CN117995647A - Mass spectrometry apparatus and method based on multiple ionization techniques - Google Patents
Mass spectrometry apparatus and method based on multiple ionization techniques Download PDFInfo
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- CN117995647A CN117995647A CN202410404729.9A CN202410404729A CN117995647A CN 117995647 A CN117995647 A CN 117995647A CN 202410404729 A CN202410404729 A CN 202410404729A CN 117995647 A CN117995647 A CN 117995647A
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000004949 mass spectrometry Methods 0.000 title claims description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- 238000001819 mass spectrum Methods 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 9
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- 238000004458 analytical method Methods 0.000 description 1
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Abstract
The invention provides a mass spectrum device and a mass spectrum method based on various ionization technologies, wherein the mass spectrum device comprises a soft ionization unit, a sample injection cone and a power supply; the hard ionization unit comprises 2N electrodes, and is arranged between the soft ionization unit and the sample cone; the electrodes uniformly distributed on the circumference enclose a cylindrical structure, the 2i electrode is connected with the positive electrode of the power supply, the (2 i-1) electrode is connected with the negative electrode of the power supply, and i=1, 2 … N, N is a positive integer greater than 1; the distance between the output end of the hard ionization unit and the sample injection coneR is the maximum distance between electrodes in the hard ionization cell, Q is the gas flow, V is the discharge voltage, A is the coefficient, and t is the time. The invention has the advantages of simple structure and the like.
Description
Technical Field
The present invention relates to mass spectrometry, and in particular to a mass spectrometry apparatus and method based on multiple ionization techniques.
Background
Mass spectrometry is a powerful technical method in material analysis, and has been rapidly developed in recent years, and is an indispensable research tool in many fields such as proteomics and tissue imaging. Currently, ESI, HESI, APCI plasma devices are widely used for gas ionization. The disadvantage of this ionization regime is that:
1. The soft ionization mode has the problems of incomplete ionization, low ionization efficiency and the like, so that the signal strength is weaker, and the signal RSD is bigger.
2. An additional heating system is required, the power consumption is huge, and the operation and the manufacture are complex.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a mass spectrum device based on various ionization technologies.
The invention aims at realizing the following technical scheme:
A mass spectrometry device based on multiple ionization techniques, the mass spectrometry device comprising a soft ionization unit, a sample cone and a power supply; further comprises:
The hard ionization unit comprises 2N electrodes and is arranged between the soft ionization unit and the sample cone; the electrodes uniformly distributed on the circumference enclose a cylindrical structure, the 2i electrode is connected with the positive electrode of the power supply, the (2 i-1) electrode is connected with the negative electrode of the power supply, and i=1, 2 … N, N is a positive integer greater than 1;
The distance between the output end of the hard ionization unit and the sample injection cone R is the maximum distance between electrodes in the hard ionization cell, Q is the gas flow, V is the discharge voltage, A is the coefficient, and t is the time.
Another object of the present invention is to provide a mass spectrometry method, which is achieved by the following technical scheme:
a mass spectrometry method of a mass spectrometry apparatus according to the present invention based on a plurality of ionization techniques, the mass spectrometry method comprising the steps of:
(S1) sample gas flow into a soft ionization cell for a first stage ionization, after which the sample enters a hard ionization cell;
(S2) electrode discharge of the hard ionization unit, the produced ions enter the sample cone;
During discharge, the sample is heated, accelerating ionization efficiency.
Compared with the prior art, the invention has the following beneficial effects:
1. The ionization efficiency is high;
The hard ionization is added on the basis of soft ionization, so that the ionization efficiency is improved;
2. The signal-to-noise ratio is high;
in a hard ionization cell, high voltage is used, and the generated heat increases the temperature of the sample, facilitating ionization and increasing the signal to noise ratio.
Drawings
The present disclosure will become more readily understood with reference to the accompanying drawings. As will be readily appreciated by those skilled in the art: the drawings are only for illustrating the technical scheme of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic diagram of a mass spectrometry apparatus based on multiple ionization techniques according to an embodiment of the present invention;
fig. 2 is a schematic structural view of a hard ionization cell according to an embodiment of the present invention.
Detailed Description
Figures 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. In order to teach the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will appreciate variations or alternatives derived from these specific embodiments that fall within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the invention is not limited to the following alternative embodiments, but only by the claims and their equivalents.
