CN107576524A - Solid sample microplasma sampler in a kind of open environment - Google Patents
Solid sample microplasma sampler in a kind of open environment Download PDFInfo
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- CN107576524A CN107576524A CN201710773869.3A CN201710773869A CN107576524A CN 107576524 A CN107576524 A CN 107576524A CN 201710773869 A CN201710773869 A CN 201710773869A CN 107576524 A CN107576524 A CN 107576524A
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- solid sample
- metal electrode
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Abstract
The invention discloses solid sample microplasma sampler in a kind of open environment, belongs to plasma generation and applied technical field, it includes：Metal electrode, medium hose, insulated dielectric tube, gas passage cylinder, high-voltage pulse power source, three-dimensional adjustable platform and protective gas；One end of insulated dielectric tube is fixed in gas passage cylinder, and the other end is to being connected to medium hose；Metal electrode is located in the centre bore of insulated dielectric tube and medium hose, and is connected with the output end of high-voltage pulse power source, as sparking electrode；The tip of three-dimensional adjustable platform and metal electrode for placing solid sample is relative, the ground terminal connection of solid sample and high-voltage pulse power source, as grounding electrode；Protective gas forms protective gas region by medium hose and metal electrode at the tip of metal electrode；The device can be sampled under open environment to solid material sample.
Description
Technical field
The invention belongs to plasma generation and applied technical field, and in particular to solid sample is micro- in a kind of open environment
Plasma sampler.
Background technology
The constituent of material is really permanent to be analyzed using means such as spectrum, mass spectrums.Spectroscopic methodology or mass spectrography pass through
The gaseous ion of sample is tested and analyzed, so that it is determined that its constituent.Spectroscopic methodology or mass spectrography can carry during once analyzing
For abundant sample structure information, therefore its extensive application in different scientific researches and field of industrial production.
Then traditional Mass Spectrometer Method process carries out gaseous ion under vacuum firstly the need of the making for carrying out sample
Preparation, separation, detection, therefore using traditional mass spectrum testing sample is carried out detection need longer sample preparation time and
Complicated operation.And increasing material with complex analysis such as the prison of reactant in alloy material, ore sample, pharmacy procedure
Survey, environmental monitoring, the science of law/judicial expertise, explosive and contraband detection etc. are intended to be rapidly completed under open environment.Simplify
Sample Preparation Procedure, realize that the sampling to sample turns into the pass that material composition is quickly analyzed in atmospheric pressure open type environment
Key link.
After active particle contacts with specimen material caused by discharge plasma, dissociating, being electric for specimen material can be caused
From formation is suitable for the gas phase sample particle of mass spectral analysis.At present, there is the sample plasma under a variety of atmospheric pressure
Source, forms the sample method in different atmospheric pressure open environments, such as PADI based on radio frequency discharge, is hindered based on medium
Keep off the DBDI to discharge, DRAT based on DC corona etc..These methods are operated in the aura or corona discharge shape of low current density
State, the energy density of input is smaller, and plasma temperature is low, is suitable for holding dissociable specimen material.And this kind of plasma
The effect solid such as metal sample high to fusing point difficult to realize sampling.The power density of arc discharge input is high, can be formed
High density, high energy plasma, so as to act on materials with high melting point, give in such as many documents and put using electric arc
The method of electricity sampling metal sample.But the method described by it is in the environment of low pressure, band vacuum system.Li etc. is designed
A kind of conductive solids sample sampler using arc discharge, but it is placed in sealed chamber.And under open environment,
Due to containing aerobic isoreactivity gas in air, directly electric discharge can cause the pollution of sparking electrode and specimen material in an atmosphere,
Influence the acquisition of element in sample.
The content of the invention
In view of this, it is an object of the invention to provide solid sample microplasma sampler in a kind of open environment,
Solid material sample can be sampled under open environment.
The present invention is achieved through the following technical solutions：
Solid sample microplasma sampler in a kind of open environment, including：Metal electrode, medium hose, insulation
Medium tube, gas passage cylinder, high-voltage pulse power source, three-dimensional adjustable platform and protective gas；
The metal electrode is hollow acicular texture；
Two or more axially extending bore is machined with the dielectric end surfaces；
Gas passage is machined with the gas passage cylinder；
Integrated connection relation is as follows：One end of insulated dielectric tube is fixed in the gas passage of gas passage cylinder, another
End is to being connected to medium hose；Metal electrode is located in the centre bore of insulated dielectric tube and medium hose, and it is soft that medium is stretched out at its tip
The end face of pipe, after the other end stretches out insulated dielectric tube, in the gas passage of gas passage cylinder, and the end and high-voltage pulse
The output end connection of power supply, as sparking electrode, carries out electric discharge sampling to solid sample, obtains microplasma；
The tip of three-dimensional adjustable platform and metal electrode for placing solid sample is relative, solid sample and high-voltage pulse
The ground terminal connection of power supply, as grounding electrode；Three-dimensional adjustable platform is used to adjust between the tip of metal electrode and solid sample
Distance and solid sample sample position；
Protective gas enters the hollow and insulated dielectric tube of metal electrode by the gas passage of gas passage cylinder
In axially extending bore, then by medium hose and metal electrode in the tip formation protective gas region of metal electrode.
