the same charge state pass through the energy absorption film, the energy lost in the energy absorption film is different; after passing through the energy absorption film, the residual energy of the energy absorption film is different, and the detector measures the energy of the energy absorption film and counts the energy of the energy absorption film, and identifies two isobaric elements with the same quantity and the proportion between the isobaric elements.
The invention can disintegrate all molecular ions by utilizing the electron cyclotron resonance ion source with multiple charge states, and can distinguish isobaric ions by utilizing the thin film absorption technology and the single particle energy detection technology, thereby obviously improving the sensitivity of measuring the isotopic abundance, reducing the lower limit of detection of each element, and realizing the simultaneous, accurate and rapid measurement of the isotopic abundance ratio and the impurity content in the material or the sample.
Drawings
FIG. 1 is a schematic diagram of a mass spectrometry system of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention discloses a mass spectrum system for simultaneously measuring the abundance and the impurity content of isotopes, which is used in the fields of geology, geography, nuclear industry, biomedicine, semiconductors, metal materials and the like.
As shown in fig. 1, the mass spectrometry system of the present invention includes an ion source system 10, an acceleration subsystem, and a detector subsystem 30 connected in series.
The ion source subsystem 10 is configured to sample and extract a multi-charge-state ion beam current, and the ion source subsystem 10 includes a sample injector 11, a multi-charge Electron Cyclotron Resonance (MECR) ion source 12 connected to the sample injector 11, and a first high-voltage stage 13, where the sample injector 11 and the ion source 12 are enclosed by the first high-voltage stage 13, so that the ion source subsystem 10 is insulated from the acceleration subsystem.
The sample injector 11 is used for solid, liquid or gaseous isotope samples, and high-temperature heating, laser beam, electron beam or ion beam is used for reacting with the isotope samples, so that the isotope samples are converted into gaseous or mist states. The first high voltage stage 13 is used for support of the acceleration subsystem and provides isolation between the ion source subsystem 10 and the acceleration subsystem.
A multiple charge state refers to a charge state in which the ion source strips away more than two electrons, i.e., 2+, 3+, 4+, and even fully stripped. The ion beam current extracted by the ion source 12 can be in the range of 10nA-10mA (particle beam current) and is continuously adjustable. The invention adopts the electron cyclotron resonance ion source 12 with multiple charge states, and the microwave frequency of the MECR ion source 12 is in the range of 5-50 GHz.
The MECR ion source 12 belongs to an ultra-strong ionization technology, and the ultra-strong ionization refers to an ion source capable of generating multi-charge state ions for MS analysis, and has the following two functions: firstly, multi-charge-state ions (no molecular ions) are led out from the ion source, and when the charge state is more than or equal to +3, the molecular ions are completely disintegrated, so that the interference problem of the molecular ions, molecular fragment ions and the like is solved; second, the energy of the ions is increased, and the magnitude of the ion energy is proportional to the magnitude of the charge state. The higher the charge state, the higher the ion energy, and the more advantageous it is to distinguish isobaric species.
The acceleration subsystem is used to accelerate the ions to a higher energy, while focusing (or double focusing) and analyzing the ions in both energy and momentum. The acceleration subsystem 20 includes a pre-accelerator 21 supported by the first high voltage stage 13 and connected to the multi-charge state ecr ion source 12, an electrostatic analyzer 22 connected to the pre-accelerator 21, an accelerator 23 connected to the electrostatic analyzer 22, a magnetic analyzer 24 connected to the accelerator 23, and a second high voltage stage 25.
The pre-accelerator 21 is used to initially accelerate ions extracted from the ion source 12 in order to better double focus the ions. The acceleration voltage of the pre-accelerator 21 is typically in the range of 20-200kV and is adjustable. The electrostatic analyzer 22 is used for energy focusing, the purpose of which is to eliminate interference of the main isotope high and low energy tails with other isotope and impurity species.
The accelerator 23 is used to further accelerate the ions to a higher energy in order to discriminate between two isobaric ions, such as 40Ca and 40K ions. If there is no isobaric interference, the magnetic analyzer 24 may be connected directly to the electrostatic analyzer 22 without an accelerator.
The level of ion energy depends on two aspects: on one hand, the mass number of two isobaric ions to be distinguished is determined, and the larger the mass number is, the higher the energy for accelerating the ions is; on the other hand, the higher the charge state, the higher the energy, also depending on the level of the charge state selected. The voltage of the accelerator 23 is generally in the acceleration voltage range of 100-800 kV. The accelerator 23 may not be required if there is no isobaric interference.
The magnetic analyzer 24 is used for momentum analysis to distinguish ions of different mass-to-charge ratios according to the mass-to-charge ratio.
A second high voltage stage 25 encloses the ion source subsystem 10, pre-accelerator 21 and electrostatic analyzer 22.