Example 1:
As shown in fig. 1, a mass spectrometry apparatus based on multiple ionization techniques of embodiment 1 of the present invention includes:
the soft ionization unit 11, the sample injection cone 31 and the power supply;
A hard ionization unit 21, as shown in fig. 2, the hard ionization unit 21 includes 2N electrodes 22, and is disposed between the soft ionization unit 11 and the sample cone 31; the electrodes 22 uniformly distributed on the circumference enclose a cylindrical structure, the 2 i-th electrode 22 is connected with the positive electrode of the power supply, the (2 i-1) -th electrode 22 is connected with the negative electrode of the power supply, i=1, 2 … N, and N is a positive integer greater than 1;
the distance between the output end of the hard ionization unit 21 and the sample cone 31 R is the maximum distance between the electrodes 22 in the hard ionization cell 21, Q is the gas flow, V is the discharge voltage, A is the coefficient, and t is the time.
In order to improve ionization efficiency, further, the mass spectrometry apparatus further comprises:
A sheath 41, the soft ionization unit 11 and the hard ionization unit 21 are arranged in the sheath 41, and the sample cone 31 is arranged at the downstream of the outlet end of the sheath 41.
In order to achieve soft ionization, further, the soft ionization unit 11 includes:
The discharge needle 13 is inserted into the capillary tube 12, the two ends of the capillary tube 12 are open, the diameter of the output end is smaller than that of the input end, and the discharge needle 13 is inserted into the capillary tube.
The mass spectrometry method of the embodiment of the invention, that is, the working method of the mass spectrometry device based on various ionization technologies of the embodiment, comprises the following steps:
(S1) sample gas flow into soft ionization cell 11, first stage ionization, then sample into hard ionization cell 21;
(S2) the electrode 22 of the hard ionization unit 21 is discharged, and the generated ions enter the sample cone 31;
In the discharge, due to the high voltage, the generated heat increases the temperature of the sample, is favorable for ionization and improves the signal to noise ratio.
Example 2:
application example of mass spectrometry apparatus and method based on various ionization techniques according to embodiment 1 of the present invention.
In this application example, as shown in fig. 1, the soft ionization unit 11 includes a capillary 12 and a discharge needle 13, an output end of the capillary 12 is tapered, and a diameter of the outlet is smaller than a diameter of the input end. A discharge needle 13 is inserted into the capillary tube 12.
In the hard ionization cell 21, as shown in fig. 2, 8 rod-shaped electrodes 22 are used, uniformly distributed on the circumference. The (2 i-1) th electrode 22 is connected to the positive electrode of the power supply, and the (2 i-1) th electrode 22 is connected to the negative electrode of the power supply, i=1, 2,3,4.
The soft ionization cell 11 and the hard ionization cell 21 are both disposed within a cylindrical sheath 41, and the sample cone 31 is disposed downstream of the outlet of the sheath 41.
The power supply provides a high voltage of 5.5KV dc to the discharge needle 13 and a high voltage of 1KV ac to the electrode 22.
R is the distance between electrode plates, parameters affecting R include electrode plate materials, high voltage and sheath gas components, nitrogen is generally adopted as sheath gas, different materials can be known to have different gamma values according to Shang Xundi two coefficients gamma, and according to Shang Xundi two coefficients gamma and bar Shen Dinglv, and then according to the breakdown voltage expression, the parameters are selected to be 0.6cm in the embodiment.
Meanwhile, Q is selected to be 0.5L/min in the embodiment; a is a coefficient, which in this embodiment is selected to be 3; after D is defined, the sample is guaranteed to be in strong ionization before entering the cone opening. And the sample is fully ionized, and meanwhile, the sample is fully heated. If D is too small, the ionization range becomes small, the heating time becomes short, D is too large, the ionization range cannot be changed greatly, a period of cooling time is provided after heating, and insufficient heating is caused according to the formula: the distance between the output end of the hard ionization unit 21 and the sample cone 31R is the maximum distance between the electrodes 22 in the hard ionization cell 21, Q is the gas flow, V is the discharge voltage, a is the coefficient, t is the time, and d=2.62 cm is obtained, thereby realizing efficient ionization.
