CN110854009A - Mass spectrum device of wide-range mass measurement ion source and mass spectrum method thereof - Google Patents
Mass spectrum device of wide-range mass measurement ion source and mass spectrum method thereof Download PDFInfo
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- CN110854009A CN110854009A CN201911107933.XA CN201911107933A CN110854009A CN 110854009 A CN110854009 A CN 110854009A CN 201911107933 A CN201911107933 A CN 201911107933A CN 110854009 A CN110854009 A CN 110854009A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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- 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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- H01J49/107—Arrangements for using several ion sources
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- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/161—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
- H01J49/162—Direct photo-ionisation, e.g. single photon or multi-photon ionisation
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Abstract
The invention relates to a mass spectrum device of a wide-range mass measurement ion source in the field of mass spectrum analysis, which comprises an ionization chamber, a single photon ionization source, a guide lens, a mass analyzer and an acquisition control system, wherein the single photon ionization source is connected with the guide lens; the ionization chamber is provided with a sample inlet, an electron slit window and a filament are arranged in the ionization chamber, and the filament is positioned below the electron slit window; the single photon ionization source, the ionization chamber, the guide lens and the mass analyzer are communicated in sequence, and the acquisition control system acquires an ionized sample ejected by the mass analyzer. The invention also provides a mass spectrometry method of the wide-range mass measurement ion source. The novel mass spectrum device provided by the invention combines an electron bombardment source and a single photon ionization source, combines the advantages of the two ionization sources, realizes advantage complementation, can freely switch modes and provides more detection options.
Description
Technical Field
The invention relates to the field of mass spectrometry, in particular to a mass spectrometry device of a wide-range mass measurement ion source and a mass spectrometry method thereof.
Background
Mass spectrometry is an analytical method by which the magnitude of the mass-to-charge ratio of ions in a sample is measured. The principle is that a sample is ionized, then is separated according to the mass-to-charge ratio (m/z) through a magnetic field or an electric field to obtain a mass spectrogram, and the qualitative and quantitative analysis of the sample can be obtained by analyzing the mass spectrogram of the sample.
The instrument used to perform mass spectrometry is called a mass spectrometer. Generally, a complete mass spectrometer consists of a sample introduction system, an ion source, a focusing transmission system, a mass analyzer, a vacuum system and a data acquisition system. The ion source is called the "brain" of the mass spectrometer because of its importance and specificity. The ion source has a variety of types, and mainly comprises an electron bombardment source, a chemical ionization source, a vacuum ultraviolet single photon ionization source, an atmospheric pressure chemical ionization source, a laser desorption ionization source and the like.
Electron bombardment sources were the ionization source technology used in the first mass spectrometry and were widely used for the detection of gaseous and volatile substances. It bombards the sample with electron beam of 70eV to make the sample become positively charged ion. The electron bombardment source has high ionization efficiency, is simple and reliable, and can identify unknown compounds according to comparison of a large number of databases. However, the electron bombardment source has not been widely used for the online detection of complex samples, and the main reasons are as follows:
(1) the electron bombardment source is a hard ionization mode, and a mass spectrogram after ionization has a large number of fragment ion peaks. For the injection of complex compounds, the overlapping of mass spectrum peaks can be generated, which not only makes the spectrogram difficult to analyze, but also causes inaccurate monitoring results.
(2) The working gas pressure of the electron bombardment source needs to be lower than 1 x 10-3Pa, above this value, oxidizing gases in the air can cause filament oxidation, leading to reduced ion source lifetime and reduced sensitivity.
A single photon ionization source is a form of soft ionization, and its principle is that after the energy of a photon is absorbed by an electron in a sample molecule, if the absorbed photon energy is greater than the ionization energy of the molecule, the electron escapes from the sample molecule, so that the sample molecule is ionized to obtain the molecular ion peak of the sample. Single photon ionization sources commonly employ vacuum ultraviolet lamps as the ionization source, which have a maximum energy of 10.6eV, which is higher than the ionization energy of most organic compounds, but less than their dissociation ionization energy. And the vacuum ultraviolet lamp can not ionize water, nitrogen and oxygen, so that the ionized spectrogram has few fragment ions, simple spectrogram and convenient spectrum resolution. Therefore, it is very advantageous to analyze complex mixture samples. However, single photon ionization sources also have significant disadvantages:
(1) the structural information of the sample is less;
(2) the ionization efficiency is low.
