CN105489467B - A kind of chemi-ionization source device and its ionization detection method - Google Patents
A kind of chemi-ionization source device and its ionization detection method Download PDFInfo
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- CN105489467B CN105489467B CN201511028091.0A CN201511028091A CN105489467B CN 105489467 B CN105489467 B CN 105489467B CN 201511028091 A CN201511028091 A CN 201511028091A CN 105489467 B CN105489467 B CN 105489467B
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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
- H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
- H01J49/145—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using chemical ionisation
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- 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
- G01N27/68—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 electric discharge to ionise a gas
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Abstract
A kind of chemi-ionization source device of present invention offer and its ionization detection method, including：Mass spectrum injection port；Mass ions transfer tube runs through mass spectrum injection port；Minisize reaction room, minisize reaction room one end are fixed on mass spectrum injection port, and are penetrated through with one end of the mass ions transfer tube, minisize reaction room includes cavity, sample introduction pipeline and out sample tube road, wherein, out sample tube road is penetrated through with cavity one end, and the other end of sample introduction pipeline and cavity penetrates through；Ionization source spray point is set to the other end of minisize reaction room, and ionization source spray point includes syringe needle and applies the backshank of high pressure, and backshank is located at minisize reaction outdoor；Into and out of sampling device, respectively with disengaging sample piping connection；Sample to be tested device, connect with sampling device；Chemi-ionization source device through the invention and its ionization detection method solve the problems, such as the spectrogram vulnerable to pollution in open type atmospheric chemical ionization source in the prior art and the atmospheric chemical ionization source poor operability of large volume reative cell.
Description
Technical field
The present invention relates to a kind of ionization source device and its ionization detection methods, more particularly to a kind of closed very small chemical
Ionize source device and its ionization detection method.
Background technology
Mass spectrum (being called mass spectrography) is a kind of and spectrum spectrum method arranged side by side, refers to being widely used in respectively on ordinary meaning
By preparation, separation, detection gaseous ion come a kind of know-how of authenticating compound in a ambit.Mass spectrography is primary
Abundant structural information can be provided in analysis, it is one in separation science method breakthrough that isolation technics is combined with mass spectrography
Property progress.In numerous analysis test methods, mass spectrometric methods are considered as that one kind being provided simultaneously with high specific and highly sensitive
The universality method spent and be widely applied.Mass spectrometer generally by Sample introduction system, ion source, mass analyzer,
The part such as detector, data processing system forms.
(APCI) has the features such as simple in structure, high sensitivity in atmospheric chemical ionization source, and it is to be measured to be suitable for analysis polarity/low pole
Object.In the development of ionization mass spectrometry in situ (AIMS) in recent years, the ionization principle of APCI is also concerned, and has developed table
The technologies such as face desorption atmospheric chemical ionization (SDAPCI) are applied to the popular domains such as melamine detection, mass spectrum imaging, show
Preferable analytical performance.However, due in the ionization process of sample in the sources APCI, there is more complicated molecular ion to react
Process；Therefore, it is dirty that the spectrogram that the APCI mass spectrographies of open type record relatively is vulnerable to residual or reagent in Laboratory Air
The interference of dye.
And common commercialization atmospheric chemical ionization source (APCI) is using there is larger volume closed cavity conduct at present
The equipment of reative cell is (such as：The House components of power & light company, about 10~20cm square).The sources APCI usually by sample solution from
The capillary for being cased with atomization gas bushing introduces, then from capillary end ejection and by the carrier gas stream of big flow (High Purity Nitrogen air-flow)
Atomization, the fine drop of formation are vaporized in heating evaporation device, form gaseous neutral molecule, and heating pipe end has corona to put
Solvent molecule ionization is generated a large amount of reagent ion by acusector, corona discharge, and reagent ion is touched with gaseous state neutral species molecule
It hits, chemi-ionization occurs.As it can be seen that have larger dead volume in this reative cell, while detection process needs the load using big flow
Gas (high pure nitrogen) simultaneously need to be heated to (300 degree or so) auxiliary sample gasifications of higher temperature, and therefore, which is difficult to realize in real time
On-line monitoring, and operability is poor, actual effect is also unsatisfactory.
