CN209624506U - A kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus - Google Patents
A kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus Download PDFInfo
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- CN209624506U CN209624506U CN201920042010.XU CN201920042010U CN209624506U CN 209624506 U CN209624506 U CN 209624506U CN 201920042010 U CN201920042010 U CN 201920042010U CN 209624506 U CN209624506 U CN 209624506U
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Abstract
The utility model discloses a kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus, feature is: including gas-chromatography, mass spectrograph, metal electrode and insulation chamber, the surrounding of insulation chamber is disposed with the first passage of connection, second channel, third channel and fourth lane, first passage is connected to the capillary column outlet end of gas-chromatography, second channel is connected to carrier gas outlet side, third channel is connected to or is aligned with mass spectrometric injection port by insulated dielectric tube, fourth lane is connect with metal electrode, one end of metal electrode is set to enter insulation chamber, the other end of metal electrode is connect with power supply unit, airtight component is provided in each channel, advantage is: can reduce the diffusion of sample detached peaks, improve the Ionization Efficiency of sample.
Description
Technical field
The utility model relates to low temperature plasma technology of ion source fields more particularly to a kind of gas-chromatography-low temperature etc.
Gas ions ion-source mass spectrometer combined apparatus.
Background technique
Mass spectrograph is a kind of chemical analysis instrument being currently widely used, the basic principle is that each ingredient in sample is made to exist
It is ionized in ion source, generates the charged ion of various different mass-to-charge ratioes, recycle electric field or magnetic field to not homogeneity lotus
The ion motion of ratio generates different influences, to realize the detection of substance.
Ion source provides sample ions for mass spectrograph, and key is ionization techniques.Wherein, with dielectric barrier discharge from
Component (DBDI) is that the low temperature plasma ion source of representative is a kind of for mass spectrometric soft ionization ion source, main feature
It is that can generate stable low temperature plasma under atmospheric conditions.Low temperature plasma technology of ion source has without before sample
The advantages that processing, analysis speed fast, easy to use, therefore it has been widely used in the fields such as food inspection.
Low temperature plasma ion-source mass spectrometer is combined with gas chromatograph often in analysis gaseous sample, and sample is by gas phase
Chromatography capillary tubing string is separated, and is then mixed and is ionized with low temperature plasma Shu Jinhang near mass spectrograph injection port
Sample ions are generated, subsequent section sample ions enter mass spectrograph and analyzed.A kind of existing common low temperature plasma from
Coupling device associated with source mass spectrometer and gas chromatograph, structure can be found in shown in Fig. 1, and wherein GC indicates gas-chromatography,
Gas phase sample after gas-chromatography separates flows in a direction indicated by the arrow, and another channel metal electrodes connect high-voltage electricity HV, low temperature
(a-quadrant) ionizes gas near mass spectrograph injection port at an angle for plasma ion source and gas-phase chromatographic capillary column
Aspect product make after forming sample ions, sample segment ion can under the action of carrier gas stream enter mass spectrograph injection port into
Row analysis.
But above-mentioned existing low temperature plasma ion-source mass spectrometer is with gas chromatograph combined apparatus that there are still following
Problem: 1) the outlet air pressure of gas-phase chromatographic capillary column is atmospheric pressure, therefore is worked compared to conventional gas phase chromatography capillary tubing string
Low vacuum condition, isolated gaseous sample concentration can substantially be diluted in outlet end, and detached peaks is caused seriously to spread；2)
Gaseous sample is only converged with low temperature plasma beam in intersection with limited sectional area, therefore the sample size being ionized has
Limit causes ionization to be not thorough；3) sample ions that ionization generates enter mass spectrograph injection port by gas flow path effect, this
Kind ion transmission mode will cause biggish losses of ions in transmission process.Existing gas-chromatography-low temperature plasma ion
Above three problem existing for source mass spectrometer combined apparatus can integrate the amount of ions that limitation enters mass spectrograph detection, to limit
The detection limit of mass spectrograph detection.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the utility model provide a kind of gas-chromatography-low temperature etc. from
Daughter ion source mass spectrometer combined apparatus, can reduce the diffusion of sample detached peaks, improve the Ionization Efficiency of sample.
