CN111223753B - Control method of ion mobility spectrometry-time-of-flight mass spectrometer - Google Patents
Control method of ion mobility spectrometry-time-of-flight mass spectrometer Download PDFInfo
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- CN111223753B CN111223753B CN201811431541.4A CN201811431541A CN111223753B CN 111223753 B CN111223753 B CN 111223753B CN 201811431541 A CN201811431541 A CN 201811431541A CN 111223753 B CN111223753 B CN 111223753B
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Abstract
The invention relates to a combined instrument, in particular to an ion mobility spectrometry-time-of-flight mass spectrometry combined instrument and a control method thereof. In the invention, the high-efficiency ionization of the molecules of a sample to be detected is realized based on an ionization source, characteristic ions enter an ion mobility spectrum through ion through holes, are sequentially separated according to different mobility rates, sequentially enter a time-of-flight mass spectrometer and are detected, and finally, signals are acquired and analyzed in a data acquisition system. The on-line ion mobility spectrometry-mass spectrometry two-dimensional combination instrument developed by the structure can realize the rapid and on-line two-dimensional analysis of a complex mixture sample, is particularly suitable for qualitative and quantitative analysis of an isomer mixture, and has wide application space.
Description
Technical Field
The invention relates to a combined two-dimensional analyzer, in particular to an ion mobility spectrometry-time-of-flight mass spectrometry combined instrument and a control method thereof.
Background
At present, for the detection and analysis of isomer products, the common methods are qualitative and quantitative analysis by gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS). However, these chromatographic-based methods typically require tens of minutes for analysis, are time consuming, and are difficult to use for rapidly changing process analyses. In addition, although the Infrared (IR), Raman (Raman), ultraviolet-visible (UV-Vis) and other spectroscopic techniques can measure various hydrocarbons and obtain functional group information of organic substances, spectral peaks are easily overlapped when complex mixtures are analyzed, and the quantitative analysis capability is insufficient; the Nuclear Magnetic Resonance (NMR) can detect gaseous and adsorbed molecules in a reaction system and carry out accurate quantitative analysis, but the spectrogram of a complex mixture system is not easy to analyze, and the practical application is limited to a certain extent.
Time-of-flight mass spectrometry (TOFMS) is a technology for separating and analyzing according to the mass-to-charge ratio of an object to be detected, has high analysis speed, high resolution and sensitivity and strong qualitative analysis capability on complex mixtures, has unique advantages in rapid and online detection and process analysis, and particularly has been widely applied to online detection by the online mass spectrometry technology which is rapidly developed in recent years and takes a soft ionization source as a core. However, because the TOFMS realizes the separation of a sample to be detected based on the mass number of a substance, for the detection of isomers, the isomers in a soft ionization mass spectrogram often only show a single mass spectrum peak with the same mass-to-charge ratio, and the loss of a characteristic fragment ion peak makes it impossible to obtain information related to a molecular structure, so that it is difficult to realize qualitative analysis.
Aiming at the analysis of an isomer mixture, the analysis capability of online mass spectrometry can be effectively improved by combining soft ionization mass spectrometry with a proper pre-separation method, an online two-dimensional mass spectrometry technology is formed by combining an ultrafast gas phase separation technology and a mass spectrometry, and the method is an important development direction in the future of online mass spectrometry. Ion Mobility Spectrometry (IMS) is a fast gas phase separation technique with response speeds on the order of milliseconds, while the principle of IMS separation is based on the fact that different ions have different mobilities. Because the mobility of the ions depends not only on the mass of the ions, but also on information such as the structures of the ions, the IMS can quickly separate isomers, and the isomers can be effectively made up for mass spectrum preceding stage separation by using the IMS, so that a powerful analysis means is formed.
Disclosure of Invention
The invention aims to develop an online ion mobility spectrometry-time-of-flight mass spectrometry two-dimensional combined key technology based on an ion mobility spectrometry and time-of-flight mass spectrometry analysis method, and establish an online two-dimensional mass spectrometry research platform for qualitative and quantitative analysis methods of isomer mixtures.
