CN104810234A - Mass spectrometer and ionization device thereof - Google Patents
Mass spectrometer and ionization device thereof Download PDFInfo
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- CN104810234A CN104810234A CN201410042449.4A CN201410042449A CN104810234A CN 104810234 A CN104810234 A CN 104810234A CN 201410042449 A CN201410042449 A CN 201410042449A CN 104810234 A CN104810234 A CN 104810234A
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Abstract
The invention provides an ionization device used for ionizing sample molecules. The ionization device comprises an atomizer and a microwave plasma emitter, wherein the atomizer receives and atomizes the sample molecules; and the microwave plasma emitter is used for emitting microwave plasmas and enabling the atomized sample molecules to be ionized through the microwave plasmas. According to the mass spectrometer and the ionization device, the high temperature atomizing method and the microwave plasma ionizing method are combined, so that the sample atomizing and ionizing are achieved, an original defect of insufficient light source energy of a microwave plasma is overcome ingeniously, and sensitivity of the mass spectrometer is improved. High temperature generated by the atomizer has large energy, so that the majority of samples can be atomized and metal ground-state atoms of the samples are obtained. The shortcomings of weak light source energy and low degree of ionization of the microwave plasma are effectively compensated.
Description
Technical field
The present invention relates to spectral instrument technical field, particularly relate to a kind of mass spectrometer and ionization apparatus thereof.
Background technology
Atomic spectroscopy is the main means that people carry out elementary composition analysis always.After particularly there is ICP light source (power is between 500 watts to the 5000 watts) appearance of excellent atomization and excitating performance.ICP spectroscopic methodology becomes the predominant methods of emission spectrographic analysis.For ultra trace analysis, ICP mass spectrography occupies obvious advantage.
Microwave plasma (MWP) light source that another and ICP grow up simultaneously have also been obtained to be applied comparatively widely.But the microwave energy that this kind of method uses is more weak.When sample introduction, sample is generally form aerosol by atomizer to send in microwave plasma source, and the input mode of this input mode and Flame Atomic Absorption Spectrometry is closely similar.Difference is, because microwave cannot provide enough energy and power, so the power of most of microwave all can absorb by sample solvent, the microwave energy really playing ionization effect is a very little part, cause weakening the ionizing power of sample, cause the ion current remitted its fury of mass spectral analysis, affect the sensitivity of complete machine.
Therefore, a kind of microwave plasma mass spectrometry method or the microwave plasma light source with higher microwave energy are provided, to overcome microwave plasma energy of light source (the chances are about 150 watts) shortcoming on the weak side, become a large technical problem urgently to be resolved hurrily in the industry.
Summary of the invention
The present invention will solve the more weak technical problem of the microwave energy of microwave plasma mass spectrometry method in prior art.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
The present invention proposes a kind of ionization apparatus, for ionization of sample molecule, wherein, described ionization apparatus comprises atomizer and microwave plasma launcher, described atomizer receives described sample molecule and makes its atomization, described microwave plasma launcher for penetrating microwave plasma, and makes atomizing sample molecule ionization by described microwave plasma.
According to an embodiment of the present invention, described atomizer is flame atomizer, and described flame atomizer is produced the flame region of flat by the burning of burning gases and made described sample molecule atomization.
According to another execution mode, the injection direction of described microwave plasma is perpendicular to the plane of described flame region.
According to another execution mode, described burning gases are air acetylene mist.
According to another execution mode, described atomizer is graphite furnace atomizer, comprise body of heater, be located at described furnace interior can through light graphite-pipe, be located at the sample introduction window of described body of heater upper end and be opened in the perforate of described body of heater both side ends, described sample molecule enters graphite-pipe by sample introduction window, sample molecule described in described graphite-pipe high temperature atomic, described microwave plasma injects described graphite-pipe with sample molecule described in ionization through described perforate.
According to another execution mode, direction is injected perpendicular to the light in described graphite-pipe in the injection direction of described microwave plasma.
According to another execution mode, the microwave plasma that described microwave plasma launcher sends is argon plasma.