Further, mass spectrograph is installed between three-dimensional adjustable platform in the sophisticated of metal electrode；Mass spectrograph is used to examine
Survey the microplasma and act on the gaseous ion for the metallic element to be formed with solid sample, to obtain forming into for solid sample
Point.
Further, spectrometer is installed between three-dimensional adjustable platform in the sophisticated of metal electrode；Spectrometer is used to examine
The spectrum that the microplasma acts on the gaseous ion for the metallic element to be formed with solid sample is surveyed, to obtain solid sample
Constituent.
Further, the tip diameter of the metal electrode is 2~200 μm.
Further, the insulated dielectric tube is using ceramics or PTFE.
Further, the gas passage cylinder uses tetrafluoro or ceramic material.
Further, the protective gas is the nitrogen or inert gas of setting flow velocity.
Further, the pulse voltage for the high-voltage pulse signal that the high-voltage pulse power source provides is more than 1KV, frequency
100Hz~10kHz, pulse width are the μ s of 200ns~5.
Further, the adjustable range of the three-dimensional adjustable platform is 0~1000 μm.
Beneficial effect：(1) under conditions of the present invention can realize under open environment i.e. atmospheric pressure, directly quickly to solid
Sample is sampled separation, avoids the Sample Preparation Procedure and power consumption of complexity, and saves the investment of the vacuum equipment of costliness, saves
Industrialize cost.
(2) present invention is passed through protective gas by using hollow needle-like metal electrode and insulated dielectric tube, makes ionization
Influence of the solid sample composition afterwards from caused various complicated ingredients after air ionization, so as to get solid sample information more
Add and purely well, be advantageous to the efficiency and accuracy rate that increase post analysis；Also achieve simultaneously to metal electrode (i.e. electric discharge electricity
Pole) protection, avoid frequently change electrode band cumbersome and fund consumption.
(3) present invention being used in combination by using three-dimensional adjustable platform and open environment, flexible can be realized with convenient
The sampling of coarse scale structures sample, sample diverse location.
(4) materials of the present invention are common, cheap, simple to operate, are very beneficial to scientific research use and industrialized production.
Brief description of the drawings
Fig. 1 is the structure composition schematic diagram of the present invention.
Fig. 2 is the spectrogram of the gained sample iron of embodiments of the invention 1.
Fig. 3 is the spectrogram of the gained sample aluminium of embodiments of the invention 2.
Fig. 4 is the spectrogram of the gained sample copper of embodiments of the invention 3.
Wherein, 1- metal electrodes, 2- medium hoses, 3- insulated dielectric tubes, 4- gas passage cylinders, 5- high-voltage pulse electrics
Source, 6- solid samples, 7- three-dimensional adjustable platforms, 8- mass spectrographs, 9- protective gas.
Embodiment
The present invention will now be described in detail with reference to the accompanying drawings and examples.