In order to achieve the above purpose, the invention adopts the technical scheme that:
the ion mobility spectrometry-time-of-flight mass spectrometer and the control method thereof comprise an ionization source, an ion mobility spectrometry, a time-of-flight mass spectrometry and a control system, and are characterized in that:
the ionization source is arranged at the front end of the ion mobility spectrometry and is hermetically connected with the ion mobility spectrometry, and an ion through hole is formed in an interface electrode;
the ion mobility spectrometry is arranged at the front end of the time-of-flight mass spectrometry and is hermetically connected with the time-of-flight mass spectrometry, a Skimmer electrode with an ion through hole is arranged at the center of the interface and is used as an ion outlet of the ion mobility spectrometry, and a slit is arranged at the center of the interface and is used as an ion inlet of the time-of-flight mass spectrometry;
respectively applying an ion mobility spectrometry ion gate trigger pulse, a time-of-flight mass spectrometry repulsion pulse and an acquisition card trigger pulse to the ion mobility spectrometry ion gate system, the time-of-flight mass spectrometry repulsion electrode and the data acquisition system;
the control system is the core of the control method and is used for setting pulse frequency and time sequence relations among ion mobility spectrum ion gate trigger pulses, time-of-flight mass spectrum repulsion pulses and acquisition card trigger pulses, so that accurate synchronization of ion mobility spectrum-time-of-flight mass spectrum data acquisition is realized, and a two-dimensional combined working spectrogram is obtained;
the control system is a time delay pulse generator system and outputs 1-4 paths of pulse signals, and the pulse width range is 0.1 mus-20 ms;
the Skimmer electrode can be used as an ion channel, or can be used as an ion channel and an ion mobility spectrometry ion receiving polar plate at the same time;
the ion mobility spectrometry ion gate system is an ion mobility spectrometry working mode control core, can be designed into a BN type ion gate or a TP type ion gate, and can control the ion mobility spectrometry to work in a forward mode or a reverse mode;
the ionization source is a photo-ionization source,63A Ni radioactive or discharge ionization source;
the inner diameter size range of the central through hole of each interface of the ion through hole, the Skimmer electrode and the slit is set to be 0.5-3 mm;
the time-of-flight mass spectrum is set to be linear, single reflection type or multiple reflection type;
the data acquisition system (23) is set as a TDC acquisition card or an ADC acquisition card;
in the ion mobility spectrometry-time-of-flight mass spectrometry combination instrument and the control method thereof, an ionization source realizes efficient ionization of molecules of a sample to be detected, characteristic ions enter an ion mobility spectrometry, are sequentially separated according to different mobility rates, and sequentially enter a time-of-flight mass spectrometry mass analyzer to be detected. The on-line ion mobility spectrometry-mass spectrometry two-dimensional combination instrument developed by the structure can realize the rapid on-line two-dimensional analysis of a complex mixture sample.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a working pulse control diagram of the ion mobility spectrometry-time-of-flight mass spectrometry in example 1, and the required pulse output is controlled by a delay pulse generator to realize accurate synchronization.
FIG. 3 is a two-dimensional signal spectrum of example 1, obtained by combining ion mobility spectrometry with time-of-flight mass spectrometry by testing 1ppm benzene, toluene and xylene.
Detailed Description
Fig. 1 is a schematic structural diagram of the present invention.