In order to solve the problems of the technologies described above, the technical scheme that the present invention proposes also comprises: propose a kind of mass spectrometer, comprise sample source, ionization apparatus, mass analyzer and detector, wherein, described ionization apparatus is described ionization apparatus, described sample source releases sample molecule, and described ionization apparatus is to described sample molecule atomization and ionization, and Ionized sample ions enters after described mass analyzer separates by mass-to-charge ratio and enters described detector.
As shown from the above technical solution, the mass spectrometer that the present invention proposes and ionization apparatus thereof have introduced atomizing method on the basis of microwave plasma body technique, high temperature atomic mode is combined with microwave plasma mode, achieve atomization and the ionization of sample, the ingenious defect that compensate for original microwave plasma light source energy shortage, improves mass spectrometric sensitivity.Wherein, the high temperature that atomizer produces has larger energy, most of sample can be made by atomization, and obtain the metal ground state atom of sample.Effectively compensate for microwave plasma energy of light source more weak, the shortcoming that degree of ionization is lower.The microwave plasma that microwave plasma launcher sends can make sample be ionized and then carry out quality analysis by mass analyzer to ionizable sample.
Accompanying drawing explanation
Fig. 1 is the structural representation of the first execution mode of the ionization apparatus that the present invention proposes;
Fig. 2 is the workflow block diagram of the first execution mode of the ionization apparatus that the present invention proposes;
Fig. 3 is the structural representation of the second execution mode of the ionization apparatus that the present invention proposes;
Fig. 4 is the mass spectrometric workflow block diagram that the present invention proposes.
Wherein, description of reference numerals is as follows:
1. atomizer; 2. microwave plasma launcher; 3. flame atomizer; 30. burners; 31. flame regions; 32. atomizers; 33. spray chambers; 4. graphite furnace atomizer; 40. bodies of heater; 41. sample introduction windows; 42. perforates; 5. sample source; 6. mass analyzer; 7. detector.
Embodiment
The exemplary embodiments embodying feature & benefits of the present invention will describe in detail in the following description.Be understood that the present invention can have various changes in different embodiments, it neither departs from the scope of the present invention, and explanation wherein and to be shown in be the use explained in essence, and be not used to limit the present invention.
The present invention proposes a kind of mass spectrometer and this mass spectrometric ionization apparatus of composition, i.e. a kind of mass spectrometer in conjunction with atomizer and microwave plasma body technique.
Because the degree of ionization (ion number accounts for the ratio of whole atomic ion sum) of microwave plasma is lower, the ionization effect of ICP method cannot be reached.ICP method can be estimated by saha equation, and it can produce the degree of ionization close to 1%, makes ion concentration reach higher level, can be considered to hot plasma.And the degree of ionization of microwave plasma is lower, such as, the temperature of the argon flame that microwave produces, at about 2000 DEG C, according to the Boltzmann's Statistical distribution formula in atomic physics, show that ionization ionization energy is lower at the probability of the argon gas of 11ev at this temperature.Therefore existing microwave plasma light source to the degree of ionization of general metallic atom ten thousand/following, cannot instructions for use be met.
In order to solve the lower problem of microwave plasma energy of light source, and improve its degree of ionization, the invention provides following execution mode, mainly can be summarized as by atomization mode particularly high temperature atomic mode combine with microwave plasma mode, to realize the mode of " sample → atomization → ionization ".
Ionization apparatus execution mode 1
As shown in Figure 1, the present invention proposes a kind of ionization apparatus, for by sample molecule ionization.It mainly comprises atomizer 1 and microwave plasma launcher 2.Atomizer 1 is mainly used in receiving sample molecule and making its atomization.Microwave plasma launcher 2 is mainly used in penetrating microwave plasma, and makes atomizing sample molecule ionization by microwave plasma.
As depicted in figs. 1 and 2, in the present embodiment, this atomizer 1 is flame atomizer 3 and can selects traditional structure.This flame atomizer 3 produces plane thermal-flame by burning gases and makes sample molecule atomization.It mainly comprises the atomizer 32, spray chamber 33 and the burner 30 that connect successively.
In addition, as shown in Figure 1, the injection direction of microwave plasma is perpendicular to the almost plane of thermal-flame.