The detector subsystem 30 is used for detecting the beams of isotope ions, distinguishing two kinds of isobaric elements and distinguishing two kinds of ions with the same mass-to-charge ratio, and simultaneously recording the beam or single particle counting rate of each isotope, each element, each isobaric element ion.
The detector subsystem 30 includes a set of multi-reception faraday cups 31 connected to the magnetic analyzer 24, one or more (e.g., 2-4) energy absorbing films 32, and the same number of detectors 33 as the number of energy absorbing films 32, wherein the energy absorbing films 32 are connected to the faraday cups 31 and the detectors 33 are connected to the corresponding energy absorbing films 32.
A multi-reception faraday cup 31 is used to measure the beam current of the ions, the number of faraday cups being equal to the sum of the number of isotopes and the number of impurity species to be measured. For example, calcium isotopes are measured, the isotopes of which are: 40Ca, 41Ca, 42Ca, 44Ca, 46Ca and 48Ca, and also K, Be, Mg, P, Sr and other impurities. The number of faraday cups used is typically set in the range of 5-50 and even greater.
The energy absorption film 32 is used to distinguish isobaric ions, and the energy absorption film 32 refers to a solid film of metal, semiconductor, insulator or a segment of gas material equivalent to the solid film with a very uniform thickness. The energy absorbing film 32 has a thickness of 30-3000 nm.
When two isobaric elements with the same energy and the same charge state, such as 40Ca +11 and 40K +11, pass through the energy-absorbing film 32 due to their different atomic numbers, the energy lost in the energy-absorbing film 32 is also different. After passing through the energy absorption film 32, the residual energy of the film itself is different, and the detector 33 can be used for measuring the energy and the counted amount of the film, so that two isobaric elements and the proportion of the film can be identified.
The detector 33 is a single particle energy detector, the single particle energy detector is capable of measuring the energy and the counting rate of charged particles, the number of the detectors 33 is the same as that of the energy absorption films 32, and the detectors 33 are generally semiconductor detectors, gas detectors or liquid energy detectors.
By utilizing the energy absorption film and the detector, the problem of interference of the background of the same amount of the alloplastic ions and the ions with the same mass-to-charge ratio is solved, the most important essential problem which troubles MS measurement is solved, the isotope abundance sensitivity is obviously improved and is improved by more than 10000 times; the lower limit of the detection of the impurity elements can be greatly reduced by more than 1000 times, and the sensitivity of the isotope abundance and the content of the impurity can be simultaneously measured.
The invention can disintegrate all molecular ions by utilizing the electron cyclotron resonance ion source with multiple charge states, and can distinguish isobaric ions by utilizing the thin film absorption technology and the single particle energy detection technology, thereby obviously improving the sensitivity of measuring the isotopic abundance, reducing the lower limit of detection of each element, and realizing the simultaneous, accurate and rapid measurement of the isotopic abundance ratio and the impurity content in the material or the sample; the mass spectrometry system of the invention is based on Isotopic (isotoic) and Inorganic (Inorganic) MS of MECR ion source, i.e. II-MS.
The invention can be very goodThe method solves the three problems of sample preparation, molecular background and isobaric background in the prior art, greatly improves the measurement sensitivity, and has isotope abundance sensitivity which is better than 10-12 and is more than 10000 times better than that of the current double-focusing isotope MS. The lower limit of the content of the impurity element to be detected was less than 0.1ppt (10 in the case of a sample amount of 1mg, 10) 6 Atomic), by more than 1000 times than the current high resolution ICP-MS.
The invention also discloses a mass spectrum method for simultaneously measuring the isotope abundance and the impurity content, which comprises the following steps:
s1: the sample injector 11 acts on the isotope sample to convert the isotope sample into a gaseous state or a mist state;
s2: the multiple charge state electron cyclotron resonance ion source 12 causes the isotope sample that has become gaseous or mist to generate multiple charge state ions;
s3: the pre-accelerator 21 accelerates ions of multiple charge states;
s4: the electrostatic analyzer 22 energy-focuses the accelerated multi-charge state ions;
s5: the magnetic analyzer 24 performs momentum analysis on the multi-charge-state ions subjected to energy focusing, and distinguishes ions with different mass-to-charge ratios according to the size of the mass-to-charge ratio;
s6: a multi-reception faraday cup 31 measures the beam current of ions;
s7: the energy absorption film 32 distinguishes isobaric ions;
s8: the detector 33 records the ion beam current or single particle count rate for each isotope, each element, each isobaric ion, or both.
In steps S7 and S8, when two isobaric elements with the same energy and the same charge state, such as 40Ca +11 and 40K +11, pass through the energy-absorbing film 32 due to their different atomic numbers, the energy lost in the energy-absorbing film 32 is also different. After passing through the energy absorption film 32, the residual energy of the two isobaric elements is different, and the detector 33 is used for measuring the energy of the two isobaric elements and the number of the isobaric elements and the ratio of the two isobaric elements.
