CN209247687U - A kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry - Google Patents
A kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry Download PDFInfo
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- CN209247687U CN209247687U CN201821935176.6U CN201821935176U CN209247687U CN 209247687 U CN209247687 U CN 209247687U CN 201821935176 U CN201821935176 U CN 201821935176U CN 209247687 U CN209247687 U CN 209247687U
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Abstract
The utility model relates to a kind of organic matter detection devices of double focusing type fly chemical ionization mass spectrometry, including the gradually smaller source drift tube of discharge ion source, internal diameter and reaction tube, mass spectrometry detection system, alternating current-direct current composite power source etc.；The utility model detection method is realized by the source drift tube of ion focusing and the reaction tube of ion focusing to the parent ion of chemi-ionization and the double focus of product ion, by mass spectrometry detection system to the highly sensitive detection of the present line of ion core.The utility model compensates for the deficiency that ion boot efficiency is low in conventional source drift tube and reaction tube by double focusing pyrophosphate ion guidance reaction and Mass Spectrometer Method, and the efficient focusing guidance of ion may be implemented, to realize the highly sensitive on-line mass spectroscopy detection of organic matter.
Description
Technical field
The utility model belongs to analysis detection field, and in particular to a kind of volatility of double focusing type fly chemical ionization mass spectrometry
Organic matter detection device.
Background technique
Proton transfer reaction mass spectrometry technology is a kind of new development using ion-molecule reaction as the chemical ionization mass spectrometry of principle
Technology, it is usually to discharge to prepare the parent ion H of ion-molecule reaction by vapor3O+, then pass through ion source and reaction tube
Between aperture parent ion H3O+Reaction tube is introduced, in reaction tube, volatile organic matter M to be measured can be with H3O+Ion-occurs
Molecule reaction, is ionized as MH+。MH+It can finally be arrived by Mass Spectrometer Method, obtain molecular weight information and concentration information.The technology because
Have that highly sensitive, response is fast, soft ionization, does not need the advantages that calibration, is got in recent years in volatile organic matter monitoring analysis field
Paid attention to get over.
Although Proton transfer reaction mass spectrometry has been the chemical ionization mass spectrometry of most sensitive volatile organic matter detection at present
Technology, but its technology itself still has to be further improved and improves place, such as parent ion and product ion meeting in reaction tube
Off-axis diffusion, cannot be directed into adapter cavity and mass spectrum chamber so as to cause ion completely, so that detection sensitivity is affected,
(Wang Yujie and is applied to medical material detection research, the Chinese Academy of Sciences at Proton transfer reaction mass spectrometry technology so Wang Yujie et al.
Graduate school's doctoral thesis, 2011) it proposes ion funnel concept introducing reaction tube, improve detection sensitivity.However, putting
Also there is aperture to be connected between ionization component and reaction tube, in order to transmit parent ion H3O+If small aperture is become larger, react
Inner air tube is easy to participate in electric discharge in reflux to discharge ion source, generates a large amount of foreign ions, this can be by the ion-in reaction tube
Molecule reaction complicates, so the aperture between discharge ion source and reaction tube, which also limits parent ion, is efficiently entering reaction tube.
So the parent ion prepared in discharge ion source is increasingly introducing in reaction, and keeps in reaction tube ion efficiently to focus and draw
It leads, then can be further improved Proton transfer reaction mass spectrometry sensitivity.
Summary of the invention
The technology of the utility model solves the problems, such as: overcoming cannot be effective in existing Proton transfer reaction mass spectrometry discharge ion source
The deficiency for focusing guidance ion, provides a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry, passes through discharge ion
Source prepares parent ion H3O+、CH5 +Or NH4 +Deng being used as reactive ion, acted in focus type source drift tube and reaction tube internal electric field
Under, it realizes the efficient focusing guidance of parent ion and product ion, realizes to the highly sensitive on-line mass spectroscopy of volatile organic matter in atmosphere
Detection.