Technical solution adopted by the utility model to solve the above technical problems is as follows: a kind of gas-chromatography-low-temperature plasma
Body ion-source mass spectrometer combined apparatus, including gas-chromatography, mass spectrograph, metal electrode and insulation chamber, the insulation chamber
Surrounding be disposed with first passage, second channel, third channel and fourth lane with the described insulation chamber, institute
The first passage stated is connected to the capillary column outlet end of the gas-chromatography, and the second channel is with external for mentioning
For the carrier gas outlet side connection of carrier gas, the third channel is connected to by insulated dielectric tube with the mass spectrometric injection port
Or with the mass spectrometric injection port parallel alignment, the fourth lane connect with the metal electrode, makes described
One end of metal electrode enters the insulation chamber, and the other end of the metal electrode is electrically connected with external powering device,
Between the first passage and the capillary column outlet end, the second channel and the carrier gas outlet side it
Between, between the third channel and the insulated dielectric tube, between the fourth lane and the metal electrode
It is provided with airtight component.
In some embodiments, metal ring electrode, the metal ring electrode are arranged with outside the insulated dielectric tube
Inner sidewall and the outer wall of the insulated dielectric tube fit, the metal ring electrode be separately provided or be grounded or with
External powering device electrical connection.When thus applying different voltages on metal pin electrode and metal ring electrode, not similar shape can be constituted
The low temperature plasma ionization source of state.
In some embodiments, the insulation chamber is the central part of cross four-way, is connected with the insulation chamber
It is described that the logical first passage, the second channel, the third channel and the fourth lane is followed successively by this
Cross four-way four channels.Thus the central part of cross four-way can preferably provide a narrow airtight space, for low
The generation of isothermal plasma and the ionization of sample improve Ionization Efficiency to reduce the diffusion of sample detached peaks.
In some embodiments, the airtight component includes multiple casings and multiple matches with the casing
Ferrule fitting, multiple casings are respectively sleeved between the first passage and the capillary column outlet end, institute
Between the second channel stated and the carrier gas outlet side, between the third channel and the insulated dielectric tube and institute
Between the fourth lane stated and the metal electrode, the ferrule fitting keeps its guarantee airtight for casing described in clamping
Property.Multiple casings are used to prevent between each channel and pipeline/electrode to prevent gas leakage, guarantee air-tightness there are gap as a result,；Card
Bell and spigot joint further ensures that the air-tightness of device entirety for gripping sleeve.
In some embodiments, the arrival end insertion of the insulated dielectric tube third channel, described is exhausted
The outlet end insertion of the edge medium tube mass spectrometric injection port, the insulated dielectric tube use vitreous silica capillary.
Thus, it is possible to guarantee that sample ions completely into mass spectrograph, further avoid the loss of the sample ions in transmission process.
In some embodiments, the metal electrode uses metal pin electrode, one end of the metal pin electrode
Into the insulation chamber, the other end of the metal pin electrode is electrically connected with external powering device, described for Denso
Set load AC high voltage, the material that the metal pin electrode uses are as follows: tungsten, nickel, platinum, copper, the metal pin electrode
Outer diameter is 100~1000 microns.
In some embodiments, the material that the metal ring electrode uses are as follows: tungsten, nickel, platinum, copper, the metal
The spacing of ring electrode and the metal pin electrode depends on the easily ionizable degree and the power supply unit of the carrier gas
The AC high voltage amplitude of load.
In some embodiments, the carrier gas uses one of nitrogen, argon gas, helium, air or a variety of any
Mixing, the flow rates of the carrier gas are 10~100ml/min, and keep flow velocity uniform.Thus to guarantee mass spectrograph sample introduction
The low vacuum state of the mouth first order.
In some embodiments, the material that the cross four-way and the ferrule fitting use is polyethers ether
Ketone.Thus, it is possible to there is a situation where high-tension circuit short circuits during avoiding low temperature plasma from generating.
In some embodiments, the material that the casing uses is fluorinated ethylene propylene copolymer.Thus, it is possible to protect
Air-tightness between card capillary column, carrier gas capillary, insulated dielectric tube and metal pin electrode and cross four-way.
Compared with the prior art, the advantages of the utility model are: by one insulation chamber of building, it is narrow airtight using this
Space makes isolated gaseous sample concentration will not be in capillary for the generation of low temperature plasma and the ionization of sample
Column outlet end is substantially diluted, to reduce the diffusion of sample detached peaks；Gaseous sample and low temperature plasma beam are in insulated cavity
It crosses in the confined space of room, and is sufficiently reacted along insulated dielectric tube, keep reaction more thorough, to greatly improve by ion
The sample size of change improves Ionization Efficiency；Sample ions after ionization are directly entered spectrometer analysis through insulated dielectric tube, keep away
Losses of ions caused by having exempted from ion transmission process.In conclusion the utility model, which can be improved, eventually enters into mass spectrograph
The sample ions quantity of detection, to improve the detection limit of mass spectrograph detection.