In consideration of it, it is necessary to design a kind of new chemi-ionization source device and its ionization detection method to solve above-mentioned skill
Art problem.
Invention content
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of chemi-ionization source device and its
Ionization detection method, the spectrogram vulnerable to pollution and large volume for solving open type atmospheric chemical ionization source in the prior art are anti-
The problem of answering the atmospheric chemical ionization source poor operability of room.
In order to achieve the above objects and other related objects, the present invention provides a kind of chemi-ionization source device, including：
Mass spectrum injection port；
Mass ions transfer tube, the mass ions transfer tube run through the mass spectrum injection port；
Minisize reaction room, minisize reaction room one end are fixed on the mass spectrum injection port, and with the mass spectrum from
One end of sub- transfer tube penetrates through, and the minisize reaction room includes cavity, sample introduction pipeline and out sample tube road, wherein it is described go out sample
Pipeline is penetrated through with described cavity one end, and the other end of the sample introduction pipeline and the cavity penetrates through；
Ionization source spray point, is fixed on the other end of the minisize reaction room, the ionization source spray point include syringe needle and
Apply the backshank of high direct voltage or coupled oscillations voltage, wherein the backshank is located at the minisize reaction outdoor；
Sampling device, with the sample introduction piping connection；
Go out sampling device, is connect with the out sample tube road；
Sample to be tested device is connect with the sampling device.
Preferably, apply the voltage of 0~500V in the inner wall of the minisize reaction room, or apply and passed with the mass ions
Defeated pipe is the same as equipotential voltage.
Preferably, it is described go out sampling device be asepwirator pump, sealing device or out sample tube one kind.
Preferably, the sampling device is one kind of head-space sampler or sample feeding pipe.
Preferably, it is described go out sampling device be out sample tube, the sampling device be sample feeding pipe, the out sample tube and the sample introduction
Pipe is penetrated through with the sample to be tested device respectively.
Preferably, the ionization source device further includes for adding to the sample introduction pipeline and minisize reaction room heating
Thermal, controllable temperature ranging from room temperature~400 DEG C of the heating device.
Preferably, the inner wall of the minisize reaction room is stainless steel material.
The present invention also provides a kind of ionization detection methods of atmospheric chemical ionization source device：
1) by the out sample tube road with it is described go out sampling device connect, described in sample to be tested in sample to be tested device warp
Sampling device and sample introduction pipeline enter in the minisize reaction room；
2) apply high direct voltage or coupled oscillations voltage at the backshank of the ionization source spray point, make that electricity occurs at needle point
Corona ionizes the sample to be tested gas；
3) ion generated sucks corresponding detection device by mass ions transfer tube, carries out Mass Spectrometer Method.
As described above, a kind of chemi-ionization source device and its ionization detection method of the present invention, have the advantages that：
Common external hanging type atmospheric chemical ionization source is miniaturized the chemi-ionization source device, and be directly installed on mass spectrographic normal pressure from
Son introduces interface；Narrow space in the reative cell of micromation, dead volume is small, improves the ion concentration near injection port, with
And Mass Spectrometer Method sensitivity, and air flow direction is more single, is conducive to ion and enters mass spectrum injection port；Meanwhile closed ion
Source and sampling device are exposed to the problems in air after having completely cut off sample collection, and avoid double between sample and laboratory
To pollution.As it can be seen that described device can effectively improve the ionizing efficiency and ion of ion source while simplifying instrument external structure
Efficiency of transmission improves Instrumental Analysis sensitivity；Suitable for the small-sized mass spectroscopy device such as bench device and portable, vehicular, more
It can be used for the related applications such as scene, mass spectrum monitoring real-time, in situ and process mass spectrum.
