CN114235937B - Method for simultaneously detecting positive ions and negative ions in ion trap of mass spectrometer - Google Patents
Method for simultaneously detecting positive ions and negative ions in ion trap of mass spectrometer Download PDFInfo
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- CN114235937B CN114235937B CN202111444605.6A CN202111444605A CN114235937B CN 114235937 B CN114235937 B CN 114235937B CN 202111444605 A CN202111444605 A CN 202111444605A CN 114235937 B CN114235937 B CN 114235937B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Abstract
A method for simultaneously detecting positive ions and negative ions in a mass spectrometer ion trap, wherein the power-up sequence of the ion trap comprises an ion cooling stage, an ion scanning stage and an idle stage. In the ion cooling stage, the upper polar plate and the lower polar plate of the ion trap have the applied amplitude of V RF With frequency f RF Is applied with amplitude of sine alternating current before and after ion trapThe frequency isAnd respectively with direct current voltage-V DC And +V DC And coupling is carried out to ensure that positive ions and negative ions are stably bound at the center of the XY section of the ion trap and are mutually separated in the Z-axis direction. In the ion scanning stage, the amplitude V is applied to the upper polar plate and the lower polar plate of the ion trap RF With frequency f RF Sinusoidal alternating current with linearly increased amplitude is respectively applied on the left polar plate and the right polar plate of the ion trapThe frequency isBut sine alternating current with opposite phase causes positive and negative ion resonance in the ion trap to be excited out. The invention can realize the simultaneous detection of positive ions and negative ions by using only a single ion trap as a mass analyzer, and greatly improves the sample detection efficiency.
Description
Technical Field
The invention relates to a mass spectrometer detection technology, in particular to a method for simultaneously detecting positive ions and negative ions in an ion trap of a mass spectrometer.
Background
Mass spectrometry is a method for performing qualitative or quantitative analysis of chemical compounds by ionizing a substance and then separating the substance according to the mass-to-charge ratio of the ion, and then obtaining a mass spectrum by measuring the peak intensities of the ions with various mass-to-charge ratios. In many fields of application, mass spectrometers are required to obtain mass spectral information of complex samples in a relatively short time, whereas samples of different properties generate positive or negative ions under different ionization methods.
Most of the existing mass spectrometers only have a positive ion detection mode or a negative ion detection mode, a small number of mass spectrometers can switch between the positive ion detection mode and the negative ion detection mode, and two sets of mass analyzers are simultaneously arranged in a small number of mass spectrometers to realize the separate detection of positive ions and negative ions. The mass spectrometer with the positive ion detection mode or the negative ion detection mode can not realize the ion detection capability of positive and negative polarities, and can possibly cause the loss of key information of mass spectrum; a mass spectrometer with a positive ion detection mode and a negative ion detection mode switching function needs to realize detection of positive and negative ions by switching the two modes, but the longer switching time can reduce the detection efficiency; mass spectrometers with two sets of mass analyzers can detect ions of both positive and negative polarities, respectively, but can cause problems with functional redundancy and large volumes of the mass spectrometers.
It should be noted that the information disclosed in the above background section is only for understanding the background of the present application and thus may include information that does not form the prior art that is already known to those of ordinary skill in the art.
Disclosure of Invention
The main object of the present invention is to overcome the above-mentioned drawbacks of the background art and to provide a method for simultaneously detecting positive and negative ions in an ion trap of a mass spectrometer.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method of simultaneously detecting positive and negative ions in a mass spectrometer ion trap, the power-up sequence of the ion trap comprising an ion cooling phase, an ion scanning phase and an idle phase;
in the ion cooling stage: applying an amplitude of V to the ion trap upper plate and the ion trap lower plate RF With frequency f RF Sinusoidal alternating current V of (2) RF ×sin(2π·f RF T) so that positive ions and negative ions are stably bound near the center of the XY cross section of the ion trap; the ion gate is applied with amplitude value before the ion trap and after the ion trapFrequency of->Sinusoidal alternating current of (2)And respectively with direct current voltage-V DC And +V DC Coupling is performed, namely the ion gate before the ion trap and the ion gate after the ion trap are respectively applied with +.>And->So that the positive ions and the negative ions are stably restrained at the central position of the Z axis of the ion trap and kept in a mutually separated state in the Z axis;
in the ion scanning stage: applying a frequency f to the ion trap upper plate and the ion trap lower plate RF And amplitude V RF Sinusoidal alternating current V with linear increase RF ×sin(2π·f RF T), where f RF And ion cooling stage f RF Keeping consistency; the applied amplitude values applied on the left polar plate of the ion trap and the right polar plate of the ion trap are respectivelyFrequency of->But with opposite phaseIs +.>And->So as to excite positive ions and negative ions in the ion trap to resonate.