Detailed description of the invention
Fig. 1 is coupling device associated with existing commonly a kind of low temperature plasma ion-source mass spectrometer and gas chromatograph
Structural schematic diagram；
Fig. 2 is a kind of gas-chromatography of the utility model-low temperature plasma ion-source mass spectrometer combined apparatus embodiment one
Structural schematic diagram；
Fig. 3 is a kind of gas-chromatography of the utility model-low temperature plasma ion-source mass spectrometer combined apparatus embodiment two
Structural schematic diagram.
Wherein, gas-chromatography 1, mass spectrograph 2, metal electrode 3, insulate chamber 4, first passage 5, second channel 6, and third is logical
Road 7, fourth lane 8, capillary column outlet end 9, carrier gas outlet side 10, insulated dielectric tube 11, injection port 12, carrier gas capillary
13, metal ring electrode 14, casing 15, ferrule fitting 16.
Specific embodiment
Below in conjunction with attached drawing gas-chromatography a kind of to the utility model-low temperature plasma ion-source mass spectrometer combined apparatus
It is described in further detail, but not as the restriction to the utility model.
Embodiment one
As shown in Fig. 2, a kind of gas-chromatography of the utility model-low temperature plasma ion-source mass spectrometer combined apparatus,
Including gas-chromatography 1, mass spectrograph 2, metal electrode 3 and insulation chamber 4, the surrounding of insulation chamber 4 is disposed with and insulated cavity
First passage 5, second channel 6, third channel 7 and the fourth lane 8 that room 4 is connected to, the capillary of first passage 5 and gas-chromatography
Column outlet end 9 is connected to, and second channel 6 is connected to the external carrier gas outlet side 10 for providing carrier gas, and third channel 7 passes through exhausted
Edge medium tube 11 is connected to the injection port 12 of mass spectrograph 2, and fourth lane 8 is connect with metal electrode 3, makes one end of metal electrode 3
Into insulation chamber 4, the other end of metal electrode 3 is electrically connected with external powering device (not shown), in first passage 5 and capillary
Between tubing string outlet end 9, between second channel 6 and carrier gas outlet side 10, between third channel 7 and insulated dielectric tube 11, the 4th
It is provided with airtight component between channel 8 and metal electrode 3, whole device is made to keep air-tightness.After the separation of gas-chromatography 1
Gas phase sample enters insulation chamber 4 through first passage 5, and carrier gas enters insulation chamber 4 through second channel 6, loads on metal electrode 3
After AC high voltage, carrier gas is ionized in insulated dielectric tube 11 and generates low temperature plasma, while in insulated dielectric tube 11,
Low temperature plasma sufficiently acts on generation sample ions with the gas phase sample after separating, and then sample ions pass under airflow function
Mass spectrograph 2 is transported to be tested and analyzed.
In the present embodiment, insulated dielectric tube 11 uses vitreous silica capillary, the arrival end insertion the of insulated dielectric tube 11
Mass spectrometric injection port 12 is inserted into triple channel 7, the outlet end of insulated dielectric tube 11, and the insertion of the outlet end of insulated dielectric tube 11 is deep
For degree in 1cm or so, thus, it is possible to guarantee that sample ions completely into mass spectrograph, further avoid the loss of sample ions.Specifically
Insulated dielectric tube 11 can be used internal diameter be 50~250 microns, outer diameter be 360 microns, length be 100~250mm tekite
English capillary.
In the present embodiment, gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus further includes carrier gas capillary
Pipe 13 is connected to capillary 13 with carrier gas outlet side 10 by carrier gas.
In the present embodiment, metal electrode 3 uses metal pin electrode, and one end of metal pin electrode enters insulation chamber 4, metal
The other end of pin electrode is electrically connected with external powering device, and power supply unit loads AC high voltage.
Also be arranged with metal ring electrode 14 in the present embodiment, outside insulated dielectric tube 11, the inner sidewall of metal ring electrode 14 with
The outer wall of insulated dielectric tube 11 fits, and metal ring electrode 14 is separately provided or is grounded or is electrically connected with external powering device
It connects.Apply different voltage on metal pin electrode and metal ring electrode as a result, the low temperature plasma electricity of different shape can be constituted
From source.Specifically can include: the first applies AC high voltage on metal pin electrode, metal ring electrode ground connection is constituted reversed low
Isothermal plasma ion source；Second, apply AC high voltage on metal pin electrode, metal ring electrode is earth-free, then is inserted into matter
The outlet end gas of the vitreous silica capillary of spectrometer injection port is formed virtually, is constituted and is applied ac high-voltage on metal pin electrode
Electricity, metal ring electrode ground connection；The third, metal pin electrode is grounded, and applies AC high voltage on metal ring electrode, constitutes low temperature etc.