Description of the drawings
Fig. 1 is shown as the structural schematic diagram of the embodiment of the present invention one.
Fig. 2 is shown as the structural schematic diagram of minisize reaction room of the present invention.
Fig. 3 is shown as the structural schematic diagram of ionization source spray point of the present invention.
Fig. 4 is shown as the structural schematic diagram of the embodiment of the present invention two.
Fig. 5 is shown as the structural schematic diagram of the embodiment of the present invention three.
Fig. 6 is shown as the schematic diagram of ionization detection method of the present invention.
Component label instructions
1 mass spectrum injection port
2 mass ions transfer tubes
3 minisize reaction rooms
31 cavitys
32 sample introduction pipelines
33 out sample tube roads
4 ionization source spray points
41 syringe needles
42 backshanks
51 head-space samplers
52 sample feeding pipes
61 asepwirator pumps
62 sealing devices
63 out sample tubes
71 sample bottles
72 pipeline liquid injecting devices
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this specification below by way of specific specific example
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
It please refers to Fig.1 and Fig. 5.It should be clear that structure, ratio, size etc. depicted in this specification institute accompanying drawings, only to
Coordinate the revealed content of specification, so that those skilled in the art understands and reads, being not limited to the present invention can be real
The qualifications applied, therefore do not have technical essential meaning, the tune of the modification of any structure, the change of proportionate relationship or size
It is whole, in the case where not influencing the effect of present invention can be generated and the purpose that can reach, should all still fall in disclosed skill
Art content obtains in the range of capable of covering.Meanwhile in this specification it is cited as "upper", "lower", "left", "right", " centre " and
The term of " one " etc. is merely convenient to being illustrated for narration, rather than to limit the scope of the invention, relativeness
It is altered or modified, in the case where changing technology contents without essence, when being also considered as the enforceable scope of the present invention.
Embodiment one
As shown in Figure 1 to Figure 3, the chemi-ionization source device includes：
Mass spectrum injection port 1；
Mass ions transfer tube 2, the mass ions transfer tube 2 run through the mass spectrum injection port 1；
Minisize reaction room 3, described 3 one end of minisize reaction room are fixed on the mass spectrum injection port 1, and with the mass spectrum
One end of ion transfer tube 2 penetrates through, and the minisize reaction room 3 includes cavity 31, sample introduction pipeline 32 and out sample tube road 33,
In, the out sample tube road 33 is penetrated through with 31 one end of the cavity, and the sample introduction pipeline 32 and the other end of the cavity 31 penetrate through；
Ionization source spray point 4, is fixed on the other end of the minisize reaction room 3, and the ionization source spray point 4 includes syringe needle
41 and apply the backshank 42 of high direct voltage or coupled oscillations voltage, wherein the backshank 42 is located at outside the minisize reaction room 3
Portion；
Sampling device is connect with the sample introduction pipeline 32；
Go out sampling device, is connect with the out sample tube road 33；
Sample to be tested device is connect with the sampling device.
It should be noted that in the present embodiment, the mass spectrum injection port 1 is centrum.
It should be noted that in the present embodiment, the sample introduction pipeline 32 makes to enter the chamber at the syringe needle 41
Under test gas in body 31 is as fast as possible to be ionized；The out sample tube road 33 is located at the right side of the mass ions transfer tube 2
Top avoids ion from advancing into the out sample tube road into the mass ions transfer tube 2.
It should be noted that the length range of the minisize reaction room 3 is 10~30mm, inside diameter ranges are 3~7mm.It is excellent
Selection of land, in the present embodiment, the minisize reaction room 3 are the cylinder of internal diameter 6mm, long 20mm, wherein the sample introduction pipeline 32
Overall diameter is 1.6mm, interior diameter 1mm.
