CN105717092B - A kind of DBD excitaton sources, DBD-AES systems and its determination method - Google Patents
A kind of DBD excitaton sources, DBD-AES systems and its determination method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000012159 carrier gas Substances 0.000 claims abstract description 59
- 210000002381 plasma Anatomy 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 24
- 238000000295 emission spectrum Methods 0.000 claims abstract description 21
- 239000010453 quartz Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012530 fluid Substances 0.000 claims abstract description 15
- 238000002347 injection Methods 0.000 claims abstract description 15
- 239000007924 injection Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000000443 aerosol Substances 0.000 claims description 8
- 230000005284 excitation Effects 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 12
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000004445 quantitative analysis Methods 0.000 abstract description 3
- 238000000712 atomic emission detection Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 9
- 230000004888 barrier function Effects 0.000 description 7
- 239000011888 foil Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000005030 aluminium foil Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 241001474374 Blennius Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/69—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence specially adapted for fluids, e.g. molten metal
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Abstract
The present invention for DBD-AES system liquids sample introduction in the prior art there are the problem of, provide a kind of DBD excitaton sources, DBD-AES systems and its determination method, belong to atomic emission detection equipment and analysis technical field.The DBD excitaton sources are open plasma exciatiaon source, are made of electrode one, electrode two and power supply system；Electrode one is the conductive metal sheet being attached on quartz plate；Electrode two is made of atomizer and the conductive metal paillon being wrapped on atomizer exit side wall.The DBD-AES systems are by above-mentioned DBD excitaton sources, sequential injection system, carrier gas bottle and CCD detector composition.The excitaton source of the system uses style of opening DBD plasmas and Liquid sample introduction mode, it is ensured that while DBD plasma stabilities are discharged, is introduced directly into fluid sample, generates sensitive emission spectrum signal, quantitative analysis is carried out to determinand；The system sample introduction flow velocity is fast, detection frequency is high, substantially increases analysis efficiency, saves detection time.
Description
Technical field
The invention belongs to atomic emission detection equipment and analysis technical field, more particularly to a kind of Liquid sample introduction
DBD excitaton sources, DBD-AES systems and its determination method.
Background technology
Dielectric barrier discharge (DBD) is a kind of simple in structure, low energy consumption, and what can be generated at normal temperatures and pressures is non-equilibrium
State plasma.Characteristic research about DBD plasmas is it has been reported that it is generally believed that when breakdown voltage is hit more than Pachen
When wearing voltage, interelectrode gas can be breakdown, generates the light of bluish violet.In DBD discharge processes, produce a large amount of free radicals and
Quasi-molecule, their chemical property is very active, can provide energy for the test substance in analyte, make its atomization or by
Ground state atom is energized into higher excitation state, generates spectral signal.In atomic spectroscopic analysis, DBD can be used in excitaton source, original
Sonization device, induced chemical vapor generation etc..
DBD-AES system full name are dielectric barrier discharge plasma atomic emission spectrum, and DBD plasmas are sent out in atom
The application penetrated in spectrum includes mainly two parts, gas sampling AES analyses and Liquid sample introduction AES analyses.
Gas sampling AES analyses, since the mode of solution (atomization) sample introduction can consume the energy of DBD plasmas, even
Plasma is quenched, in order to avoid these problems, the general sample introduction by the way of steam generation.For DBD-AES systems,
The input mode occurred using steam, can be isolated element to be measured in the form of volatile matter or half volatile matter from solution
Come, sample matrices is avoided to interfere, reduces energy of plasma consumption, improve sensitivity.However, the main side that steam occurs
Formula --- hydride will produce a large amount of hydrogen and vapor, and DBD plasmas is easily caused to quench；Other steams occur
Mode or application element are limited in scope, and steam luminous efficiency is low, and speed is slow, unstable products or gas occurrence condition compared with
For harshness.The measurement range of DBD-AES systems is greatly limited to.