Gas ions ion source.
In the present embodiment, the material of metal pin electrode and the use of metal ring electrode 14 are as follows: tungsten, nickel, platinum or copper etc., metal needle
The outer diameter of electrode is 100~1000 microns, and the spacing of metal ring electrode 14 and metal pin electrode depends on the easily ionizable journey of carrier gas
Degree and the AC high voltage amplitude of power supply unit load.Specifically, carrier gas more easily ionizable, load AC high voltage amplitude more
Greatly, then the spacing of metal ring electrode 14 and metal pin electrode can be bigger, and the range of spacing is in 1~5cm.Metal pin electrode or gold
The AC high voltage amplitude loaded on category ring electrode is 1~5 kilovolt, frequency is 1~100 kHz.
In the present embodiment, insulation chamber 4 uses the central part of a cross four-way, thus constitutes narrow airtight insulation
Chamber 4.First passage 5, second channel 6, third channel 7 and the fourth lane 8 being connected to insulation chamber 4 are followed successively by the cross four
Logical four channels along clockwise direction.Airtight component includes multiple casings 15 and multiple ferrule fittings matched with casing 15
16, multiple casings 15 are respectively sleeved between first passage 5 and capillary column outlet end 9, second channel 6 and carrier gas outlet side 10
Between between (further second channel 6 and carrier gas are between capillary 13), third channel 7 and insulated dielectric tube 11 and
Between four-way 8 and metal pin electrode.There are gaps for preventing between each channel and pipeline/electrode for casing 15, prevent gas leakage,
Ferrule fitting 16 is used to clamp the air-tightness to further ensure that device entirety.
Cross four-way and ferrule fitting 16 need to use insulating materials, occur during generating to avoid low temperature plasma high
The situation of volt circuit short circuit, in the present embodiment, the material that cross four-way and ferrule fitting 16 use is polyether-ether-ketone
(polyetheretherketone, PEEK), but not limited to this material.The material that casing 15 uses is perfluoroethylenepropylene copolymerization
Object (Fluorinated ethylene propylene, FEP), but not limited to this material.Thus, it is possible to guarantee capillary column, carry
Air-tightness between gas capillary, insulated dielectric tube and metal pin electrode and cross four-way.
In the present embodiment, carrier gas can be used one of nitrogen, argon gas, helium, air or it is a variety of mix in any proportion,
The flow rates of carrier gas are 10~100ml/min, and keep flow velocity uniform.Thus to guarantee 12 first order of mass spectrograph injection port
Low vacuum state.
Embodiment two
As shown in figure 3, a kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus, remaining structure and reality
It is identical to apply example one, the difference is that: in the present embodiment, third channel 7 passes through the sample introduction of insulated dielectric tube 11 and mass spectrograph 2
12 parallel alignments of mouth, the spacing range between the outlet end and injection port 12 of insulated dielectric tube 11 are 5~30mm.
A kind of gas-chromatography of the utility model-low temperature plasma ion-source mass spectrometer combined apparatus, basic principle are as follows: logical
One insulation chamber of building is crossed, using the narrow airtight space for the generation of low temperature plasma and the ionization of sample.Through gas
Gas phase sample after phase chromatographic isolation enters insulation chamber through first passage, and carrier gas enters insulation chamber, metal through second channel
After loading AC high voltage on electrode, carrier gas is ionized in insulated dielectric tube and generates low temperature plasma, while is situated between in insulation
In matter pipe, low temperature plasma sufficiently acts on generation sample ions with the gas phase sample after separating, and then sample ions are in air-flow
Mass spectrograph is transmitted under effect to be tested and analyzed.Based on features described above, the isolated gaseous sample of utility model device
Concentration will not substantially be diluted in capillary column outlet end, to reduce the diffusion of sample detached peaks；Gaseous sample and low temperature etc.
Gas ions beam crosses in insulation chamber confined space, and is sufficiently reacted along insulated dielectric tube, keeps reaction more thorough, from
And the sample size being ionized is greatly improved, improve Ionization Efficiency；Sample ions after ionization are direct through insulated dielectric tube
Losses of ions into spectrometer analysis, caused by avoiding in ion transmission process.In conclusion a kind of gas of the utility model
Phase chromatography-low temperature plasma ion-source mass spectrometer combined apparatus can be improved the sample ions number for eventually entering into mass spectrograph detection
Amount, to improve the detection limit of mass spectrograph detection.
