CN104377108A - In-situ pyrolytic ion source for detecting free radicals and reaction intermediates - Google Patents
In-situ pyrolytic ion source for detecting free radicals and reaction intermediates Download PDFInfo
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- CN104377108A CN104377108A CN201310352098.2A CN201310352098A CN104377108A CN 104377108 A CN104377108 A CN 104377108A CN 201310352098 A CN201310352098 A CN 201310352098A CN 104377108 A CN104377108 A CN 104377108A
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- ion source
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- reaction intermediate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N27/626—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 using heat to ionise a gas
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
Provided is an in-situ pyrolytic ion source for detecting free radicals and reaction intermediates. The ion source comprises a sample tube, a repelling electrode, an ionization chamber, a lamp filament, an outgoing electrode, a focusing electrode, an emitting electrode, a repelling plate and a grounding grid plate. The ion source starts from the sample tube, and the repelling electrode, the ionization chamber, the lamp filament, the outgoing electrode, the focusing electrode, the emitting electrode, the grounding grid plate and the repelling plate are arranged in sequence. Compared with the prior art, the in-situ pyrolytic ion source for detecting the free radicals and the reaction intermediates has the advantages that the structure is simple, cleaning is easy to carry out, detected materials can be pyrolyzed in the ionization chamber directly, and pyrolyzed products will enter a detector instantly. The in-situ pyrolytic ion source can be used for detecting the free radicals and the reaction intermediates in various chemical reactions.
Description
Technical field
The invention belongs to technology of instrument and meter field, being specifically related to a kind of in-situ heat solution ion source for detecting free radical and reaction intermediate.
Background technology
Mass-spectrometric technique is a kind of analytical method measuring ion charge-mass ratio, and its principle is that each component in sample is ionized in an ion source, generates the positively charged ion of different charge-mass ratio, through the effect of accelerating field, forms ion beam, enters mass analyzer.In the mass analyser, they are focused on and obtain mass spectrogram, thus determining its quality by velocity dispersion that recycling Electric and magnetic fields makes generation contrary respectively.
Mass spectrometer realizes above-mentioned separate analytical technique, thus the instrument of the quality of mensuration material, content and structure thereof.Utilize mass spectrometer can carry out the ultrapure trace analysis etc. of isotope analysis, compound analysis, gas composition analysis and metal and non-metal solid sample.The analysis and research of organic mixture demonstrate mass spectrometry and have more remarkable superiority than chemical analysis and Optical Analysis Method, and wherein organic compound mass spectral analysis accounts for maximum proportion in mass-spectrometry.At present be unable to do without mass spectrometer in the research of the scientific domains such as organic, biological, medical science, while mass spectrometer also play an important role in fields such as environmental monitoring, food security, production control and even national defense safeties.
Mass spectrometer conventional at present has level Four bar mass spectrometer, ion trap mass spectrometer, time-of-flight mass spectrometer etc.Level Four bar mass spectrum is the ion utilizing different quality, and in radiofrequency field, the difference of movement locus is analyzed by measured ion; Ion trap mass spectrometry is by the different ions different quality distinguishing ion of restraint conditions in an ion trap; Flight time mass spectrum is by after giving identical energy, and the ion flight that ion flight speed is slow, quality is little that quality is large this feature fast measures the quality of ion.
But the material overwhelming majority of real world is neutral state, and the prerequisite that the said equipment plays a role is by substance ion to be analyzed, the equipment completing this part work is called ion source.Current ion source generally has electron impact ion source, photo ionization ion source, gas discharge ion source, electric spray ion source, laser splash ion source etc. in principle.Wherein electron impact ion source is the technology that the gas utilizing beam bombardment to be measured makes it to ionize; Photo ionization ion source utilizes ultraviolet to live laser etc. by gas ionization; Gas discharge ion source utilizes gas discharge to ionize tested gas.Above-mentioned several ion source is applicable to the analysis of gas.Electric spray ion source utilizes liquid in time spraying with the capillary of high pressure, can be produced ion by attached charged phenomenon.Laser splash ion source is the technology utilizing superlaser bombardment solid directly to produce ion, for the analysis of solid sample.Ion source needs an ion transfer system by ion transfer in analyzer after generation ion.No analyzer is different to the requirement of ion beam, often have different ion transfer systems for the ion source of different analyzer.
Current ion source is generally made up of " sampling-ionization-ion transfer " three parts.Due to product to be measured or neutral state in sampling process, so some short-life molecules---free radical or reaction intermediate etc. easily react, reduce the real-time of analysis.The ion of some specific moleculars is also unstable simultaneously, in ion transfer process, also easily cancellation occurs, the integrality that impact detects.