Relative to gas sampling, the AES analyses of Liquid sample introduction are more difficult to the excitation of metallic element in liquid.This is needed
Higher plasma exciatiaon ability, it is necessary to note that the Matrix effects and sample plasma of solvent interference.2010,
Tombrink etc. is that DBD-AES fluid analysis aspects have done a large amount of research work, establishes liquid electrode dielectric barrier discharge
Device；2012, He etc. reported a kind of DBD devices of liquid film generation atomic emission spectrum；But these device and method
Defect is that analyze speed is slow, and sensitivity is low, and the needs of routine testing are not achieved in the detection limit of element to be measured.
Invention content
The present invention for DBD-AES system liquids sample introduction in the prior art there are the problem of, provide a kind of DBD excitations
Source, DBD-AES systems and its determination method.The excitaton source of the system uses style of opening DBD plasmas and Liquid sample introduction
Mode, it is ensured that while DBD plasma stabilities are discharged, be introduced directly into fluid sample, generate sensitive emission spectrum
Signal carries out quantitative analysis to determinand；The system sample introduction flow velocity is fast, detection frequency is high, substantially increases analysis efficiency, saves
Detection time.
One of technical scheme of the present invention is a kind of DBD excitaton sources, be open plasma exciatiaon source, by electrode one,
Electrode two and power supply system composition, two electrodes are connected respectively to the two poles of the earth of power supply system by conducting wire；
Electrode one is the conductive metal sheet being attached on quartz plate；
Electrode two is made of atomizer and the conductive metal paillon being wrapped on atomizer exit side wall；
Atomizer exit vertically electrode one, region of discharge is formed between electrode one and the atomizer exit of electrode two
Domain；
Wherein, a conducting wire is connected to the conductive metal on piece of electrode one, and another conducting wire is wrapped in the conduction of electrode two
Outside metal foil；
The atomizer is the casing being made of inner and outer tubes, and inner and outer pipes are not connected to；Inner tube is equipped with sample inlet and sample
Product export, and outer tube is equipped with carrier gas inlet and carrier gas exports, and sample export and carrier gas outlet port are concentric, and carrier gas is exported in carrier gas
The solution atomization exported at sample export is dispersed into liquid little particle；
The metal of the conductive metal sheet of electrode one is tungsten, platinum etc.；
The metal of the conductive metal paillon of electrode two is aluminium, gold, tungsten, platinum etc.；
Preferably, power supply system is 3~4kV of voltage, the AC power of 35~45kHz of frequency；
Atomizer is quartz material；
Outer wall thickness is 0.1~0.4mm at atomizer exit；Sample export internal diameter be 0.3~0.6mm, carrier gas outlet in
Diameter is 0.6~0.9mm；
Metal foil thickness is 0.01~0.5mm；
Atomizer exit to the distance between electrode one be 0.2~1000mm；
Preferably, other a piece of quartz plate is set on the quartz plate of electrode one as side quartz plate, the angle of the two is
45~90 °, the purpose of setting side quartz plate is the water mist pollution lens generated when sample being avoided to be excited, influences the sight of detector
Examine effect.
When atomizer have carrier gas (helium, argon gas etc.) by when, electrode both ends apply power supply system provide 3~4kV
High-frequency ac voltage has the stable dielectric barrier discharge plasma formed by carrier gas to generate in region of discharge at this time；And
And carrier gas at the atomizer exit i.e. in region of discharge by fluid sample aerosol dispersion at liquid little particle；It therefore, can be by Jie
Matter barrier discharge plasma excites the liquid little particle of dispersion as excitaton source, generates the emission spectrum signal of determinand.
The two of technical scheme of the present invention are a kind of DBD-AES systems, by above-mentioned DBD excitaton sources, sequential injection system
System, carrier gas bottle and CCD (Charge-Coupled Device, charge-coupled device) detector composition；
Wherein, sequential injection system is connect with the sample inlet of DBD excitaton source atomizers, for fluid sample to be inputted mist
Change device；
Carrier gas bottle is connect with the carrier gas inlet of DBD excitaton source atomizers, for carrier gas to be inputted atomizer；
CCD is located at the side in electrode discharge region, the emission spectrum signal for observing determinand；Preferably, CCD is carried
The storage system or CCD that can be read are connected with electronic computer；
Flow rate of carrier gas of the above system in detectable range is 0~800mL/min；Flow rate of liquid is 0~120 μ L/s；
Sample frequency is 0~80 time/h；
The measurable metallic element of above system is Cd, Zn, Hg, Pb etc..