Explanation is needed further exist for, due to narrow space in reative cell, dead volume is small for the minisize reaction room 3, improves
Ion concentration near mass spectrum injection port 1, and then Mass Spectrometer Method sensitivity is improved, and air-flow in minisize reaction room 3
Flow direction is more single, is conducive to ion and enters mass spectrum injection port 1.3 compact of minisize reaction room can be directly anchored to described
On mass spectrum injection port 1.
It should be noted that apply high direct voltage or coupled oscillations voltage at the backshank 42 of the ionization source spray point 4,
Make that corona discharge occurs at syringe needle 41.In the present embodiment, apply 1.5~4kV at the backshank 42 of the ionization source spray point 4
High direct voltage so that at the syringe needle 41 occur corona discharge, the sample to be tested is ionized.
Explanation is needed further exist for, corona discharge is a complicated chemical process.In the present embodiment, put in ionization source
The high direct voltage for applying 1.5~4kV at the backshank 41 of acusector 4, when the electric field strength of syringe needle 42 is sufficiently high, the syringe needle 42 weeks
The easily ionizable substance enclosed by partial ionization, generates part of cation and electronics, the quantity of cation and electronics is basic at this time first
It is equal, and be distributed in close in the narrow space on 42 surface of syringe needle, so that the medium around syringe needle is in integrally electroneutral.But
It is that these charged particles obtain rapidly energy under the action of electric field, continues to collide with other neutral molecules, collide ionization
Reaction generates more charged particles, and these newly generated charged particle continuation obtain energy from electric field, then and around
Neutral molecule collides ionization reaction again, avalanche and discharge is ultimately formed, to obtain a large amount of high density sample to be tested
Ion.
It should be noted that the syringe needle 41 of the ionization source spray point 4 transmits at a distance from nozzle with mass ions in corona
In the bloom condition and range of electric discharge, usually 5~15mm, it is preferable that in the present embodiment, the syringe needle 41 and mass spectrum from
The distance of son transmission nozzle is 10mm.
It should be noted that the sample to be tested device is the device equipped with sample to be tested, it is preferable that the sample to be tested
Device can be sample bottle 71, closed container or pipeline liquid injecting device 72 equipped with sample to be tested.It is further preferred that in the present embodiment
In, the sample to be tested device is sample bottle 71.
Specifically, the inner wall of the minisize reaction room 3 is stainless steel material.
Specifically, it further includes for the heating to the sample introduction pipeline and minisize reaction room heating to state ionization source device
Device, controllable temperature ranging from room temperature~400 DEG C of the heating device.
It should be noted that the heating device can heat the minisize reaction room 3 and sample introduction pipeline 32.It is right
The minisize reaction room 3 is heated, first, the minisize reaction room 3 is directly connected to the mass ions transfer tube 2, it is described
Mass ions transfer tube 2 will heat, thus will by the minisize reaction room 3 carry out heating realize to the mass spectrum from
The heating of sub- transfer tube 2；Second is that have in the minisize reaction room 3 certain temperature (>80 degree or more are usual) after, ion and inner wall
Charge easy to be lost is not allowed after colliding.The heating device heats the sample introduction pipeline 32, to reduce memory effect.
Specifically, the inner wall in the minisize reaction room 3 applies the voltage of 0~500V, or apply and the mass ions
Transfer tube 2 is the same as equipotential voltage.
It should be noted that the voltage applied on the inner wall of the minisize reaction room 3 includes 0V, i.e., the described minisize reaction
The inner wall of room 3 can be grounded.By applying voltage on the inner wall of the minisize reaction room 3, first, being carried out centainly to ion
Repel, reduce its probability collided with inner wall, is strapped near axis transmission；Second is that the case where applying voltage to inner wall
Under, even if ion can reduce the probability for causing ion to lose charge because of collision if colliding with inner wall.
Specifically, the sampling device is one kind of head-space sampler 51 or sample feeding pipe 52.