The utility model technical solution: a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry, including
The gradually smaller source drift tube 2 of discharge ion source 1, electrode internal diameter, the gradually smaller reaction tube 3 of electrode internal diameter, mass spectrometry detection system
System 4, alternating current-direct current composite power source 5；The described outlet of discharge ion source 1 with drift tube 2 entrance in source is concentric communicates, source drift tube 2
Outlet is communicated with 3 entrance of reaction tube by axle center aperture；The outlet of reaction tube 3 and the concentric phase of 4 entrance of mass spectrometry detection system
It is logical；The alternating current-direct current composite power source 5 is connected with discharge ion source 1, source drift tube 2 and reaction tube 3 respectively by conducting wire.The source
Drift tube 2 includes the diminishing source drift pipe electrode 6 of multiple internal diameters and multiple source drift tube insulation spacers 7, the multiple source
Drift tube insulation spacer 7 is interposed between the diminishing source drift pipe electrode 6 of multiple internal diameters；The reaction tube 3 includes in multiple
The diminishing reaction pipe electrode 8 of diameter, multiple reaction tube insulation spacers 9, sample introduction electrode 10, the multiple reaction tube insulation spacer
9 are interposed between the diminishing reaction pipe electrode 8 of multiple internal diameters；The sample introduction electrode 10 is 3 top inlet electrode of reaction tube.
Air pressure range is 60Pa~500Pa in the source drift tube 2 and reaction tube 3, and effective electric field range is 10V/cm
~700V/cm.
The discharge ion source 1 includes gas source 11 and discharge cavity 12, and gas source 11 is connected by gas pipeline with discharge cavity 12；
Air pressure range is 5Pa~200Pa in discharge cavity 12.
The mass spectrometry detection system 4 includes adapter cavity 13, mass spectrum chamber 14, vacuum pump group 15 and ion detection mass spectrum 16；It crosses
It crosses chamber 13 and is communicated with mass spectrum chamber 14 by concentric aperture；Vacuum pump group 15 passes through gas path pipe and adapter cavity 13, mass spectrum chamber 14
It communicates；Ion detection mass spectrum 16 is located at the intracavitary of mass spectrum chamber 14.
Segment electrode internal diameter is greater than 12 internal diameter of discharge cavity before the source drift tube 2, blocks without aperture therebetween, source drift tube
The hole diameter communicated between 2 and reaction tube 3 is 1mm~20mm；It is communicated between the reaction tube 3 and mass spectrometry detection system 4
Pore diameter range is 0.1mm~5mm；The hole diameter communicated between the adapter cavity 13 and mass spectrum chamber 14 be 0.1mm~
5mm。
The gas source 11 is vapor, methane gas or ammonia, and the gas flow of gas source 11 is 0.5ml/min~40ml/
min。
The utility model detection mode is as follows: parent ion prepared by discharge ion source 1, in the gradually smaller source of electrode internal diameter
It is focused guidance under rf electric field effect in drift tube 2, by the aperture between source drift tube 2 and reaction tube 3, by injection electricity
In the gradually smaller reaction tube 3 of pole internal diameter, it is inhaled into the organic matter to be measured of reaction tube 3, it is anti-that chemi-ionization occurs in reaction tube 3
It answers, obtains the product ion of organic matter to be measured；Product ion is focused guidance under the rf electric field effect in reaction tube 3, wears
The aperture communicated between reaction tube 3 and mass spectrometry detection system 4 is crossed, is detected into mass spectrometry detection system 4.Pass through source drift tube
Double focusing with reaction tube guides, and the high efficiency of transmission of parent ion and product ion is realized, thus to volatile organic matter in atmosphere
Highly sensitive on-line mass spectroscopy detection.