It has been found through prior art search that chinese patent publication No. CN106548920B discloses an elemental mass spectrometer that uses a mass filter to select ions from ions received from an ion source and to emit the selected ions. A reaction or collision cell receives the emitted ions and reacts or collides these ions with a gas to thereby provide product ions. A mass analyzer receives the product ions, analyzes them, and provides at least one output based on detection of the analyzed ions. The elemental mass spectrometer is operated to provide a first output from the mass analyser measuring ions within a first analysis range of mass to charge ratios including a desired mass to charge ratio M, to provide a second output from the mass analyser measuring ions within a second analysis range of mass to charge ratios including a mass to charge ratio (M-i) at least 0.95 atomic mass units lower than the desired mass to charge ratio, i ≧ 0.95, and to correct the first output based on the second output. This mass spectrometer also suffers from the problems described above.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a mass spectrum device of a wide-range mass measurement ion source and a mass spectrum method thereof, and a composite ion source device and a technology for wide-range detection of a mass spectrometer.
The invention provides a mass spectrum device of a wide-range mass measurement ion source, which is characterized by comprising an ionization chamber, a single photon ionization source, a guide lens, a mass analyzer and an acquisition control system, wherein the single photon ionization source is connected with the guide lens;
the ionization chamber is provided with a sample inlet, an electron slit window and a filament are arranged in the ionization chamber, and the filament is positioned below the electron slit window;
the single photon ionization source, the ionization chamber, the guide lens and the mass analyzer are communicated in sequence, and the acquisition control system acquires an ionized sample ejected by the mass analyzer.
In some embodiments, the acquisition control system controls the electron slit window and the filament to switch between a complex sampling mode and a wide-range measurement mode.
In some embodiments, the electron slit window loading voltage U is in the range of-300V ≦ U ≦ -15V.
In some embodiments, the ionization chamber further comprises a permanent magnet disposed on a side of the ionization chamber.
In some embodiments, the single photon ionization source is a vacuum ultraviolet lamp.
In some embodiments, the power source of the single photon ionization source is a dc power source or a radio frequency power source.
In some embodiments, the mass analyzer is an ion trap mass analyzer, a quadrupole mass analyzer, or a time-of-flight mass spectrometer.
In some embodiments, the acquisition control system comprises a signal conversion circuit, an acquisition circuit and a human interaction system.
The invention also provides a mass spectrum method of the wide-range mass measurement ion source, and the mass spectrum device adopting the wide-range mass measurement ion source comprises the following steps:
step S1, opening a sample inlet, and enabling a sample to enter an ionization chamber;
step S2, selecting a complex sample mode in the acquisition control system: opening the single photon ionization source, emitting photons, and carrying out soft ionization on the sample;
step S3, introducing the ionized sample ions into a mass analyzer through a guide lens, and sequentially ejecting the ionized sample ions to an acquisition control system according to the mass-to-charge ratio of the ionized sample ions to obtain the molecular ion peak of the sample ions;
step S4, selecting a wide-range measurement mode in the acquisition control system: the single photon ionization source is continuously opened, the electron slit window loads voltage, the lamp filament is lightened, the sample molecules are ionized simultaneously by hardness and softness, and water, oxygen and nitrogen in the air are ionized simultaneously;
and step S5, introducing all ionized ions into a mass analyzer through a guide lens, and sequentially ejecting the ionized ions to an acquisition control system according to the mass-to-charge ratio of the ionized ions to obtain a mass spectrogram with a wide mass number range.
In some embodiments, in step S4, the electron slit window loading voltage U is in the range of-300V ≦ U ≦ -15V.
Compared with the prior art, the invention has the following beneficial effects:
1. the novel mass spectrum device provided by the invention combines an electron bombardment source and a single photon ionization source, combines the advantages of the two ionization sources, realizes advantage complementation, can freely switch modes and provides more detection options.
2. The mass spectrometer device provided by the invention has the advantages of simple structure, high sensitivity and wide detection range, opens up the diversified selection of complex samples and lays a foundation for the sustainable development of mass spectrometry technology.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a timing diagram illustrating the control of the present invention;
FIG. 3 is a molecular ion peak mass spectrum of the sample ions of the present invention;
FIG. 4 is a mass spectrum of a wide range of mass numbers according to the invention;
FIG. 5 is a schematic view of the electron slit window loading voltage and ionization effect.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Referring to fig. 1, the present embodiment provides a mass spectrometer of wide range mass measurement ion source, including ionization chamber 1, the ionization source left side is single photon ionization source 2, ionization chamber 1 upside is sample inlet 5, be provided with electron slit window 4 in the ionization chamber, 4 downside of electron slit window is filament 3, ionization chamber 1 upper and lower part all is equipped with permanent magnet 6, ionization chamber 1 right side is guide lens 7, the guide lens right side is mass analyzer 8, mass analyzer 8 right side is acquisition control system 9.
The acquisition control system 9 controls the electron slit window 4 and the filament 3 to switch between the complex sample injection mode and the wide-range measurement mode, that is, the electron slit window is loaded with voltage to switch between the complex sample injection mode and the wide-range measurement mode. The voltage is applied to the electron slit window 4 only when the wide-range measurement mode is in use, and the filament 3 is simultaneously turned on, that is, the filament 3 is turned on only when the wide-range measurement mode is in use, so that the problems of filament oxidation caused by oxidizing gas in the air, which is mentioned in the background art, and the service life of the ion source is shortened and the sensitivity is reduced are avoided.