The three of technical scheme of the present invention are using the analyzing detecting method of above-mentioned DBD-AES systems, including to walk as follows
Suddenly：
1) carrier gas is opened to flow speed stability, carrier gas is made persistently to be sprayed by atomizer exit, opens power supply system, and DBD swashs
It rises in the sustainable generation DBD plasmas of region of discharge；
2) start sample introduction after plasma stability excitation；Fluid sample is passed through atomizer by sequential injection system,
By carrier gas aerosol dispersion at liquid little particle at atomizer exit, while liquid little particle enters DBD plasma exciatiaons
By DBD plasma exciatiaons in the region of discharge in source, characteristic emission spectrum is generated；
3) it utilizes CCD to capture characteristic emission spectrum, and records data；
4) after the completion of testing, cleaning sequence injecting systems and atomizer are ready for sample introduction next time；
In the above method, flow rate of carrier gas is 1~800mL/min；Flow rate of liquid is 1~120 μ L/s；Sample frequency be 0~
80 times/h.
Compared with prior art, advantage of the invention is that：
1, the present invention is opening DBD emission spectrum excitaton source, it is ensured that DBD plasmas are stable in the air to be put
Electricity solves the problem of residual and repeatedly excitation of the general closed excitaton source sample in excitation chamber, no quantitative analysis；
2, fluid sample can be directly introduced into excitaton source by this system, need not carry out steam to element-specific,
It can indistinguishably realize that the analysis of multiple element measures；
3, sample flow rate of the invention is very fast, detection frequency is high, substantially increases analysis efficiency, saves detection time.
Description of the drawings
Fig. 1, one structural schematic diagram of electrode of the present invention；
Fig. 2, two structural schematic diagram of electrode of the present invention；
Fig. 3, atomizer exit schematic diagram of the present invention；
Fig. 4, a kind of DBD-AES system schematics of the present invention；
The pictorial diagram of Fig. 5, DBD excitaton sources of the present invention；
Wherein, 1, electrode one, 2, electrode two, 3, power supply system, 4, quartz plate, 5, conductive metal sheet, 6, atomizer, 7, gold
Belong to paillon, 8, conducting wire, 9, carrier gas inlet, 10, sample inlet, 11, carrier gas outlet, 12, sample export, 13, atomizer exit,
14, side quartz plate, 15, sequential injection system, 16, carrier gas bottle, 17, CCD detector, 18, electrode discharge region.
Specific implementation mode
CCD type number is the AvaSpec-ULS2048-4-USB2 of AVANTES companies；
Sequential injection system is purchased from FIAlab Instruments Inc.；
Carrier gas is helium.
Embodiment 1
A kind of DBD excitaton sources are open plasma exciatiaon source, by electrode 1, electrode as shown in Fig. 1,2,3 and 4
22 and power supply system 3 form, electrode 1 is the conductive metal sheet (leaf) 5 being attached on quartz plate 4, and electrode 22 is by atomizer 6
It is formed with the metal foil (aluminium foil) 7 being wrapped on 13 side wall of atomizer exit, gold foil may be tungsten, platinum foil piece, mist
Change vertically electrode 1 of device outlet 13, forms region of discharge 18, two electrodes between electrode 1 and atomizer exit 13
The two poles of the earth of power supply system 3 are connected respectively to by conducting wire 8；
Wherein, a conducting wire 8 is connected on the platinized platinum 5 of electrode 1, and another conducting wire 8 is wrapped in the metal foil of electrode 22
Outside piece (aluminium foil) 7；
The atomizer 6 is the casing being made of inner and outer tubes, and inner and outer pipes are not connected to；Inner tube is equipped with 10 He of sample inlet
Sample export 12, outer tube is equipped with carrier gas inlet 9 and carrier gas outlet 11, and sample export 12 and 11 positions of carrier gas outlet are concentric, carry
The solution atomization exported at sample export 12 is dispersed into liquid little particle by gas in carrier gas outlet 11；
Atomizer 6 is quartz material；13 outer wall thickness of atomizer exit is 0.2mm；Sample export internal diameter is 0.4mm, is carried
Gas exit inside diameter is 0.7mm；7 thickness of aluminium foil is 0.01~0.5mm；
Power supply system 3 is 3~4kV of voltage, the AC power of 35~45kHz of frequency；
It is 0.2mm that atomizer exit 13, which arrives the distance between electrode one,；
In addition a piece of quartz plate is placed on the quartz plate 4 of electrode 1, and, as side quartz plate 14, the angle α of the two is 45
~90 °, the purpose of setting side quartz plate 14 is the water mist pollution lens generated when sample being avoided to be excited, influences the sight of detector
Examine effect.