During the idle phase: the voltage applied to the ion trap is unloaded to purge ions in the ion trap.
Further:
during the ion cooling phase, amplitude V RF Less than 600V, and frequency f RF Less than 2MHz;
during the ion cooling phase, the amplitudeLess than 600V, and frequency->Less than 10000Hz, DC voltage amplitude V DC Less than 100V.
In the ion scanning stage, V RF Less than 6000V.
During the ion scan phase, the amplitudeLess than 100V and a frequency->Less than 1MHz.
During the ion scanning phase, no voltage is applied across the ion trap front ion gate and the ion trap rear ion gate.
The negative ion detector and the positive ion detector are respectively positioned at the left side of the left polar plate of the ion trap and the right side of the right polar plate of the ion trap in the X-axis direction, and the negative ion detector and the positive ion detector are respectively positioned at positions close to the front ion gate of the ion trap and the rear ion gate of the ion trap in the Z-axis direction.
The ion trap is a rectangular ion trap or a linear ion trap.
A computer readable storage medium storing a computer program which, when executed by a processor, performs the method.
The invention can realize that the mass spectrometer only uses a single ion trap as a mass analyzer to realize the simultaneous detection of positive ions and negative ions, thereby greatly improving the sample detection efficiency.
Drawings
Fig. 1 is a schematic diagram of a rectangular ion trap according to an embodiment of the present invention;
FIG. 2 is a timing diagram of voltage applied to a rectangular ion trap plate according to one embodiment of the present invention;
FIG. 3 is a schematic diagram showing the effect of separating positive and negative ions from each other when low and high DC voltages are not applied to the rectangular ion trap z-axis plate, respectively, in accordance with an embodiment of the present invention;
FIG. 4 is a schematic diagram of the positional relationship between a rectangular ion trap and a mass analyzer according to an embodiment of the present invention;
fig. 5 is a schematic diagram of a rectangular ion trap for simultaneously detecting positive ions and negative ions according to an embodiment of the present invention.
Detailed Description
The following describes embodiments of the present invention in detail. It should be emphasized that the following description is merely exemplary in nature and is in no way intended to limit the scope of the invention or its applications.
It will be understood that when an element is referred to as being "mounted" or "disposed" on another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element. In addition, the connection may be for both a fixing action and a coupling or communication action.
It is to be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are merely for convenience in describing embodiments of the invention and to simplify the description by referring to the figures, rather than to indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be construed as limiting the 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 such feature. In the description of the embodiments of the present invention, the meaning of "plurality" is two or more, unless explicitly defined otherwise.
Referring to fig. 1 to 5, an embodiment of the present invention provides a method for simultaneously detecting positive ions and negative ions in a mass spectrometer ion trap, wherein a single ion trap is used as a mass analyzer for simultaneously detecting positive ions and negative ions, and the ion trap is a rectangular ion trap or a linear ion trap. The power-up sequence of the ion trap comprises an ion cooling stage, an ion scanning stage and an idle stage. In the ion cooling stage, the upper polar plate and the lower polar plate of the ion trap have the applied amplitude of V RF With frequency f RF Is applied with amplitude of sine alternating current before and after ion trapFrequency of->And respectively with direct current voltage-V DC And +V DC And coupling is carried out to ensure that positive ions and negative ions are stably bound at the center of the XY section of the ion trap and are mutually separated in the Z-axis direction. In the ion scanning stage, the amplitude V is applied to the upper polar plate and the lower polar plate of the ion trap RF With frequency f RF Sinusoidal alternating current with linear increase is respectively applied on the left polar plate and the right polar plate of the ion trap, and the amplitude is +.>Frequency of->But sine alternating current with opposite phase causes positive and negative ion resonance in the ion trap to be excited out. After the positive and negative ion detectors detect the signals of the positive and negative ions respectively, the positive and negative ion mass spectrograms can be obtained simultaneously. During the idle phase, all voltages applied across the ion trap are unloaded to purge ions in the ion trap.
Referring to fig. 1, two plates with slits in the X-axis direction of the ion trap are an ion trap left plate 1 and an ion trap right plate 2, two plates in the Y-axis direction of the ion trap are an ion trap upper plate 3 and an ion trap lower plate 4, and two plates in the Z-axis direction of the ion trap are an ion trap front ion gate 5 and an ion trap rear ion gate 6 respectively.