The range of the loading voltage U of the electronic slit window 4 is-300V and U is not more than-15V. Specifically, when the voltage is gradually increased from-15V to-100V, the ionization effect gradually increases, the maximum ionization effect can reach 85% when the voltage is-100V, and then the ionization effect gradually decreases when the voltage is increased from-100V to-300V.
The ionization chamber further comprises a permanent magnet 6, and the permanent magnet 6 is arranged on the side surface of the ionization chamber 1. Preferably, the permanent magnets 6 are symmetrically arranged on two side surfaces of the ionization chamber 1, and further, symmetrically arranged on the sample inlet 5 and the other side surface of the ionization chamber 1 opposite to the sample inlet 5, so that the ionization efficiency can be remarkably improved, and the sensitivity of the instrument can be improved.
The single photon ionization source 2 is a vacuum ultraviolet lamp. The power supply of the single photon ionization source is a single photon ionization source direct current power supply or a single photon ionization source radio frequency power supply.
The mass analyser 8 is an ion trap mass analyser, a quadrupole mass analyser or a time-of-flight mass spectrometer.
The acquisition control system 9 comprises a signal conversion circuit, an acquisition circuit and a manual interaction system.
The invention combines the advantages of an electron bombardment source and a single photon ionization source and can be switched between the electron bombardment source and the single photon ionization source. Not only can obtain the molecular ion peak of the sample ion, but also can obtain the fragment ion information of the sample ion. Different ionization modes can be selected according to requirements, the accuracy of analyzing a complex mixed sample is improved, the detection range is enlarged, the loss can be reduced, the ionization efficiency and the comprehensive utilization rate of the sample are improved, and the detection range and the sensitivity of an instrument are effectively improved. The ion source is not only suitable for testing high-end instruments in a laboratory, but also suitable for real-time online in-situ detection of portable instruments.
Example 2
As shown in fig. 1-5, the present embodiment provides a mass spectrometry method of a wide-range mass measurement ion source, comprising the steps of:
step S1, opening a sample inlet, and enabling a sample to enter the ionization chamber 1;
step S2, selecting a complex sample mode in the acquisition control system 9: the single photon ionization source 2 is opened, a vacuum ultraviolet lamp is selected as the single photon ionization source 2, photons are emitted, and the sample is subjected to soft ionization;
step S3, introducing the ionized sample ions into a mass analyzer 8 through a guide lens 7, and sequentially ejecting the ionized sample ions to an acquisition control system 9 according to the mass-to-charge ratio of the ionized sample ions to obtain molecular ion peaks of the sample ions;
step S4, selecting a wide-range measurement mode in the acquisition control system 9: the single photon ionization source is continuously opened, the electronic slit window 4 is loaded with voltage, the U range of the loaded voltage is-300V and is more than or equal to U and less than or equal to-15V, and the voltage is preferably loaded to-100V so as to obtain the optimal ionization effect, the filament 3 is lightened, the sample molecules are ionized simultaneously by hardness and softness, and water, oxygen and nitrogen in the air are also ionized;
in step S5, all the ionized ions are introduced into the mass analyzer 8 through the guide lens 7 and are ejected to the acquisition control system 9 in sequence according to the mass-to-charge ratio, so as to obtain a mass spectrum with a wide mass number range.
The first embodiment is as follows:
certain organic silicon oil and air are selected as samples, a vacuum ultraviolet lamp is selected as a single photon ionization source 2, and the ionization energy is 10.6 eV.
Firstly, opening a sample inlet, and introducing a mixed gas of certain organic silicon oil and air into an ionization chamber 1;
second, a complex sample pattern in the acquisition control system 9 is selected: the vacuum ultraviolet lamp is turned on to emit photons, and the silicon oil molecules are subjected to soft ionization, and the time sequence is shown in figure 2;
then, the ionized silicon oil sample ions are introduced into a mass analyzer 8 through a guide lens 7 and are sequentially ejected to an acquisition control system 9 according to the mass-to-charge ratio of the silicon oil sample ions, so that molecular ion peaks of the silicon oil sample ions are obtained, and the peak is shown in fig. 3;
again, a wide range measurement mode in the acquisition control system 9 is selected: the vacuum ultraviolet lamp is continuously opened, the electronic slit window 4 is loaded with voltage of-100V, the filament 3 is lightened, the sample molecules are ionized simultaneously, and water, oxygen and nitrogen in the air are also ionized, wherein a timing chart is shown in figure 2; the voltage is applied to the electron slit window 4 only when the wide-range measurement mode is in use, and the filament 3 is simultaneously turned on, that is, the filament 3 is turned on only when the wide-range measurement mode is in use, so that the problems of filament oxidation caused by oxidizing gas in the air, which is mentioned in the background art, and the service life of the ion source is shortened and the sensitivity is reduced are avoided.