The invention has the following advantages:
firstly, the combination of the multi-charge electron cyclotron resonance ion source and the single particle energy detector is adopted, so that the abundance sensitivity of isotope measurement is remarkably improved (by more than 10000 times), the detection lower limit of impurity content measurement is greatly reduced (by more than 1000 times), and the difficult problems that the former content is too low and the measurement is difficult can be solved. For example: accurate measurement of high purity semiconductor impurities and doping; isotope fingerprint and element fingerprint problems in article identification, and the like.
And secondly, the simultaneous measurement of the isotope abundance ratio and the impurity content in the isotope material can be realized. The mass spectrum system of the invention has three working modes: firstly, simultaneously measuring the isotope abundance ratio and the impurity content mode; second, the isotopic abundance ratio model is measured separately. Third, the impurity level mode is measured separately. For example, the chronogeology K-Ar method, Ar-Ar method, and U-Ph method provide simultaneous and accurate measurement of isotopes and elements.
Thirdly, due to the improvement of the measurement sensitivity, the problem that some very important existing measurement data are not accurate enough can be realized. For example, many important inventory sample accurate measurement problems are addressed.
Fourthly, sample preparation is not needed, so that the sample measurement accuracy is greatly improved. Because the loss of impurities or the influence of isotope fractionation must be caused in the sample preparation process.
Fifthly, the measuring time is greatly saved. Previous sample preparation and measurement typically required hours to tens of hours. The system of the invention only needs 1-15 minutes of sample introduction and measurement time because sample preparation is not needed.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. A mass spectrometry system for simultaneously measuring isotopic abundance and impurity content, comprising:
the ion source system is used for injecting and extracting multi-charge-state ion beam current and comprises a sample injector and a multi-charge-state electron cyclotron resonance ion source connected with the sample injector;
the acceleration subsystem is used for accelerating the multi-charge-state ions and simultaneously focusing and analyzing the energy and momentum of the multi-charge-state ions, and is connected with the electron cyclotron resonance ion source; and
the detector subsystem is used for detecting the beam current of isotope ions, distinguishing two isobaric elements with the same quantity and distinguishing two ions with the same mass-to-charge ratio and comprises a group of multi-receiving Faraday cups connected with the acceleration subsystem, at least one path of energy absorption film connected with the multi-receiving Faraday cups and detectors which are the same in quantity with the energy absorption films and connected with the corresponding energy receiving films;
the ion source system further comprises a first high-pressure rack, and the first high-pressure rack wraps the sample injector and the ion source;
the acceleration subsystem comprises a pre-accelerator connected with an electron cyclotron resonance ion source with multiple charge states, an electrostatic analyzer connected with the pre-accelerator, a magnetic analyzer connected with the electrostatic analyzer, an accelerator connected between the electrostatic analyzer and the magnetic analyzer, and a second high-voltage stage; the second high-voltage gantry encloses the ion source subsystem, pre-accelerator, and electrostatic analyzer;
the detector is a single-particle energy detector, a semiconductor detector, a gas detector or a liquid energy detector.
2. The mass spectrometry system of claim 1, wherein the number of faraday cups is equal to the sum of the number of isotopes to be measured and the number of impurity species.
3. A mass spectrometry method for simultaneously measuring isotope abundance and impurity content is characterized by comprising the following steps:
s1: the sample injector acts on the isotope sample to convert the isotope sample into a gas state or a fog state;
s2: the multi-charge-state electron cyclotron resonance ion source enables the isotope sample changed into a gas state or a fog state to generate multi-charge-state ions;
s3: the pre-accelerator accelerates multi-charge-state ions;
s4: the electrostatic analyzer carries out energy focusing on the accelerated multi-charge-state ions;
s5: the magnetic analyzer performs momentum analysis on the multi-charge-state ions subjected to energy focusing, and distinguishes ions with different mass-to-charge ratios according to the size of the mass-to-charge ratio;
s6: measuring the ion beam current by a multi-receiving Faraday cup;
s7: the energy absorption film distinguishes isobaric ions;
s8: the detector records each isotope, each element, each isobaric ion beam current or single particle counting rate.
4. The mass spectrometry method for simultaneously measuring the abundance and the impurity content of an isotope according to claim 3, wherein for steps S7 and S8, when two isobaric elements having the same energy and the same charge state pass through the energy absorption film, the energy lost in the energy absorption film is different; after passing through the energy absorption film, the residual energy of the energy absorption film is different, and the detector measures the energy of the energy absorption film and counts the energy of the energy absorption film, and identifies two isobaric elements with the same quantity and the proportion between the isobaric elements.
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