The invention provides solid sample microplasma sampler in a kind of open environment, referring to accompanying drawing 1, including：
Metal electrode 1, medium hose 2, insulated dielectric tube 3, gas passage cylinder 4, high-voltage pulse power source 5, solid sample 6, three-dimensional can
Leveling platform 7, mass spectrograph 8 and protective gas 9；
The metal electrode 1 is hollow acicular texture, and its tip diameter is 2~200 μm, has satisfactory electrical conductivity, is used
In as sparking electrode and being passed through protective gas 9；
Two or more is machined with the end face of insulated dielectric tube 3 along its circumferential evenly distributed axial through hole, insulation to be situated between
Matter pipe 3 is using ceramics or PTFE；
Cavity is machined with the gas passage cylinder 4, the cavity is gas passage, be easy to metal electrode 1 and absolutely
Protective gas 9 is passed through in edge medium tube 3, gas passage cylinder 4 is process using isolation materials such as tetrafluoro or ceramics；
The protective gas 9 is sets the nitrogen or inert gas of flow velocity, for example, helium, argon gas, neon etc., are used
In interference of the complicated ingredient to the constituent analysis of solid sample 6 caused by isolation air ionization, and it is more conducive to the breakdown of electric discharge and steady
It is fixed；
The pulse voltage for the high-voltage pulse signal that the high-voltage pulse power source 5 provides is more than 1KV, and frequency 100Hz~
10kHz, pulse width are the μ s of 200ns~5；
The adjustable range of the three-dimensional adjustable platform 7 is 0~1000 μm；
Integrated connection relation is as follows：One end of insulated dielectric tube 3 is fixed in the cavity of gas passage cylinder 4, the other end
Being coaxial docking has medium hose 2；Metal electrode 1 sequentially passes through insulated dielectric tube 3 and medium hose 2, and with insulated dielectric tube 3 and
Medium hose 2 is co-axially mounted；The tip of metal electrode 1 stretches out in the end face of medium hose 2, and the other end stretches out insulated dielectric tube 3
Afterwards, in the cavity of gas passage cylinder 4, and the end is connected with the output end of high-voltage pulse power source 5, as sparking electrode,
Electric discharge sampling is carried out to solid sample 6, obtains microplasma；
Three-dimensional adjustable platform 7 for placing solid sample 6 is relative with the tip of metal electrode 1, and three-dimensional adjustable platform 7
Platform surface it is vertical with metal electrode 1；Solid sample 6 is connected with the ground terminal of high-voltage pulse power source 5, as grounding electrode, three
Dimension adjustable platform 7 is used for the sample position of the distance between tip and solid sample 6 for adjusting metal electrode 1 and solid sample 6；
Protective gas 9 enters the hollow and insulated dielectric tube of metal electrode 1 by the gas passage of gas passage cylinder 4
In 3 axially extending bore, then by medium hose 2 and metal electrode 1 in the tip formation protective gas region of metal electrode 1；
Sophisticated in metal electrode 1 is provided with mass spectrograph 8 between three-dimensional adjustable platform 7；Mass spectrograph 8 is described for detecting
The gaseous ion for the metallic element that microplasma is formed with the effect of solid sample 6, to obtain the constituent of solid sample 6；
The mass spectrograph 8 could alternatively be spectrometer；Spectrometer is used to detect what the microplasma was formed with the effect of solid sample 6
The spectrum of the gaseous ion of metallic element, to obtain the constituent of solid sample 6.
Operation principle：After solid sample 6 is positioned on three-dimensional adjustable platform 7, pass through movable regulation metal electrode 1
Tip the distance between with solid sample 6, by left and right, move up and down the sample position of regulation solid sample 6；
After giving the pressure high-voltage pulse signal of metal electrode 1 by high-voltage pulse power source 5, at the tip of metal electrode 1 and admittedly
Micro- arc discharge is produced between body sample 6, forms microplasma, gold is formed by microplasma and the effect of solid sample 6
Belong to the gaseous ion of element, realize the separation to metallic element in solid sample 6, complete sampling；Then detected by mass spectrograph 8
The gaseous ion of solid sample 6, obtain so that it is determined that the constituent of solid sample 6；
Protective gas 9 is passed through from medium hose 2, insulated dielectric tube 3 and metal electrode 1 simultaneously, can avoid entering
During row electric discharge sampling, around gas condition produces pollution to sparking electrode and the sample elemental composition to being sampled causes shadow
Ring.
Embodiment 1：
The protective gas 9 is nitrogen (purity 99.99%), and solid sample 6 is pure iron (purity 99.99%)；
After connecting high-voltage pulse power source 5, metal sampler is carried out to pure iron, and using spectrum caused by the collection electric discharge of spectrometer 8, obtain spectrum
As shown in Figure 2；From spectrogram it can clearly be seen that except nitrogen ionizes spectral line, there is obvious iron atom spectral line：240nm,
260nm, 274nm, 301nm.Fe 3d is corresponded to respectively6(5D) 4p to 3d6(5D) transition between 4d, 3d6(3G)4s-3d6(3F2)4p
Between transition, 3d6(5D)4s-3d6(5D) transition between 4p, 3d64s4p3H4-3d74s3G3.Thus achieve the sampling of iron sample.
Embodiment 2：
The protective gas 9 is nitrogen (purity 99.99%), and flow 200slm, solid sample 6 is that aluminium foil is (pure
Spend for 99.99%)；The discharge voltage for connecting stabilization is 1.33kv, the high-voltage pulse that discharge current 8mA, pulse width are 2 μm
After power supply 5, metal sampler is carried out to aluminium foil, and using spectrum caused by the collection electric discharge of spectrometer 8, obtain spectrum as shown in Figure 3；
394nm and 396nm spectral lines are the spectral lines of emission of aluminium in figure.