The utility model difference compared with prior art and advantage are:
(1) in Proton transfer reaction mass spectrometry, electric discharge is participated in due to preventing sample air from entering discharge ion source, so electric discharge
Ion source is connected by aperture with reaction tube, however the parent ion that discharge ion source generates but is easily detected by the entrance of this aperture
Reaction tube；In addition, because needing certain reaction pressure in reaction tube, and mass spectrum chamber needs low pressure mass spectrum that could work, institute
Also ion can only be guided by current limliting aperture to react pipe end, this also causes parent ion and product ion in reaction tube to be not easy to lead to
Small holes walk out reaction tube.This can all reduce the ion signal intensity that mass spectrum measures, and weaken detection sensitivity.The utility model
The source drift tube of ion focusing is increased between discharge ion source and reaction tube, reaction tube also uses the reaction of ion focusing type
Pipe realizes parent ion and product ion in the double focus of different phase jointly, improves the efficiency that ion passes through two apertures,
To further increase detection sensitivity, realize the chemical ionization mass spectrometry of similar Proton transfer reaction mass spectrometry to volatile organic matter
Highly sensitive detection.The utility model mainly include discharge ion source, the gradually smaller source drift tube of electrode internal diameter and reaction tube,
Adapter cavity, mass spectrum chamber, adapter cavity molecular pump, mass spectrum chamber molecular pump, fore pump, alternating current-direct current composite power source, injection port, ion detection
Mass spectrum, gas source etc..Source drift tube and reaction tube use simultaneously the gradually smaller electrode structure of internal diameter and with alternating current-direct current composite power source
Connected connection type is unlike the prior art.
(2) innovation of the utility model is: the gradually smaller source drift tube of electrode internal diameter and reaction tube while connecting
Connect alternating current-direct current composite power source, alternating current-direct current composite power source can in the gradually smaller source drift tube of electrode internal diameter and reaction tube shape simultaneously
At focusing electric field, off-axis ion can also be focused onto central core region after through source drift tube and reaction tube, to be easier
Pass through two apertures before and after reaction tube.For existing conventional protic transfer reaction mass spectrum, the utility model is maximum
Advantage is that can focus more parent ions enters reaction tube participation reaction, can be improved more parent ions and product ion
Fly out reaction tube, is arrived by rear end Mass Spectrometer Method, so detection volatile organic matter is sensitiveer.
Detailed description of the invention
Fig. 1 is a kind of volatile organic compound detection device signal of double focusing type fly chemical ionization mass spectrometry of the utility model
Figure；
Fig. 2 is that rf electric field modulates reaction tube and customary DC electric field reaction tube comparative test mass spectrogram.
Specific embodiment
As shown in Figure 1, a kind of volatile organic compound detection device of double focusing type fly chemical ionization mass spectrometry of the utility model
Embodiment include: discharge ion source 1, the gradually smaller source drift tube 2 of electrode internal diameter, the gradually smaller reaction tube 3 of electrode internal diameter,
Mass spectrometry detection system 4, alternating current-direct current composite power source 5；The described outlet of discharge ion source 1 with drift tube 2 entrance in source is concentric communicates,
The outlet of source drift tube 2 is communicated with 3 entrance of reaction tube by axle center aperture；The outlet of reaction tube 3 and 4 entrance of mass spectrometry detection system
It is concentric to communicate；The alternating current-direct current composite power source 5 by conducting wire respectively with 3 phase of discharge ion source 1, source drift tube 2 and reaction tube
Even.The source drift tube 2 includes the diminishing source drift pipe electrode 6 of multiple internal diameters and multiple source drift tube insulation spacers 7, institute
Multiple source drift tube insulation spacers 7 are stated to be interposed between the diminishing source drift pipe electrode 6 of multiple internal diameters；The reaction tube 3 wraps
Include the diminishing reaction pipe electrode 8 of multiple internal diameters, multiple reaction tube insulation spacers 9, sample introduction electrode 10, the multiple reaction tube
Insulation spacer 9 is interposed between the diminishing reaction pipe electrode 8 of multiple internal diameters；The sample introduction electrode 10 is that 3 top of reaction tube enters
Mouth electrode.The discharge ion source 1 includes gas source 11 and discharge cavity 12, and gas source 11 is connected by gas pipeline with discharge cavity 12；
The mass spectrometry detection system 4 includes adapter cavity 13, mass spectrum chamber 14, vacuum pump group 15 and ion detection mass spectrum 16；Adapter cavity 13 with
Mass spectrum chamber 14 is communicated by concentric aperture；Vacuum pump group 15 is communicated by gas path pipe with adapter cavity 13, mass spectrum chamber 14；Ion
Detection mass spectrum 16 is located at the intracavitary of mass spectrum chamber 14.Before the source drift tube 2 segment electrode internal diameter be greater than 12 internal diameter of discharge cavity, the two it
Between blocked without aperture.