As shown in Figure 1, in the present embodiment, this microwave plasma launcher 2 can select traditional structure, and its microwave plasma launched can select argon plasma.Owing to containing argon ion in argon plasma, its electron affinity is 15.76V, can snatch away an electron outside nucleus relatively easily, whole metallic atom is ionized from metallic atom.
As shown in Figure 2, in the course of the work, sample molecule enters atomizer 32 and is atomized by this atomizer 32, and then becomes aerosol state.Sample molecule under aerosol state enters spray chamber 33 by further refinement and to mix with burning gases are full and uniform, reaches more stable laminar condition with the thermal-flame making flame atomizer 3 send.Wherein burning gases can select air acetylene mist, but not as limit, the flame temperature of this kind of burning gases can reach more than 2300 DEG C, can provide higher gross energy, the moisture in aerosol can be evaporated, and in combustion atomization major part sample molecule.Enter burner 30 with the full and uniform mixed sample molecule of burning gases and evaporate in thermal-flame, dry form Dry aerosol droplet, then being heated to dissociate becoming ground state free atom steam through thermal-flame melting, realizing atomizing function.Microwave plasma launcher 2 launches argon plasma with vertical angle to the thermal-flame region 31 in almost plane shape, the argon ion wherein contained snatches away an electron outside nucleus in atomizing sample molecule, sample atoms realizes ionization and releases, enter other analytical equipments, as mass analyzer etc.
In addition, the input mode of the sample molecule in present embodiment is not necessarily confined to the Sprayables such as aerosol, also can adopt solid-state or gaseous state direct injected.
Ionization apparatus execution mode 2
The second execution mode of ionization apparatus that the present invention proposes, the difference of itself and above-mentioned first execution mode is:
As shown in Figure 3, in the present embodiment, the atomizer 1 of this ionization apparatus is graphite furnace atomizer 4, and it utilizes larger current by the graphite-pipe of higher resistance value, makes sample molecule atomization to produce high temperature.This graphite furnace atomizer 4 also comprises body of heater 40, and this body of heater 40 inside is provided with can through the graphite-pipe originally for the light of atomic absorption spectroscopy, and this body of heater 40 upper end offers sample introduction window 41, and this body of heater 40 both side ends offers perforate 42.
In the course of work, sample molecule is entered the graphite-pipe being located at body of heater 40 inside by sample introduction window 41, and in graphite-pipe, make graphite-pipe produce high temperature by larger current, this temperature can reach 2000 ~ 3000 DEG C, to make sample molecule atomization.Microwave plasma launcher 2 is to penetrate argon plasma perpendicular in graphite-pipe through the angle of light, inject body of heater 40 by perforate 42 and enter graphite-pipe, the argon ion contained in argon plasma snatches away an electron outside nucleus in atomizing sample molecule, sample atoms realizes ionization and releases, and enters other analytical equipments.
Mass spectrometer execution mode
As shown in Figure 4, the mass spectrometer that the present invention proposes, comprise release sample molecule sample source 5, sample molecule carried out to Ionized ionization apparatus, receive ionizable sample molecule that ionization apparatus releases and the mass analyzer 6 that it is separated according to mass-to-charge ratio and detector 7.Wherein ionization apparatus is the ionization apparatus that the present invention proposes.
In the course of work, sample source 5 releases sample molecule, ionization apparatus is to sample molecule atomization and ionization, Ionized sample molecule enters mass analyzer 6, and after sample molecule separates by mass-to-charge ratio by mass analyzer 6, sample molecule enters detector 7, sample ions after separation enters detector 7 successively, gather and amplify ion signal, machine process as calculated, is depicted as mass spectrogram.
In addition, in the present embodiment, when the atomizer 1 in ionization apparatus is flame atomizer 3, light can be passed through in its thermal-flame region 31, to carry out atomic absorption spectroscopy, the mass spectrometer that namely the present invention proposes also can be used as a spectrum-mass spectrum double-duty plant.
Though exemplary embodiment describe mass spectrometer of the present invention and ionization apparatus thereof with reference to several, should be understood that term used be illustrate and illustrative, and not restrictive.Its design or essence is not departed from because the present invention can specifically implement in a variety of forms, therefore, above-described embodiment is not limited to any aforesaid details, and explain widely in the design that should limit in claim of enclosing and scope, therefore the whole change fallen in claim or its equivalent scope and remodeling all should be claim of enclosing and contained.