Summary of the invention
In order to overcome the defect that prior art exists, the object of the present invention is to provide a kind of in-situ heat solution ion source for detecting free radical and reaction intermediate, its design philosophy is by measured matter directly pyrolysis in ionization chamber, and after thermal decomposition product is produced, the very first time is ionized.Adopt miniaturized design, reduce the distance that ion source transmits to analyzer, reduce the losses of ions in ion transfer process.
The invention provides a kind of in-situ heat solution ion source for detecting free radical and reaction intermediate, this ionization source comprises sample cell, repeller electrode, ionization chamber, filament, extraction pole, focusing electrode, goes out emitter-base bandgap grading, ground connection screen and repeller plate; Described ion source take sample cell as starting point, and sample cell is embedded in repeller electrode, connects ionization chamber, extraction pole, focusing electrode successively, goes out emitter-base bandgap grading, ground connection screen and repeller plate after repeller electrode, and filament is positioned on the left of ionization chamber.
In-situ heat solution ion source for detecting free radical and reaction intermediate provided by the invention, described sample cell is directly embedded in repeller electrode, and material is quartz.
In-situ heat solution ion source for detecting free radical and reaction intermediate provided by the invention, described filament adopts G4 type miniature bulb filament, and the voltage of filament is-70V.The voltage of described repeller electrode is 5 ~ 30V.The voltage of described extraction pole is 0 ~ 15V.The voltage of described focusing electrode is-110 ~ 0V.Described go out the voltage of emitter-base bandgap grading be-50 ~ 0V.
Material to be measured pyrolysis in sample cell, thermal decomposition product enters ionization chamber after the osculum ejection of repeller electrode.Ionization chamber has two kinds of ionization modes, and the light well of side is used for photo ionization.Ultraviolet light, laser, synchrotron radiation light etc. enter ionization chamber by light well and are ionized by thermal decomposition product.Because the distance of pyrolysis zone and ionization chamber is very near, so decrease the loss of free radical and reaction intermediate to greatest extent.The ion that ionization produces to analyzer repulsion by repeller electrode, is converged via extraction pole and focusing electrode, finally converges in ionogenic outlet in repulsion process.Energy and the directional spreding of outgoing ion can be regulated by regulating the voltage of repeller electrode, extraction pole, focusing electrode.
The present invention's advantage is compared with prior art: structure is simple, be convenient to cleaning, and tested substance can directly pyrolysis in ionization chamber, and thermal decomposition product will enter detector in the very first time.Ion source of the present invention may be used for the detection of various chemical reaction intermediate and free radical.
Accompanying drawing explanation
Fig. 1 is a kind of ionogenic structural representation of in-situ heat solution for detecting free radical and reaction intermediate of the present invention; Wherein, (1) is sample cell; (2) be repeller electrode; (3) be ionization chamber; (4) be filament; (5) be extraction pole; (6) be focusing electrode; (7) for going out emitter-base bandgap grading; (8) be ground connection screen; (9) be repeller plate.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further details.
As shown in Figure 1, a kind of in-situ heat solution ion source for detecting free radical and reaction intermediate of the present invention, this ionization source comprises sample cell, repeller electrode, ionization chamber, filament, extraction pole, focusing electrode, goes out emitter-base bandgap grading, ground connection screen and repeller plate (structure as shown in Figure 1); Described ion source is starting point with sample cell, is followed successively by repeller electrode, ionization chamber, filament, extraction pole, focusing electrode, goes out emitter-base bandgap grading, ground connection screen and repeller plate.
Sample feeding pipe is directly embedded in repeller electrode, and object is that the distance of pyrolysis zone and ionization chamber is diminished, and can reduce the loss of free radical and reaction intermediate to greatest extent.The ion that ionization produces to analyzer repulsion by repeller electrode, is converged via extraction pole and focusing electrode, finally converges in ionogenic outlet in repulsion process.Energy and the directional spreding of outgoing ion can be regulated by regulating the voltage of repeller electrode, extraction pole, focusing electrode.
Claims (7)
1. for detecting an in-situ heat solution ion source for free radical and reaction intermediate, it is characterized in that: this ionization source comprises sample cell, repeller electrode, ionization chamber, filament, extraction pole, focusing electrode, going out emitter-base bandgap grading, ground connection screen and repeller plate;
Sample cell is embedded in repeller electrode, connects ionization chamber, extraction pole, focusing electrode successively, goes out emitter-base bandgap grading, ground connection screen and repeller plate after repeller electrode, and filament is positioned on the left of ionization chamber.