When atomizer 6 have carrier gas (helium, argon gas etc.) by when, electrode both ends apply 3~4kV high-frequency alternating current
Pressure has stable dielectric barrier discharge plasma to generate in electrode discharge region 18 at this time；And carrier gas can go out in atomizer
At mouthfuls 13 i.e. electrode discharge region 18 by fluid sample aerosol dispersion at liquid little particle；It therefore, can be by the dielectric barrier discharge
Plasma excites the liquid little particle of dispersion as excitaton source, generates the emission spectrum signal of determinand.
Embodiment 2
A kind of DBD excitaton sources, structure is with embodiment 1, and difference lies in the conductive metal sheet 5 of electrode 1 is platinized platinum；Electrode
22 metal foils 7 being wrapped on atomizer exit side wall are gold foil；
6 outer wall thickness of atomizer is 0.1~0.4mm；12 internal diameter of sample export is 0.3~0.6mm, and carrier gas exports 11 internal diameters
For 0.6~0.9mm；7 thickness of gold foil is 0.01~0.5mm；
It is 0.2~1000mm that atomizer exit 13, which arrives the distance between electrode one,.
Embodiment 3
A kind of DBD-AES systems, as shown in Figure 4 and Figure 5, by the DBD excitaton sources in embodiment 1, sequential injection system 15,
Carrier gas bottle 16 and CCD (Charge-Coupled Device, charge-coupled device) detector 17 composition；
Wherein, sequential injection system 15 is connect with the sample inlet 10 of DBD excitaton sources atomizer 6, is used for fluid sample
Input atomizer 6；
Carrier gas bottle 16 is connect with carrier gas inlet 11, for carrier gas to be inputted atomizer 6；
CCD detector 17 is located at the side in electrode discharge region 18, the emission spectrum signal for observing determinand；
Flow rate of carrier gas of the above system in detectable range is 0~800mL/min；Flow rate of liquid is 0~120 μ L/s；
Sample frequency is 0~80 time/h.
Embodiment 4
Using the analyzing detecting method of the DBD-AES systems of embodiment 3, include the following steps：
1) carrier gas is opened, flow rate of carrier gas is 1~800mL/min, until flow speed stability, makes carrier gas be continued by atomizer exit
It sprays, connects circuit, the high-frequency ac voltage for 3~4kV that load is provided by power supply system at electrode both ends, DBD excitaton sources can
Persistently generate DBD plasmas；
2) start sample introduction after plasma stability excitation, fluid sample be passed through by atomizer by sequential injection system,
The flow velocity that sample passes through atomizer is 1~120 μ L/s, 1~100 μ L of sample size；Fluid sample is through carrier gas at atomizer exit
Aerosol dispersion enters in region of discharge at liquid little particle by DBD plasma exciatiaons, generates characteristic emission spectrum；
3) CCD is utilized, captures characteristic emission spectrum, and record data, sample frequency is 0~80 time/h；
4) after the completion of testing, cleaning sequence injecting systems and atomizer are ready for sample introduction next time.