The invention relates to an ion mobility spectrometry-time-of-flight mass spectrometry combined instrument and a control method thereof, which consists of an ionization source 1, an ion mobility spectrometry 2, a time-of-flight mass spectrometry 4 and a control system 9, and is characterized in that:
the ionization source 1 is arranged at the front end of the ion mobility spectrometry 2 and is hermetically connected with the ion mobility spectrometry 2, and an ion through hole 10 is arranged on an interface electrode;
the ion mobility spectrometry 2 is arranged at the front end of the time-of-flight mass spectrometry 4 and is hermetically connected with the time-of-flight mass spectrometry 4, a Skimmer electrode 11 with an ion through hole is arranged at the center of the interface and is used as an ion outlet of the ion mobility spectrometry 2, and a slit 12 is arranged at the center of the interface and is used as an ion inlet of the time-of-flight mass spectrometry 4;
respectively applying an ion mobility spectrometry ion gate trigger pulse 6, a time-of-flight mass spectrometry repulsion pulse 7 and an acquisition card trigger pulse 8 to the ion mobility spectrometry ion gate system 3, the time-of-flight mass spectrometry repulsion electrode 13 and the data acquisition system 23;
the control system 9 is the core of the control method and is used for setting the pulse frequency and time sequence relation among the ion mobility spectrum ion gate trigger pulse 6, the flight time mass spectrum repulsion pulse 7 and the acquisition card trigger pulse 8, so that the data acquisition of the ion mobility spectrum-flight time mass spectrum realizes accurate synchronization, and a two-dimensional combined working spectrogram is obtained;
the control system 9 is a delay pulse generator system and outputs 1-4 paths of pulse signals, and the pulse width range is 0.1 mus-20 ms;
the Skimmer electrode 11 can be used as an ion channel, or can be used as an ion channel and an ion receiving polar plate of an ion mobility spectrometry 2 at the same time;
the ion mobility spectrometry ion gate system 3 is a control core of the working mode of the ion mobility spectrometry 2, can be designed into a BN type ion gate or a TP type ion gate, and can control the ion mobility spectrometry 2 to work in a forward mode or a reverse mode;
the ionization source 1 is set as a photo-ionization source,63A Ni radioactive or discharge ionization source;
the inner diameter size range of each interface center through hole of the ion through hole 10, the Skimmer electrode 11 and the slit 12 is set to be 0.5-3 mm;
the time-of-flight mass spectrum 4 is set to be linear, single reflection type or multiple reflection type;
the data acquisition system 23 is set as a TDC acquisition card or an ADC acquisition card;
in the ion mobility spectrometry-time-of-flight mass spectrometry combination instrument and the control method thereof, an ionization source realizes efficient ionization of molecules of a sample to be detected, characteristic ions enter an ion mobility spectrometry, are sequentially separated according to different mobility rates, and sequentially enter a time-of-flight mass spectrometry mass analyzer to be detected. The on-line ion mobility spectrometry-mass spectrometry two-dimensional combination instrument developed by the structure can realize the rapid on-line two-dimensional analysis of a complex mixture sample.
Example 1
The method comprises the steps of taking 1ppm of benzene, toluene and xylene mixed standard gas as a test sample, debugging a two-dimensional signal of ion mobility spectrometry-time-of-flight mass spectrometry, wherein the ion mobility spectrometry spectrogram signal is obtained by scanning the total ion current intensity of the time-of-flight mass spectrometry, and the pulse width of an ion gate of the ion mobility spectrometry is set to be 100 mu s. In order to make the display effect more intuitive, a Matlab program is written to perform noise reduction and other processing on the combined signal, and the two-dimensional spectrogram display as shown in the figure is realized.