It is worth noting that, the above is only the preferred embodiment of the present invention, it is practical new not thereby to limit this
The scope of patent protection of type, the utility model can also carry out the improvement of material and structure to the construction of above-mentioned various components,
Either it is replaced using technically equivalent ones.Therefore, the specification of the utility model is applied and diagramatic content made by equivalent knot
Structure variation, directly or indirectly applies to other correlative technology fields and is similarly all contained in the range that the utility model is covered
It is interior.
Claims (10)
1. a kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus, which is characterized in that including gas-chromatography,
Mass spectrograph, metal electrode and insulation chamber, the surrounding of the insulation chamber are disposed with and the insulation chamber
First passage, second channel, third channel and fourth lane, the capillary of the first passage and the gas-chromatography
The connection of column outlet end, the second channel are connected to the external carrier gas outlet side for providing carrier gas, and the third is logical
Road by insulated dielectric tube be connected to the mass spectrometric injection port or with the mass spectrometric injection port parallel alignment, institute
The fourth lane stated is connect with the metal electrode, and one end of the metal electrode is made to enter the insulation chamber, institute
The other end for the metal electrode stated is electrically connected with external powering device, is exported in the first passage and the capillary column
Between second channel and the carrier gas outlet side between end, described, the third channel and the insulated dielectric tube
Between, between the fourth lane and the metal electrode be provided with airtight component.
2. a kind of gas-chromatography according to claim 1-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, metal ring electrode, the inner sidewall of the metal ring electrode and the insulation is arranged with outside the insulated dielectric tube
The outer wall of medium tube fits, and the metal ring electrode is separately provided or is grounded or is electrically connected with external powering device.
3. a kind of gas-chromatography according to claim 1-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, the insulation chamber is the central part of cross four-way, the first passage, institute with the insulation chamber
Second channel, the third channel and the fourth lane stated are followed successively by four channels of the cross four-way.
4. a kind of gas-chromatography according to claim 3-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, the airtight component includes multiple casings and multiple ferrule fittings matched with the casing, multiple described
Casing is respectively sleeved between the first passage and the capillary column outlet end, the second channel and described
Between third channel and the insulated dielectric tube between carrier gas outlet side, described and the fourth lane and described
Between metal electrode, the ferrule fitting makes it guarantee air-tightness for casing described in clamping.
5. a kind of gas-chromatography according to claim 1-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, the arrival end insertion of the insulated dielectric tube third channel, the outlet end insertion of the insulated dielectric tube
The mass spectrometric injection port, the insulated dielectric tube use vitreous silica capillary.
6. a kind of gas-chromatography according to claim 2-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, the metal electrode uses metal pin electrode, and one end of the metal pin electrode enters the insulation chamber, institute
The other end for the metal pin electrode stated is electrically connected with external powering device, and the power supply unit loads AC high voltage, described
The material that uses of metal pin electrode are as follows: tungsten, nickel, platinum, copper, the outer diameter of the metal pin electrode are 100~1000 microns.
7. a kind of gas-chromatography according to claim 6-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, the material that the metal ring electrode uses are as follows: tungsten, nickel, platinum, copper, the metal ring electrode and the metal needle
The spacing of electrode depends on the easily ionizable degree of the carrier gas and the AC high voltage amplitude of the power supply unit load.
8. a kind of gas-chromatography according to claim 1-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, the carrier gas uses one of nitrogen, argon gas, helium, air or a variety of any mixing, the flow velocity of the carrier gas
Range is 10~100ml/min, and keeps flow velocity uniform.
9. a kind of gas-chromatography according to claim 4-low temperature plasma ion-source mass spectrometer combined apparatus, feature
It is, the material that the cross four-way and the ferrule fitting use is polyether-ether-ketone.
10. a kind of gas-chromatography according to claim 4-low temperature plasma ion-source mass spectrometer combined apparatus, special
Sign is that the material that the casing uses is fluorinated ethylene propylene copolymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920042010.XU CN209624506U (en) | 2019-01-10 | 2019-01-10 | A kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920042010.XU CN209624506U (en) | 2019-01-10 | 2019-01-10 | A kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN209624506U true CN209624506U (en) | 2019-11-12 |
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ID=68449383
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920042010.XU Withdrawn - After Issue CN209624506U (en) | 2019-01-10 | 2019-01-10 | A kind of gas-chromatography-low temperature plasma ion-source mass spectrometer combined apparatus |
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| Country | Link |
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| CN (1) | CN209624506U (en) |
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2019
- 2019-01-10 CN CN201920042010.XU patent/CN209624506U/en not_active Withdrawn - After Issue
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