It should be noted that the head-space sampler 51 is to solid sample, the fluid sample in the sample bottle 71
Or viscous samples are handled and are transported in the minisize reaction room 3, are specially heated in the sample bottle 71 and are waited for test sample
Product make volatile component be evaporated from sample matrices, balance are reached in gas-liquid or gas-particle two-phase, directly by heat temperature raising
Extraction top gas is connect to enter in the minisize reaction room 3.The sample feeding pipe 52 is then directly connected in 32 He of sample introduction pipeline
Between sample to be tested device, directly the volatile ingredient in the sample to be tested device is transported to by the sample feeding pipe 52 described
In minisize reaction room 3.In the present embodiment, the sampling device be head-space sampler 51, using head-space sampler 51 can in order to avoid
Except the sample pretreatment process of redundant and complicated, organic solvent is avoided to interfere, reduced to chromatographic column and injection port caused by analysis
Pollution.
Explanation is needed further exist for, the sampling device can assist, using other means for promoting desorption, improving
Sampling efficiency.Such as：Laser, heating, plasma etc..
Specifically, it is described go out sampling device be asepwirator pump 61, sealing device 62 or out sample tube 63 one kind.
It should be noted that in the present embodiment, it is described go out sampling device be asepwirator pump 61, to the minisize reaction room 3 into
Row pumping makes to form certain negative pressure in the minisize reaction room 3, in 32 pipette samples gas of sample introduction pipeline.
As shown in figures 1 to 6, a kind of ionization detection method of chemi-ionization source device：
1) by the out sample tube road 33 with it is described go out sampling device connect, the sample to be tested in the sample to be tested device is through institute
It states sampling device and sample introduction pipeline 32 enters in the minisize reaction room 3；
2) apply high direct voltage or coupled oscillations voltage at the backshank 42 of the ionization source spray point 4, make at needle point 41
Corona discharge occurs, the sample to be tested gas is ionized；
3) ion generated sucks corresponding detection device by mass ions transfer tube 2, carries out Mass Spectrometer Method.
It should be noted that in the present embodiment, the head-space sampler 51 is by the sample to be tested in the sample bottle 71
After being handled, enter in the cavity 31 through the sample introduction pipeline 32；The out sample tube road 33 is connect with the asepwirator pump 61,
The asepwirator pump 61 is evacuated the minisize reaction room 3, makes to form certain negative pressure in the minisize reaction room 3, pass through
Sample to be tested gas componant in the head-space sampler 51 is transported in the minisize reaction room 3 by sample introduction pipeline 32.
Embodiment two
As shown in figure 4, the chemi-ionization source device includes：
Mass spectrum injection port 1；
Mass ions transfer tube 2, the mass ions transfer tube 2 run through the mass spectrum injection port 1；
Minisize reaction room 3, described 3 one end of minisize reaction room are fixed on the mass spectrum injection port 1, and with the mass spectrum
One end of ion transfer tube 2 penetrates through, and the minisize reaction room 3 includes cavity 31, sample introduction pipeline 32 and out sample tube road 33,
In, the out sample tube road 33 is penetrated through with 31 one end of the cavity, and the sample introduction pipeline 32 and the other end of the cavity 31 penetrate through；
Ionization source spray point 4, is fixed on the other end of the minisize reaction room 3, and the ionization source spray point 4 includes syringe needle
41 and apply the backshank 42 of high direct voltage or coupled oscillations voltage, wherein the backshank 42 is located at outside the minisize reaction room 3
Portion；
Sampling device is connect with the sample introduction pipeline 32；
Go out sampling device, is connect with the out sample tube road 33；
Sample to be tested device is connect with the sampling device.
Specifically, the sampling device is one kind of head-space sampler 51 or sample feeding pipe 52.Preferably, in the present embodiment
In, the sampling device is head-space sampler 51.
Specifically, in the present embodiment, it is described go out sampling device be sealing device 62, will be described by the sealing device 62
Out sample tube road 33 blocks.