The mass spectrometry method of the embodiment of the invention, that is, the working method of the mass spectrometry device based on various ionization technologies of the embodiment, comprises the following steps:
(S1) sample gas flow enters sheath 41 and then passes through capillary 12, soft ionization cell 11, first stage ionization occurs, and then sample enters hard ionization cell 21;
(S2) the electrode 22 of the hard ionization unit 21 is discharged, and the generated ions enter the sample cone 31;
in the discharge, the sample is heated, and the ionization effect is improved.
Example 3:
an application example of the mass spectrometry apparatus and method based on various ionization techniques according to embodiment 1 of the present invention is different from embodiment 2 in that:
1. The electrode 22 is elongated.
Claims (6)
1. A mass spectrometry device based on multiple ionization techniques, the mass spectrometry device comprising a soft ionization unit, a sample cone and a power supply; the mass spectrum device based on the ionization technology is characterized by further comprising:
The hard ionization unit comprises 2N electrodes and is arranged between the soft ionization unit and the sample cone; the electrodes uniformly distributed on the circumference enclose a cylindrical structure, the 2i electrode is connected with the positive electrode of the power supply, the (2 i-1) electrode is connected with the negative electrode of the power supply, and i=1, 2 … N, N is a positive integer greater than 1;
The distance between the output end of the hard ionization unit and the sample injection cone R is the maximum distance between electrodes in the hard ionization cell, Q is the gas flow, V is the discharge voltage, A is the coefficient, and t is the time.
2. The mass spectrometry apparatus of claim 1, wherein the mass spectrometry apparatus further comprises:
The sheath, soft ionization unit and hard ionization unit set up in the sheath, the syringe cone sets up the low reaches of sheath exit end.
3. The mass spectrometry apparatus of claim 1, wherein the soft ionization unit comprises:
The discharge needle stretches into the capillary tube.
4. The mass spectrometry apparatus of claim 1, wherein the electrodes are sheet-like.
5. A method of mass spectrometry of a mass spectrometry device based on a plurality of ionization techniques according to any one of claims 1 to 4, the method comprising the steps of:
(S1) sample gas flow into a soft ionization cell for a first stage ionization, after which the sample enters a hard ionization cell;
(S2) electrode discharge of the hard ionization unit, the produced ions enter the sample cone;
During discharge, the sample is heated, accelerating ionization efficiency.
6. The method of mass spectrometry of claim 5, wherein a power supply applies a dc high voltage to the soft ionization and an ac high voltage to the hard ionization cell.
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US20160005578A1 (en) * | 2013-01-28 | 2016-01-07 | Westfaelische Wilhelms-Universitaet Muenster | Parallel elemental and molecular mass spectrometry analysis with laser ablation sampling |
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CN111551628A (en) * | 2020-06-08 | 2020-08-18 | 中国计量科学研究院 | Electron bombardment ionization source device, ionization bombardment method and substance analysis method |
CN213424921U (en) * | 2020-10-21 | 2021-06-11 | 杭州蔚领知谱检测技术有限公司 | Electron bombardment and VUV ultraviolet lamp composite ion source system |
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 |
CN219123181U (en) * | 2022-11-27 | 2023-06-02 | 浙江双谱科技有限公司 | Time-of-flight mass spectrometry system based on dual ion sources |
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- 2024-04-07 CN CN202410404729.9A patent/CN117995647A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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US20160005578A1 (en) * | 2013-01-28 | 2016-01-07 | Westfaelische Wilhelms-Universitaet Muenster | Parallel elemental and molecular mass spectrometry analysis with laser ablation sampling |
US20160276144A1 (en) * | 2015-03-16 | 2016-09-22 | Sri International | Ruggedized advanced identification mass spectrometer |
CN109887833A (en) * | 2019-03-06 | 2019-06-14 | 杭州蔚领知谱检测技术有限公司 | A kind of combined type ion source bipolarity linear ion trap mass analyzer |
CN111551628A (en) * | 2020-06-08 | 2020-08-18 | 中国计量科学研究院 | Electron bombardment ionization source device, ionization bombardment method and substance analysis method |
CN213424921U (en) * | 2020-10-21 | 2021-06-11 | 杭州蔚领知谱检测技术有限公司 | Electron bombardment and VUV ultraviolet lamp composite ion source system |
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 |
CN219123181U (en) * | 2022-11-27 | 2023-06-02 | 浙江双谱科技有限公司 | Time-of-flight mass spectrometry system based on dual ion sources |
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