The voltages applied to the ion trap upper plate 3 and the ion trap lower plate 4 are: v (V) RF ×sin(2π·f RF T); the voltages applied to the left polar plate 1 of the ion trap and the right polar plate 2 of the ion trap are respectivelyAndthe voltages applied to the ion gate 5 before the ion trap and the ion gate 6 after the ion trap are respectivelyAnd->
Referring to fig. 2, the power-up sequence of the ion trap includes an ion cooling stage S1, an ion scanning stage S2, and an idle stage S3. In the ion cooling stage S1, positive ions and negative ions enter an ion trap from a round hole on an ion trap front ion gate 5 or an ion trap rear ion gate 6 to be subjected to ion cooling; in the ion scanning stage S2, positive ions and negative ions are scanned out of the ion trap; in idle phase S3, all voltages applied to the ion trap are unloaded in order to leave a certain time for the ion trap to be purged of ions.
In the ion cooling stage S1, when the positive ions and the negative ions enter the ion trap and begin to be cooled, in order to bind the positive ions and the negative ions in the ion trap, an amplitude V is applied to the upper polar plate 3 of the ion trap and the lower polar plate 4 of the ion trap RF With frequency f RF Sinusoidal alternating current V of (2) RF ×sin(2π·f RF T) to stably confine the positive and negative ions near the center of the XY cross-section of the ion trap. Wherein the amplitude V RF Less than 600V, and f RF As the resonance frequency of the ion trap is less than 2MHz under the vacuum environment, the better ion cooling effect is ensured.
In the ion cooling stage S1, voltages applied to the ion gate 5 before ion trap and the ion gate 6 after ion trap are respectivelyAnd->Wherein the applied amplitude is +.>Frequency of->Is +.>The purpose of (1) is to stabilize positive and negative ions at the center dimension position of the Z axis of the ion trap, and apply-V DC And +V DC The purpose of the dc voltage is to keep the positive and negative ions separated from each other in the Z-axis during the ion cooling phase to reduce interactions between the positive and negative ions. Wherein the amplitude->Less than 600V, and frequency->Less than 10000Hz, DC voltage amplitude V DC Less than 100V.
The ion cooling stage applies sine alternating current to ensure that positive ions and negative ions can be stably bound at the central position of the Z axis of the ion trap, the positive direct voltage and the negative direct voltage are coupled on the basis of alternating voltage, so that the positive ions and the negative ions can keep a mutually separated state in the Z axis to reduce the mutual reaction between the positive ions and the negative ions, wherein the stable position of the positive ions in the Z axis is biased to apply negative direct voltage-V DC The stable position of the negative ions in the Z-axis direction is biased to apply positive direct current voltage +V DC Is provided. And V is DC The larger the value of (2), the more obvious the phenomenon of separation between positive and negative ions.
Referring to fig. 3, the darker charged ions are negative ions and the lighter charged ions are positive ions. In the ion cooling stage S1, voltages applied to the ion gate 5 before ion trap and the ion gate 6 after ion trap are respectivelyAnd->At applied V DC The distribution of positive and negative ions at 0 is shown as a in FIG. 3, when smaller and larger V are applied DC The distribution of positive and negative ions is shown in b and c in FIG. 3, respectively, wherein the stable position of the positive ion group in the Z-axis direction is biased to apply negative DC voltage-V DC The ion trap front ion gate 5 of (2) is provided with positive direct current voltage +V at the stable position bias of the negative ion group in the Z-axis direction DC Ion trap front ion gate 6 of (a).
Referring to fig. 4, the relative positions of the left plate 1 and the right plate 2 of the ion trap and the positive ion detector 9 and the negative ion detector 8 can be known in the present invention. The negative ion detector 8 and the positive ion detector 9 are respectively on the left side of the ion trap left plate 1 and the right side of the ion trap right plate 2 in the X-axis direction, and are respectively located near the ion trap front ion gate and the ion trap rear ion gate in the Z-axis direction.
Referring to fig. 5, during the ion scanning stage S2, no voltage is applied across the ion trap front ion gate 5 and the ion trap rear ion gate 6 to keep the positive and negative ions stable at the Z-axis position of the ion trap; applying a frequency f to the ion trap upper plate 3 and the ion trap lower plate 4 RF And amplitude V RF Sinusoidal alternating current V with linear increase RF ×sin(2π·f RF T), where f RF And ion cooling stage f RF Keep consistent, and V RF Less than 6000V; the left polar plate 1 of the ion trap and the right polar plate 2 of the ion trap are respectively applied with amplitude valuesFrequency of->Sinusoidal alternating current with opposite phase>Andthe method is used for resonating and exciting positive and negative ions in the ion trap from small to large according to the absolute value of the mass-to-charge ratio. Amplitude->Less than 100V, and frequency->Less than 1MHz.