2. according to described in claim 1 for detecting the in-situ heat solution ion source of free radical and reaction intermediate, it is characterized in that: described sample cell is directly embedded in repeller electrode, material be quartz.
3. according to described in claim 1 for detecting the in-situ heat solution ion source of free radical and reaction intermediate, it is characterized in that: described filament adopts G4 type miniature bulb filament, and the voltage of filament is-70V.
4. according to described in claim 1 for detecting the in-situ heat solution ion source of free radical and reaction intermediate, it is characterized in that: the voltage of described repeller electrode is 5 ~ 30V.
5. according to described in claim 1 for detecting the in-situ heat solution ion source of free radical and reaction intermediate, it is characterized in that: the voltage of described extraction pole is 0 ~ 15V.
6. according to described in claim 1 for detecting the in-situ heat solution ion source of free radical and reaction intermediate, it is characterized in that: the voltage of described focusing electrode is-110 ~ 0V.
7. according to described in claim 1 for detecting the in-situ heat solution ion source of free radical and reaction intermediate, it is characterized in that: described in go out emitter-base bandgap grading voltage be-50 ~ 0V.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310352098.2A CN104377108A (en) | 2013-08-13 | 2013-08-13 | In-situ pyrolytic ion source for detecting free radicals and reaction intermediates |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310352098.2A CN104377108A (en) | 2013-08-13 | 2013-08-13 | In-situ pyrolytic ion source for detecting free radicals and reaction intermediates |
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| CN104377108A true CN104377108A (en) | 2015-02-25 |
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| CN201310352098.2A Pending CN104377108A (en) | 2013-08-13 | 2013-08-13 | In-situ pyrolytic ion source for detecting free radicals and reaction intermediates |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107958833A (en) * | 2017-11-28 | 2018-04-24 | 厦门大学 | A kind of original position intermediate detection mass spectrometer |
| CN109192648A (en) * | 2018-08-09 | 2019-01-11 | 金华职业技术学院 | A kind of free radical photoproduct test method |
| WO2019084953A1 (en) * | 2017-11-02 | 2019-05-09 | 王健 | Ion counting detection device for tumor-related molecules, and using method therefor |
Citations (4)
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| CN101063673A (en) * | 2006-04-26 | 2007-10-31 | 中国科学院大连化学物理研究所 | Vacuumeultraviolet lamp ionization device in time-of-flight mass spectrometer |
| US20080142702A1 (en) * | 2006-12-18 | 2008-06-19 | Juergen Frosien | Gas field ion source for multiple applications |
| CN101592628A (en) * | 2009-06-30 | 2009-12-02 | 上海华质生物技术有限公司 | A kind of device and method that strengthens photoionization efficiency |
| CN202172061U (en) * | 2011-07-21 | 2012-03-21 | 厦门大学 | Compound ion source |
-
2013
- 2013-08-13 CN CN201310352098.2A patent/CN104377108A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101063673A (en) * | 2006-04-26 | 2007-10-31 | 中国科学院大连化学物理研究所 | Vacuumeultraviolet lamp ionization device in time-of-flight mass spectrometer |
| US20080142702A1 (en) * | 2006-12-18 | 2008-06-19 | Juergen Frosien | Gas field ion source for multiple applications |
| CN101592628A (en) * | 2009-06-30 | 2009-12-02 | 上海华质生物技术有限公司 | A kind of device and method that strengthens photoionization efficiency |
| CN202172061U (en) * | 2011-07-21 | 2012-03-21 | 厦门大学 | Compound ion source |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019084953A1 (en) * | 2017-11-02 | 2019-05-09 | 王健 | Ion counting detection device for tumor-related molecules, and using method therefor |
| US10859530B2 (en) | 2017-11-02 | 2020-12-08 | Jian Wang | Detection device for ion count in tumor-related molecules and usage method thereof |
| CN107958833A (en) * | 2017-11-28 | 2018-04-24 | 厦门大学 | A kind of original position intermediate detection mass spectrometer |
| CN109192648A (en) * | 2018-08-09 | 2019-01-11 | 金华职业技术学院 | A kind of free radical photoproduct test method |
| CN109192648B (en) * | 2018-08-09 | 2023-09-15 | 金华职业技术学院 | Free radical photo-product testing method |
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Application publication date: 20150225 |