Embodiment 3：
The protective gas 9 is nitrogen (purity 99.99%), and flow 200slm, solid sample 6 is that copper foil is (pure
Degree is 99.99%)；The discharge voltage for connecting stabilization is 1.33kv, the high-voltage pulse electric that discharge current 8mA, pulse width are 2 μm
Behind source 5, metal sampler is carried out to copper foil, and using spectrum caused by the collection electric discharge of spectrometer 8, obtain spectrum as shown in Figure 4.
In summary, presently preferred embodiments of the present invention is these are only, is not intended to limit the scope of the present invention.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (9)
- A kind of 1. solid sample microplasma sampler in open environment, it is characterised in that including：Metal electrode (1), it is situated between Matter flexible pipe (2), insulated dielectric tube (3), gas passage cylinder (4), high-voltage pulse power source (5), three-dimensional adjustable platform (7) and protection Property gas (9)；The metal electrode (1) is hollow acicular texture；Two or more axially extending bore is machined with insulated dielectric tube (3) end face；Gas passage is machined with the gas passage cylinder (4)；Integrated connection relation is as follows：One end of insulated dielectric tube (3) is fixed in the gas passage of gas passage cylinder (4), separately One end is to being connected to medium hose (2)；Metal electrode (1) is located in the centre bore of insulated dielectric tube (3) and medium hose (2), its The end face of medium hose (2) is stretched out at tip, after the other end stretches out insulated dielectric tube (3), the gas positioned at gas passage cylinder (4) In passage, and the end is connected with the output end of high-voltage pulse power source (5), and as sparking electrode, solid sample (6) is discharged Sampling, obtains microplasma；It is relative with the tip of metal electrode (1) for placing the three-dimensional adjustable platform (7) of solid sample (6), solid sample (6) with The ground terminal connection of high-voltage pulse power source (5), as grounding electrode；Three-dimensional adjustable platform (7) is used for the point for adjusting metal electrode (1) The distance between end and solid sample (6) and the sample position of solid sample (6)；Protective gas (9) enters the hollow and dielectric of metal electrode (1) by the gas passage of gas passage cylinder (4) In the axially extending bore for managing (3), then by medium hose (2) and metal electrode (1) metal electrode (1) tip formation protectiveness Gas zones.
- 2. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that Mass spectrograph (8) is installed between sophisticated (7) with three-dimensional adjustable platform of metal electrode (1)；Mass spectrograph (8) is described micro- for detecting The gaseous ion for the metallic element that plasma is formed with solid sample (6) effect, to obtain forming into for solid sample (6) Point.
- 3. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that Spectrometer is installed between sophisticated (7) with three-dimensional adjustable platform of metal electrode (1)；Spectrometer is used to detect micro- plasma The spectrum of the gaseous ion for the metallic element that body is formed with solid sample (6) effect, to obtain forming into for solid sample (6) Point.
- 4. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that institute The tip diameter for stating metal electrode (1) is 2~200 μm.
- 5. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that institute Insulated dielectric tube (3) is stated using ceramics or PTFE.
- 6. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that institute State gas passage cylinder (4) and use tetrafluoro or ceramic material.
- 7. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that institute State nitrogen or inert gas of the protective gas (9) for setting flow velocity.
- 8. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that institute The pulse voltage for stating the high-voltage pulse signal of high-voltage pulse power source (5) offer is more than 1KV, frequency 100Hz~10kHz, and pulse is wide Spend for the μ s of 200ns~5.
- 9. solid sample microplasma sampler in a kind of open environment as claimed in claim 1, it is characterised in that institute The adjustable range for stating three-dimensional adjustable platform (7) is 0~1000 μm.
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| CN201710773869.3A CN107576524A (en) | 2017-08-31 | 2017-08-31 | Solid sample microplasma sampler in a kind of open environment |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109238633A (en) * | 2018-11-02 | 2019-01-18 | 北京航天益森风洞工程技术有限公司 | A kind of stream field displaying apparatus |
| CN113552208A (en) * | 2021-07-08 | 2021-10-26 | 浙江大学 | Detection method of organic explosive substance |
| CN114068287A (en) * | 2021-10-26 | 2022-02-18 | 中国科学院上海有机化学研究所 | Energy-adjustable in-situ ionization method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114068287B (en) * | 2021-10-26 | 2023-03-14 | 中国科学院上海有机化学研究所 | Energy-adjustable in-situ ionization method |
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Application publication date: 20180112 |