It should be noted that after being blocked the out sample tube road 33 with the sealing device 62, by using mass ions
The vacuum gradient pipette samples gas of itself in transfer tube 2.
Explanation is needed further exist for, for the ion source of atmospheric ionization, ion is to pass through an atmospheric pressure ion interface
(API, AP interface) introduces ion in vacuum.Usually there are two types of form, pass and transmission casts by API.The application is
Coordinate with ion transfer tube type.At mass ions transfer tube 2 in the minisize reaction room 3 in low vacuum (100Pa), institute
With, the gradient there are one from normal pressure to low vacuum is equivalent to inside mass ions transfer tube 2, for mass spectrum, ion be exactly
It is gone by air-flow inspiration under the action of this draught head, therefore, the present embodiment directly utilizes the suction of this air-breathing, and sample is inhaled
Enter into reative cell.However, the method is larger to mass spectrographic vacuum system burden, it is suitable for cleaner gaseous sample point
Analysis；Larger sample is polluted still to need to use asepwirator pump.
As shown in Figure 4 and Figure 6, a kind of ionization detection method of chemi-ionization source device：
1) by the out sample tube road 33 with it is described go out sampling device connect, the sample to be tested in the sample to be tested device is through institute
It states sampling device and sample introduction pipeline 32 enters in the minisize reaction room 3；
2) apply high direct voltage or coupled oscillations voltage at the backshank 42 of the ionization source spray point 4, make at needle point 41
Corona discharge occurs, the sample to be tested gas is ionized；
3) ion generated sucks corresponding detection device by mass ions transfer tube 2, carries out Mass Spectrometer Method.
It should be noted that in the present embodiment, the head-space sampler 51 is by the sample to be tested in the sample bottle 71
After being handled, enter in the cavity 31 through the sample introduction pipeline 32；The out sample tube road 33 connects with the sealing device 62
It connects, the out sample tube road 33 is blocked, sucked the sample to be tested using the vacuum gradient of itself in mass ions transfer tube 2
In the cavity 31.
Embodiment three
As shown in figure 5, the chemi-ionization source device includes：
Mass spectrum injection port 1；
Mass ions transfer tube 2, the mass ions transfer tube 2 run through the mass spectrum injection port 1；
Minisize reaction room 3, described 3 one end of minisize reaction room are fixed on the mass spectrum injection port 1, and the mass spectrum from
One end of sub- transfer tube 2 enters the inside of the minisize reaction room 3, and the minisize reaction room 3 includes cavity 31, sample introduction pipeline
32 and out sample tube road 33, wherein the out sample tube road 33 is penetrated through with 31 one end of the cavity, the sample introduction pipeline 32 with it is described
The other end of cavity 31 penetrates through；
Ionization source spray point 4, is fixed on the other end of the minisize reaction room 3, and the ionization source spray point 4 includes syringe needle
41 and apply the backshank 42 of high direct voltage or coupled oscillations voltage, wherein the backshank 42 is located at outside the minisize reaction room 3
Portion；
Sampling device is connect with the sample introduction pipeline 32；
Go out sampling device, is connect with the out sample tube road 33；
Sample to be tested device is connect with the sampling device.
Specifically, it is described go out sampling device be out sample tube 63, the sampling device be sample feeding pipe 52, the out sample tube 63 and institute
Sample feeding pipe 52 is stated to penetrate through with the sample to be tested device respectively.
It should be noted that when being analyzed for the sample in closed container or pipeline liquid injecting device, the sample introduction pipeline
32 and out sample tube road 33 joint be used as closed container or a branch of pipeline liquid injecting device, to avoid sampling process influence closed container
Or the environment in pipeline liquid injecting device.