The utility model method is realized are as follows: parent ion prepared by discharge ion source 1 floats in the gradually smaller source of electrode internal diameter
It is focused guidance under the rf electric field effect moved in pipe 2, by the aperture between source drift tube 2 and reaction tube 3, by injecting electrode
In the gradually smaller reaction tube 3 of internal diameter, it is inhaled into the organic matter to be measured of reaction tube 3, it is anti-that chemi-ionization occurs in reaction tube 3
It answers, obtains the product ion of organic matter to be measured；Product ion is focused guidance under the rf electric field effect in reaction tube 3, wears
The aperture communicated between reaction tube 3 and mass spectrometry detection system 4 is crossed, is detected into mass spectrometry detection system 4.Pass through source drift tube
Double focusing with reaction tube guides, and the high efficiency of transmission of parent ion and product ion is realized, thus to volatile organic matter in atmosphere
Highly sensitive on-line mass spectroscopy detection.
In order to obtain the highly sensitive detection effect of chemi-ionization, alternating current-direct current composite power source 5 should include multichannel high-voltage DC power supply
Output, the radio-frequency power supply output of 3 Electric Field Modulated of source drift tube 2 and reaction tube；Gas source 11 can be vapor, methane gas or ammonia
Equal gases, gas flow can select within the scope of 0.5ml/min~40ml/min；In discharge ion source 1 air pressure range be 5Pa~
200Pa；Air pressure range is 60Pa~500Pa, rf electric field and the DC electric field shape in source drift tube and reaction tube in reaction tube 3
At effective electric field range should be within the scope of 10V/cm~700V/cm.
Configured according to different vacuum system, the hole diameter communicated between source drift tube 2 and reaction tube 3 1mm~
Between 20mm, the pore diameter range communicated between the reaction tube 3 and mass spectrometry detection system 4 is 0.1mm~5mm；Described
The hole diameter communicated between adapter cavity 13 and mass spectrum chamber 14 is 0.1mm~5mm.
According to ion detection needs, ion detection mass spectrum 16 can be quadrupole rod mass spectrum, flight time mass spectrum, ion trap matter
The detection systems such as spectrum, Fourier transform ion cyclotron resonance mass spectroscopy or magnetic substance spectrum.
Fig. 2 gives with H3O+For chemical ionization mass spectrometry (that is: Proton transfer reaction mass spectrometry) Comparability test knot of parent ion
Fruit, line chart are the spectrograms of double focusing Proton transfer reaction mass spectrometry, and gray shade figure is the mass spectrographic spectrogram of conventional protic transfer reaction,
It can be seen that double focusing Proton transfer reaction mass spectrometry signal sensitivity more mass spectrographic than conventional protic transfer reaction is greatly improved, to difference
Substance about enhance 10~100 times and differ.
The utility model specification, which does not elaborate, partly belongs to techniques well known.
The above, only the utility model part specific embodiment, but the protection scope of the utility model not office
It is limited to this, any those skilled in the art within the technical scope disclosed by the utility model, the variation that can readily occur in or replace
It changes, should all cover within the protection scope of the present utility model.