Embodiment 5
Using the content of Cd in the DBD-AES system measurement samples of embodiment 3, include the following steps：
1) open carrier gas be 500mL/min to flow speed stability, so that carrier gas is persistently sprayed by atomizer exit, connection electricity
Road, the high-frequency ac voltage for the 4kV that load power supply system provides at electrode both ends, the sustainable generation DBD plasmas of DBD excitaton sources
Body；
2) it prepares and contains Cd2+The standard solution of a concentration of 5~1000 μ g/L starts after plasma exciatiaon is stablized and generated
Fluid sample is passed through atomizer by sample introduction by sequential injection system, and the flow velocity that sample passes through atomizer is 3 μ L/s, sample size
50 μ L through carrier gas aerosol dispersion at liquid little particle at atomizer exit, while entering the electric discharge of DBD plasma exciatiaons source
By DBD plasma exciatiaons in region, characteristic emission spectrum is generated；
3) CCD is utilized, captures characteristic emission spectrum, and record data；
4) after the completion of testing, cleaning sequence injecting systems and atomizer are ready for sample introduction next time.
Finally obtain Cd2+The standard regression curve of the solution of a concentration of 5~1000 μ g/L.
The Cd contents in seaweed, analog environmental water, city garbage burning ash are successfully determined by this method, it was demonstrated that
The reliability of this method also illustrates that this method can be applied in actual sample, meets general analysis and measures needs.
Embodiment 6
Using the content of Zn in the DBD-AES system measurement samples of embodiment 3, include the following steps：
1) open carrier gas be 600mL/min to flow speed stability, so that carrier gas is persistently sprayed by atomizer exit, connection electricity
Road, the 3kV high-frequency ac voltages that load power supply system provides at electrode both ends, the sustainable generation DBD plasmas of DBD excitaton sources
Body；
2) it prepares and contains Zn2+The standard solution of a concentration of 5~1000 μ g/L starts after plasma exciatiaon is stablized and generated
Fluid sample is passed through atomizer by sample introduction by sequential injection system, and the flow velocity that sample passes through atomizer is 6 μ L/s, sample size
100 μ L through carrier gas aerosol dispersion at liquid little particle at atomizer exit, while entering DBD plasma exciatiaons source and putting
By DBD plasma exciatiaons in electric region, characteristic emission spectrum is generated；
3) CCD is utilized, captures characteristic emission spectrum, and record data；
4) after the completion of testing, cleaning sequence injecting systems and atomizer are ready for sample introduction next time.
Finally measure Zn2+Detect 20~1000 μ g/L of the range of linearity.
Embodiment 7
Using the content of Hg in the DBD-AES system measurement samples of embodiment 3, include the following steps：
1) open carrier gas be 400mL/min to flow speed stability, so that carrier gas is persistently sprayed by atomizer exit, connection electricity
Road, the 3kV high-frequency ac voltages that load power supply system provides at electrode both ends, the sustainable generation DBD plasmas of DBD excitaton sources
Body；
2) it prepares and contains Hg2+The standard solution of a concentration of 5~1000 μ g/L starts after plasma exciatiaon is stablized and generated
Fluid sample is passed through atomizer by sample introduction by sequential injection system, and the flow velocity that sample passes through atomizer is 2 μ L/s, sample size
30 μ L through carrier gas aerosol dispersion at liquid little particle at atomizer exit, while entering the electric discharge of DBD plasma exciatiaons source
By DBD plasma exciatiaons in region, characteristic emission spectrum is generated；
3) CCD is utilized, captures characteristic emission spectrum, and record data；
4) after the completion of testing, cleaning sequence injecting systems and atomizer are ready for sample introduction next time.
Finally measure Hg2+Detect 20~1000 μ g/L of the range of linearity.