Explanation is needed further exist for, the sample feeding pipe 52 and the out sample tube 63 connect with the pipeline liquid injecting device 72 respectively
It connects.When the under test gas in the pipeline liquid injecting device 72 is trend from top to bottom, so sample feeding pipe 52 is located at the minisize reaction
The top of room 3, the out sample tube 63 are located at the lower section of the minisize reaction room 3；Under test gas in the pipeline liquid injecting device 72
It is trend from down to up, the sample feeding pipe 52 is located at the lower section of the minisize reaction room 3, and the out sample tube 63 is located at described micro-
The top of type reative cell 3.Preferably, in the present embodiment, in the pipeline liquid injecting device 72 trend of under test gas be from top to bottom,
The i.e. described sample feeding pipe 52 is located at the top of the minisize reaction room 3, and the out sample tube 63 is located under the minisize reaction room 3
Side.
As shown in Figure 5 and Figure 6, a kind of ionization detection method of chemi-ionization source device：
1) by the out sample tube road 33 with it is described go out sampling device connect, the sample to be tested in the sample to be tested device is through institute
It states sampling device and sample introduction pipeline 32 enters in the minisize reaction room 3；
2) apply high direct voltage or coupled oscillations voltage at the backshank 42 of the ionization source spray point 4, make at needle point 41
Corona discharge occurs, the sample to be tested gas is ionized；
3) ion generated sucks corresponding detection device by mass ions transfer tube 2, carries out Mass Spectrometer Method.
It should be noted that in the present embodiment, the under test gas sample in the pipeline liquid injecting device 72 is through the sample feeding pipe
52 and the sample introduction pipeline 32 enter in the cavity 31；The out sample tube road 33 is connect with the out sample tube 63, will be described micro-
Under test gas in type reative cell 3 returns to pipeline liquid injecting device 72 by the out sample tube 63, reaches to 72 institute of the pipeline liquid injecting device
In the case where system does not make significant difference, realizes and the real time on-line monitoring of the gas componant in pipeline liquid injecting device 72 is analyzed.
In conclusion a kind of chemi-ionization source device of present invention offer and its ionization detection method, have below beneficial to effect
Fruit：Common external hanging type atmospheric chemical ionization source is miniaturized the chemi-ionization source device, and is directly installed on mass spectrographic normal
Ion is pressed to introduce interface；Narrow space in the reative cell of micromation, dead volume is small, and the ion improved near injection port is close
Degree and Mass Spectrometer Method sensitivity, and air flow direction is more single, is conducive to ion and enters mass spectrum injection port；Meanwhile it is closed
Ion source and sampling device are exposed to the problems in air after having completely cut off sample collection, and avoid between sample and laboratory
Two-way pollution.As it can be seen that described device simplify instrument external structure while, can effectively improve ion source ionizing efficiency and
Ion transmission efficiency improves Instrumental Analysis sensitivity；It is set suitable for the small-sized mass spectrum such as bench device and portable, vehicular
It is standby, most probably in related applications such as scene, mass spectrum monitoring real-time, in situ and process mass spectrums.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (8)
1. a kind of chemi-ionization source device, it is characterised in that：The chemi-ionization source device includes：
Mass spectrum injection port；
Mass ions transfer tube, the mass ions transfer tube run through the mass spectrum injection port；
Minisize reaction room, minisize reaction room one end are fixed on the mass spectrum injection port, and are passed with the mass ions
One end of defeated pipe penetrates through, and the minisize reaction room includes cavity, sample introduction pipeline and out sample tube road, wherein the length of the cavity
Spend ranging from 10~30mm, inside diameter ranges are 3~7mm, the out sample tube road and described cavity one end penetrate through and set on mass spectrum from
At the mass spectrum injection port, the other end of the sample introduction pipeline and the cavity penetrates through and close at son transmission nozzle rear
At the syringe needle of ionization source spray point；
Ionization source spray point is fixed on the other end of the minisize reaction room, and the ionization source spray point includes syringe needle and application
The backshank of high direct voltage or coupled oscillations voltage, wherein the backshank is located at the minisize reaction outdoor；
Sampling device, with the sample introduction piping connection；
Go out sampling device, is connect with the out sample tube road；
Sample to be tested device is connect with the sampling device.