Claims (6)
1. a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry, it is characterised in that: including discharge ion source (1),
Electrode internal diameter gradually smaller source drift tube (2), mass spectrometry detection system (4), is handed over the gradually smaller reaction tube of electrode internal diameter (3)
Direct current composite power source (5)；Described discharge ion source (1) outlet with source drift tube (2) entrance is concentric communicates, source drift tube
(2) outlet is communicated with reaction tube (3) entrance by axle center aperture；Reaction tube (3) outlet and mass spectrometry detection system (4) entrance
It is concentric to communicate；The alternating current-direct current composite power source (5) by conducting wire respectively with discharge ion source (1), source drift tube (2) and react
(3) are managed to be connected；The source drift tube (2) includes diminishing source drift pipe electrode (6) of multiple internal diameters and multiple source drift tubes
Insulation spacer (7), the multiple source drift tube insulation spacer (7) are interposed between diminishing source drift pipe electrode (6) of multiple internal diameters
Between；The reaction tube (3) include the diminishing reaction pipe electrode (8) of multiple internal diameters, multiple reaction tube insulation spacers (9),
Sample introduction electrode (10), the multiple reaction tube insulation spacer (9) be interposed between the diminishing reaction pipe electrode (8) of multiple internal diameters it
Between；The sample introduction electrode (10) is reaction tube (3) top inlet electrode.
2. a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry according to claim 1, it is characterised in that:
Source drift tube (2) and reaction tube (3) interior air pressure range are 60Pa~500Pa, and effective electric field range is 10V/cm~700V/
cm。
3. a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry according to claim 1, it is characterised in that:
The discharge ion source (1) includes gas source (11) and discharge cavity (12), and gas source (11) passes through gas pipeline and discharge cavity (12) phase
Even；Discharge cavity (12) interior air pressure range is 5Pa~200Pa.
4. a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry according to claim 1, it is characterised in that:
The mass spectrometry detection system (4) includes adapter cavity (13), mass spectrum chamber (14), vacuum pump group (15) and ion detection mass spectrum (16)；
Adapter cavity (13) is communicated with mass spectrum chamber (14) by concentric aperture；Vacuum pump group (15) passes through gas path pipe and adapter cavity
(13), mass spectrum chamber (14) communicates；Ion detection mass spectrum (16) is located at the intracavitary of mass spectrum chamber (14).
5. a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry according to claim 4, it is characterised in that:
Segment electrode internal diameter is greater than discharge cavity (12) internal diameter before the source drift tube (2), blocks without aperture therebetween, source drift tube (2)
The hole diameter communicated between reaction tube (3) is 1mm~20mm；Phase between the reaction tube (3) and mass spectrometry detection system (4)
Logical pore diameter range is 0.1mm~5mm；The hole diameter communicated between the adapter cavity (13) and mass spectrum chamber (14) is
0.1mm~5mm.
6. a kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry according to claim 3, it is characterised in that:
The gas source (11) is vapor, methane gas or ammonia, and the gas flow of gas source (11) is 0.5ml/min~40ml/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821935176.6U CN209247687U (en) | 2018-11-22 | 2018-11-22 | A kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry |
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| CN201821935176.6U CN209247687U (en) | 2018-11-22 | 2018-11-22 | A kind of organic matter detection device of double focusing type fly chemical ionization mass spectrometry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109307706A (en) * | 2018-11-22 | 2019-02-05 | 中国科学院合肥物质科学研究院 | A kind of the organic matter detection device and detection method of double focusing type fly chemical ionization mass spectrometry |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109307706A (en) * | 2018-11-22 | 2019-02-05 | 中国科学院合肥物质科学研究院 | A kind of the organic matter detection device and detection method of double focusing type fly chemical ionization mass spectrometry |
| CN109307706B (en) * | 2018-11-22 | 2024-01-02 | 中国科学院合肥物质科学研究院 | Organic matter detection device and detection method of double-focusing chemical ionization mass spectrum |
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