Claims (7)
1. a kind of DBD excitaton sources, which is characterized in that be open plasma exciatiaon source, be by electrode one, electrode two and power supply
System composition, two electrodes are connected respectively to the two poles of the earth of power supply system by conducting wire；
Wherein, the electrode one is the conductive metal sheet being attached on quartz plate；The electrode two is by atomizer and is wrapped in atomization
Conductive metal paillon composition in device exit side wall；
The atomizer exit vertically electrode one, region of discharge is formed between electrode one and the atomizer exit of electrode two
Domain；
Atomizer exit to the distance between electrode one be 0.2~1000mm；
The atomizer is the casing being made of inner and outer tubes, and inner and outer pipes are not connected to；Inner tube is equipped with sample inlet and sample goes out
Mouthful, outer tube is equipped with carrier gas inlet and carrier gas exports, and sample export and carrier gas outlet port are concentric；
Outer wall thickness is 0.1~0.4mm at atomizer exit；Sample export internal diameter is 0.3~0.6mm, and carrier gas exit inside diameter is
0.6~0.9mm；
Power supply system is 3~4kV of voltage, the AC power of 35~45kHz of frequency.
2. a kind of DBD excitaton sources according to claim 1, which is characterized in that one, the conducting wire is connected to electrode one
Conductive metal on piece, outside another conductive metal paillon for being wrapped in electrode two.
3. a kind of DBD excitaton sources according to claim 1, which is characterized in that the gold of the conductive metal sheet of the electrode one
Belong to is tungsten, platinum；The metal of the conductive metal paillon of the electrode two is aluminium, gold, tungsten, platinum.
4. a kind of DBD excitaton sources according to claim 1, which is characterized in that be arranged on the quartz plate of the electrode one
In addition for a piece of quartz plate as side quartz plate, the angle of the two is 45~90 °.
5. a kind of DBD-AES systems, which is characterized in that by DBD excitaton sources described in claim 1, sequential injection system, carrier gas
Bottle and CCD detector composition；
Wherein, sequential injection system is connect with the sample inlet of DBD excitaton source atomizers；
Carrier gas bottle is connect with the carrier gas inlet of DBD excitaton source atomizers；
CCD is located at the side in electrode discharge region.
6. a kind of analyzing detecting method using the DBD-AES systems described in claim 5, which is characterized in that including walking as follows
Suddenly：
1) carrier gas is opened to flow speed stability, so that carrier gas is persistently sprayed by atomizer exit, is opened power supply system, DBD excitaton sources
In the sustainable generation DBD plasmas of region of discharge；
2) start sample introduction after plasma stability excitation；Fluid sample is passed through atomizer by sequential injection system, in mist
Change device exit by carrier gas aerosol dispersion into liquid little particle, while liquid little particle enters DBD plasma exciatiaons source
By DBD plasma exciatiaons in region of discharge, characteristic emission spectrum is generated；
3) it utilizes CCD to capture characteristic emission spectrum, and records data；
4) after the completion of testing, cleaning sequence injecting systems and atomizer are ready for sample introduction next time.
7. a kind of analyzing detecting method of DBD-AES systems according to claim 6, which is characterized in that flow rate of carrier gas 1
~800mL/min；Flow rate of liquid is 1~120 μ L/s；Sample frequency is 0~80 time/h.
Priority Applications (1)
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| CN106872417B (en) * | 2017-03-06 | 2019-10-11 | 大连理工大学 | Utilize the experimental provision and method of SDBD and emission spectrum detection OH concentration |
| CN107843709A (en) * | 2017-12-19 | 2018-03-27 | 农业部环境保护科研监测所 | Integrated portable heavy metal quick analytic instrument and its analyzing detecting method |
| CN112266161B (en) * | 2020-10-30 | 2023-04-14 | 烽火通信科技股份有限公司 | Vaporization device and method for D4 liquid raw material |
| CN112986219B (en) * | 2021-02-08 | 2022-05-10 | 东北大学 | Electrode sample introduction DBD micro plasma atomic emission spectrum detection system and method |
| CN113720811B (en) * | 2021-08-19 | 2022-12-30 | 中国地质大学（武汉） | Micro-plasma excitation source and excitation method based on ultrasonic atomization sampling |
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| CN102353799A (en) * | 2011-07-25 | 2012-02-15 | 中国地质大学（武汉） | Method of evaporating sample injecting inducted by dielectric barrier discharge microplasma |
| CN102445445B (en) * | 2011-10-08 | 2013-08-21 | 中国地质大学（武汉） | Method and device for detecting metal ions by adopting liquid dielectric barrier discharge (DBD) emission spectrum |
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