2. chemi-ionization source device according to claim 1, it is characterised in that：Inner wall in the minisize reaction room applies
The voltage of 0~500V, or apply with the mass ions transfer tube with equipotential voltage.
3. chemi-ionization source device according to claim 1, it is characterised in that：It is described go out sampling device be asepwirator pump, sealing
One kind of device or out sample tube.
4. chemi-ionization source device according to claim 1, it is characterised in that：The sampling device be head-space sampler or
One kind of sample feeding pipe.
5. chemi-ionization source device according to claim 1, it is characterised in that：It is described go out sampling device be out sample tube, it is described
Sampling device is sample feeding pipe, and the out sample tube and the sample feeding pipe are penetrated through with the sample to be tested device respectively.
6. chemi-ionization source device according to claim 1, it is characterised in that：The ionization source device further include for pair
The heating device of the sample introduction pipeline and minisize reaction room heating, the controllable temperature ranging from room temperature of the heating device~
400℃。
7. chemi-ionization source device according to claim 1, it is characterised in that：The inner wall of the minisize reaction room is stainless
Steel material.
8. a kind of ionization detection method of chemi-ionization source device as described in claim 1, it is characterised in that：
1) by the out sample tube road with it is described go out sampling device connect, the sample to be tested in the sample to be tested device is through the sample introduction
Device and sample introduction pipeline enter in the minisize reaction room；
2) apply high direct voltage or coupled oscillations voltage at the backshank of the ionization source spray point, generation corona at needle point is made to put
Electricity ionizes the sample to be tested gas；
3) ion generated sucks corresponding detection device by mass ions transfer tube, carries out Mass Spectrometer Method.
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| CN106876241A (en) * | 2017-03-13 | 2017-06-20 | 中国石油大学(华东) | Ultrasonic atomizatio Atomospheric pressure glow discharge ionization device |
| CN108195923A (en) * | 2018-01-02 | 2018-06-22 | 清华大学深圳研究生院 | The method and mass spectrometer arrangement detected for volatile organic compounds in sample |
| CN108414608B (en) * | 2018-01-23 | 2021-01-01 | 中国中医科学院中药研究所 | Method for real-time on-line monitoring and analyzing chemical components in complex reaction system and special device thereof |
| CN114324548B (en) * | 2021-12-30 | 2023-12-12 | 中国电子产品可靠性与环境试验研究所（（工业和信息化部电子第五研究所）（中国赛宝实验室）） | Internal atmosphere content testing device and testing method |
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| CN101201335A (en) * | 2006-12-29 | 2008-06-18 | 东华理工学院 | Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum |
| CN104538277A (en) * | 2014-12-26 | 2015-04-22 | 宁波大学 | Discharging device and method applied to ion source |
| CN105206499A (en) * | 2015-10-14 | 2015-12-30 | 中国烟草总公司郑州烟草研究院 | Two-area reverse airflow atmospheric pressure chemical ionization source |
| CN205452234U (en) * | 2015-12-31 | 2016-08-10 | 上海华质生物技术有限公司 | Chemical ionization source device |
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| JP5002365B2 (en) * | 2007-08-06 | 2012-08-15 | 株式会社日立製作所 | Mass spectrometer and mass spectrometry method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101201335A (en) * | 2006-12-29 | 2008-06-18 | 东华理工学院 | Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum |
| CN104538277A (en) * | 2014-12-26 | 2015-04-22 | 宁波大学 | Discharging device and method applied to ion source |
| CN105206499A (en) * | 2015-10-14 | 2015-12-30 | 中国烟草总公司郑州烟草研究院 | Two-area reverse airflow atmospheric pressure chemical ionization source |
| CN205452234U (en) * | 2015-12-31 | 2016-08-10 | 上海华质生物技术有限公司 | Chemical ionization source device |
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