Claims (8)
1. an ionization apparatus, for ionization of sample molecule, is characterized in that, described ionization apparatus comprises:
Atomizer (1), receives described sample molecule and makes its atomization; And
Microwave plasma launcher (2), for penetrating microwave plasma, and makes atomizing sample molecule ionization by described microwave plasma.
2. ionization apparatus according to claim 1, it is characterized in that, described atomizer (1) is flame atomizer (3), and described flame atomizer (3) is produced the flame region (31) of flat by the burning of burning gases and made described sample molecule atomization.
3. ionization apparatus according to claim 2, is characterized in that, the injection direction of described microwave plasma is perpendicular to the plane of described flame region (31).
4. ionization apparatus according to claim 2, is characterized in that, described burning gases are air acetylene mist.
5. ionization apparatus according to claim 1, it is characterized in that, described atomizer (1) is graphite furnace atomizer (4), comprise body of heater (40), being located at described body of heater (40) inside can through the graphite-pipe of light, be located at the sample introduction window (41) of described body of heater (40) upper end and be opened in the perforate (42) of described body of heater (40) both side ends, described sample molecule enters graphite-pipe by sample introduction window (41), sample molecule described in described graphite-pipe high temperature atomic, described microwave plasma injects described graphite-pipe with sample molecule described in ionization through described perforate (42).
6. ionization apparatus according to claim 5, is characterized in that, direction is injected perpendicular to the light in described graphite-pipe in the injection direction of described microwave plasma.
7. mass spectrometer according to claim 1, is characterized in that, the microwave plasma that described microwave plasma launcher (2) sends is argon plasma.
8. a mass spectrometer, comprise sample source (5), ionization apparatus, mass analyzer (6) and detector (7), it is characterized in that, described ionization apparatus is the ionization apparatus in claim 1 ~ 8 described in any one, described sample source (5) releases sample molecule, described ionization apparatus is to described sample molecule atomization and ionization, and Ionized sample ions enters after described mass analyzer (6) separates by mass-to-charge ratio and enters described detector (7).
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| CN201410042449.4A CN104810234A (en) | 2014-01-28 | 2014-01-28 | Mass spectrometer and ionization device thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI603372B (en) * | 2016-04-15 | 2017-10-21 | 國立中山大學 | A chromatographic mass spectromery apparatus using combustion reaction as ionization source |
| TWI625759B (en) * | 2015-08-21 | 2018-06-01 | 日商埃耶士股份有限公司 | Analysis system and analysis method for online-transferred analysis sample |
| CN109427536A (en) * | 2017-08-31 | 2019-03-05 | 天源华威集团有限公司 | Plasma mass spectrograph and its ionization apparatus |
| CN110100300A (en) * | 2016-10-26 | 2019-08-06 | 诺韦恩斯有限责任公司 | Method for measuring spectrum |
| CN114774838A (en) * | 2022-06-21 | 2022-07-22 | 盐城市大丰华瑞精工机械有限公司 | Processing device for valve rod |
-
2014
- 2014-01-28 CN CN201410042449.4A patent/CN104810234A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI625759B (en) * | 2015-08-21 | 2018-06-01 | 日商埃耶士股份有限公司 | Analysis system and analysis method for online-transferred analysis sample |
| TWI603372B (en) * | 2016-04-15 | 2017-10-21 | 國立中山大學 | A chromatographic mass spectromery apparatus using combustion reaction as ionization source |
| CN110100300A (en) * | 2016-10-26 | 2019-08-06 | 诺韦恩斯有限责任公司 | Method for measuring spectrum |
| US11133168B2 (en) | 2016-10-26 | 2021-09-28 | University Of Basel | Method for spectrometry |
| CN109427536A (en) * | 2017-08-31 | 2019-03-05 | 天源华威集团有限公司 | Plasma mass spectrograph and its ionization apparatus |
| CN114774838A (en) * | 2022-06-21 | 2022-07-22 | 盐城市大丰华瑞精工机械有限公司 | Processing device for valve rod |
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Application publication date: 20150729 |