Claims (7)
1. A control method of an ion mobility spectrometry-time-of-flight mass spectrometer comprises an ionization source (1), an ion mobility spectrometry (2), a time-of-flight mass spectrometry (4) and a control system (9), and is characterized in that:
the ionization source (1) is arranged at the front end of the ion mobility spectrometry (2) and is hermetically connected with the ion mobility spectrometry (2), and an ion through hole (10) is arranged at an interface electrode; the ion mobility spectrometry (2) is arranged at the front end of the flight time mass spectrometry (4) and is hermetically connected with the flight time mass spectrometry (4), a Skimmer electrode (11) with an ion through hole is arranged at the center of the interface and is used as an ion outlet of the ion mobility spectrometry (2), and a slit (12) is arranged at the center of the interface and is used as an ion inlet of the flight time mass spectrometry (4);
the ion mobility spectrometry ion gate system (3) is arranged at a position which is 10-30 mm away from one side of the ion mobility spectrometry (2) and close to the ion through hole (10), the ion mobility spectrometry ion gate system (3) is composed of two or three grid mesh ion gates which are parallel to each other and arranged at an interval of 0.5-5 mm, and the grid mesh ion gates are arranged perpendicular to the ion incidence direction;
the control system (9) is the core of the control method, and an ion mobility spectrometry ion gate trigger pulse (6) is applied to the ion mobility spectrometry ion gate system (3); simultaneously applying a time-of-flight mass spectrum repulsion pulse (7) to the time-of-flight mass spectrum repulsion electrode (13); simultaneously, applying a capture card trigger pulse (8) to a data acquisition system (23); the ion mobility spectrometry-time-of-flight mass spectrometry data acquisition is accurately synchronized by simultaneously setting an ion gate trigger pulse (6), a time-of-flight mass spectrometry repulsion pulse (7) and an acquisition card trigger pulse (8) and setting the pulse frequency and time sequence relation among the three, so that the control work of an ion mobility spectrometry-time-of-flight mass spectrometry combined mode (IMS-TOFMS) is realized;
the control method is set as follows: the trigger pulse (8) of the acquisition card is set to be a working period T0; setting continuous triggering of the normal working state of the flight time mass spectrum (4) in an ion mobility spectrum working period T1 in the flight time mass spectrum repulsion pulse (7);
after an ion mobility spectrum ion gate trigger pulse (6) is set to be opened, in a T0 cycle time, all ions sequentially pass through an ion mobility spectrum (2) to reach a time-of-flight mass spectrum repulsion electrode (13) according to the size of the ion mobility, ions arriving at different moments are separated under the action of a time-of-flight mass spectrum repulsion pulse (7), and a data acquisition system (23) is used for detecting the ions;
the control system (9) is a time delay pulse generator system and outputs 1-4 paths of pulse signals, and the range of pulse width is 0.1 mus-20 ms.
2. The method for controlling the ion mobility spectrometry-time of flight mass spectrometer according to claim 1, wherein:
the Skimmer electrode (11) is used as an ion channel, or is used as an ion channel and an ion receiving polar plate of the ion mobility spectrometry (2) at the same time.
3. The method for controlling the ion mobility spectrometry-time of flight mass spectrometer according to claim 1, wherein:
the ion mobility spectrometry ion gate system (3) is a control core of the working mode of the ion mobility spectrometry (2), can be designed into a BN type ion gate or a TP type ion gate, and can control the ion mobility spectrometry (2) to work in a forward mode or a reverse mode.
4. The method for controlling the ion mobility spectrometry-time of flight mass spectrometer according to claim 1, wherein:
the ionization source (1) is a photo-ionization source,63A Ni radioactive ionization source or a discharge ionization source.
5. The method for controlling the ion mobility spectrometry-time of flight mass spectrometer according to claim 1, wherein:
the inner diameter size range of the central through hole of each interface of the ion through hole (10), the Skimmer electrode (11) and the slit (12) is set to be 0.5-3 mm.
6. The method for controlling the ion mobility spectrometry-time of flight mass spectrometry as claimed in claim 1, wherein:
the time-of-flight mass spectrum (4) is arranged in a linear mode, a single reflection mode or a multiple reflection mode.
7. The method for controlling the ion mobility spectrometry-time of flight mass spectrometry as claimed in claim 1, wherein:
the data acquisition system (23) is set as a TDC acquisition card or an ADC acquisition card.
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| CN112461913B (en) * | 2020-11-06 | 2022-02-22 | 华南农业大学 | Method for improving identification capability of isomer compound |
| CN113539781B (en) * | 2021-07-01 | 2023-07-25 | 中国科学院大连化学物理研究所 | Pulse voltage waveform applied to BN ion gate |
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| CN101894727A (en) * | 2010-07-09 | 2010-11-24 | 复旦大学 | Primary ion source of secondary ion mass spectrometry |
| US8633436B2 (en) * | 2011-12-22 | 2014-01-21 | Agilent Technologies, Inc. | Data acquisition modes for ion mobility time-of-flight mass spectrometry |
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