Finally, all the ionized ions are introduced into a mass analyzer 8 through a guide lens 7 and are sequentially ejected to an acquisition control system according to the mass-to-charge ratio of the ions, so that a mass spectrogram with a wide mass number range is obtained, and the mass spectrogram is shown in fig. 4.
The components, the structural arrangement of the components, and the corresponding functional advantages of the mass spectrometer apparatus for a wide-range mass measurement ion source used in this embodiment 2 are described in detail in embodiment 1, and will not be described herein again.
In conclusion, the novel mass spectrum device provided by the invention combines the advantages of an electron bombardment source and a single photon ionization source, realizes advantage complementation, can freely switch modes and provides more detection options; the mass spectrometer device provided by the invention has the advantages of simple structure, high sensitivity and wide detection range, opens up the diversified selection of complex samples and lays a foundation for the sustainable development of mass spectrometry technology.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (10)
1. A mass spectrum device of a wide-range mass measurement ion source is characterized by comprising an ionization chamber (1), a single photon ionization source (2), a guide lens (7), a mass analyzer (8) and an acquisition control system (9);
the ionization chamber (1) is provided with a sample inlet (5), an electron slit window (4) and a filament (3) are arranged in the ionization chamber (1), and the filament (3) is positioned below the electron slit window (4);
the single photon ionization source (2), the ionization chamber (1), the guide lens (7) and the mass analyzer (8) are communicated in sequence, and the collection control system (9) collects ionized samples ejected by the mass analyzer (8).
2. The mass spectrometry apparatus of a wide-range mass measurement ion source according to claim 1, wherein the acquisition control system (9) implements switching between a complex sample injection mode and a wide-range measurement mode by controlling the electron slit window (4) and the filament (3).
3. The mass spectrometry apparatus of a wide range mass measurement ion source according to claim 2, wherein the electron slit window (4) is loaded with a voltage U in the range-300V ≦ U ≦ -15V.
4. The mass spectrometry apparatus of a wide range mass measurement ion source according to claim 1, further comprising a permanent magnet (6), the permanent magnet (6) being disposed at a side of the ionization chamber (1).
5. The mass spectrometry apparatus of a wide range mass measurement ion source according to claim 1, wherein the single photon ionization source (2) is a vacuum ultraviolet lamp.
6. The mass spectrometry apparatus of a wide range mass measurement ion source according to claim 5, wherein the power supply of the single photon ionization source (2) is a dc power supply or a radio frequency power supply.
7. The mass spectrometry apparatus of a wide range mass measurement ion source according to claim 1, wherein the mass analyser (8) is an ion trap mass analyser, a quadrupole mass analyser or a time-of-flight mass spectrometer.
8. The mass spectrometry apparatus of a wide range mass measurement ion source of claim 1, wherein the acquisition control system comprises signal conversion circuitry, acquisition circuitry and a human interaction system.
9. A method of mass spectrometry for a wide range mass measurement ion source employing a mass spectrometry apparatus for a wide range mass measurement ion source according to any one of claims 1 to 8, comprising the steps of:
step S1, opening a sample inlet, and enabling a sample to enter an ionization chamber (1);
step S2, selecting a complex sample pattern in the acquisition control system (9): the single photon ionization source (2) is turned on to emit photons to carry out soft ionization on the sample;
step S3, introducing the ionized sample ions into a mass analyzer (8) through a guide lens (7), and sequentially ejecting the ionized sample ions to an acquisition control system (9) according to the mass-to-charge ratio of the ionized sample ions to obtain molecular ion peaks of the sample ions;
step S4, selecting a wide-range measurement mode in the acquisition control system (9): the single photon ionization source (2) is continuously opened, the electron slit window (4) loads voltage, the filament (3) is lightened, the sample molecules are ionized in a soft and hard mode, and water, oxygen and nitrogen in the air are ionized simultaneously;
and step S5, introducing all ionized ions into the mass analyzer (8) through the guide lens (7), and ejecting the ionized ions to the acquisition control system (9) in sequence according to the mass-to-charge ratio of the ionized ions to obtain a mass spectrum with mass number in a wide range.
10. The method of mass spectrometry of a wide range mass measurement ion source of claim 9, wherein in step S4, the electron slit window (4) is loaded with a voltage U in the range of-300V ≦ U ≦ -15V.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114166927A (en) * | 2021-12-23 | 2022-03-11 | 上海裕达实业有限公司 | Mass spectrum device detection method for detecting multi-component sample |
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Application publication date: 20200228 |