The negative ion detector 9 and the positive ion detector 8 are respectively positioned on the left side of the left polar plate of the ion trap and the right side of the right polar plate of the ion trap in the X-axis direction, and the negative ion detector and the positive ion detector are respectively positioned near the front ion gate of the ion trap and the rear ion gate of the ion trap in the Z-axis direction.
The signals detected by the positive ion detector 9 and the negative ion detector 8 are respectively converted into a positive ion mass spectrogram and a negative ion mass spectrogram through subsequent processing, and the positive ion mass spectrogram and the negative ion mass spectrogram of the sample to be detected in one detection period can be obtained after the two mass spectrograms are combined.
In idle phase S3, all voltages applied to the ion trap are unloaded, leaving a certain time for ion removal from the ion trap.
The invention can realize that the mass spectrometer only uses a single ion trap as a mass analyzer to realize the simultaneous detection of positive ions and negative ions, and greatly improves the sample detection efficiency.
The background section of the present invention may contain background information about the problems or environments of the present invention and is not necessarily descriptive of the prior art. Accordingly, inclusion in the background section is not an admission of prior art by the applicant.
The foregoing is a further detailed description of the invention in connection with specific/preferred embodiments, and it is not intended that the invention be limited to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the invention, and these alternatives or modifications should be considered to be within the scope of the invention. In the description of the present specification, reference to the terms "one embodiment," "some embodiments," "preferred embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Those skilled in the art may combine and combine the features of the different embodiments or examples described in this specification and of the different embodiments or examples without contradiction. Although embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. A method for simultaneously detecting positive ions and negative ions in an ion trap of a mass spectrometer, wherein a power-up sequence of the ion trap comprises an ion cooling stage, an ion scanning stage and an idle stage;
in the ion cooling stage: applying an amplitude of V to the ion trap upper plate and the ion trap lower plate RF With frequency f RF Sinusoidal alternating current V of (2) RF ×sin(2π·f RF T) so that positive ions and negative ions are stably bound near the center of the XY cross section of the ion trap; the ion gate is applied with amplitude value before the ion trap and after the ion trapFrequency of->Sinusoidal alternating current of (2)And respectively with direct current voltage-V DC And +V DC Coupling is performed, namely the ion gate before the ion trap and the ion gate after the ion trap are respectively applied with +.>And->So that the positive ions and the negative ions are stably restrained at the central position of the Z axis of the ion trap and kept in a mutually separated state in the Z axis;
in the ion scanning stage: applying a frequency f to the ion trap upper plate and the ion trap lower plate RF And amplitude V RF Sinusoidal alternating current V with linear increase RF ×sin(2π·f RF T), where f RF And ion cooling stage f RF Keeping consistency; the applied amplitude values applied on the left polar plate of the ion trap and the right polar plate of the ion trap are respectivelyFrequency of->Sinusoidal alternating current with opposite phaseAnd->So as to excite positive ions and negative ions in the ion trap to form the ion trap in resonance;
during the idle phase: the voltage applied to the ion trap is unloaded to purge ions in the ion trap.
2. The method of claim 1, wherein during the ion cooling phase, the amplitude V RF Less than 600V, and frequency f RF Less than 2MHz.
3. A method as claimed in claim 1 or 2, wherein during the ion cooling phase, the amplitude is adjustedLess than 600V, and frequency->Less than 10000Hz, DC voltage amplitude V DC Less than 100V.
4. A method according to any one of claims 1 to 3, wherein, during the ion scanning phase, V RF Less than 6000V.
5. The method of any one of claims 1 to 4, wherein during the ion scanning phase, an amplitude valueLess than 100V and a frequency->Less than 1MHz.
6. The method of any one of claims 1 to 5, wherein no voltage is applied across the ion trap front ion gate and the ion trap rear ion gate during the ion scanning phase.
7. The method of any one of claims 1 to 6, wherein the negative ion detector and the positive ion detector are located to the left of the left plate of the ion trap and to the right of the right plate of the ion trap, respectively, in the X-axis direction, and the negative ion detector and the positive ion detector are located near the ion trap front ion gate and the ion trap rear ion gate, respectively, in the Z-axis direction.
8. The method of any one of claims 1 to 7, wherein the ion trap is a rectangular ion trap or a linear ion trap.
9. A computer readable storage medium storing a computer program, which when run by a processor performs the method of any one of claims 1 to 8.
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