CN105136749B - A kind of microwave plasma torch atomic emission spectrometer - Google Patents
A kind of microwave plasma torch atomic emission spectrometer Download PDFInfo
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- CN105136749B CN105136749B CN201510514458.3A CN201510514458A CN105136749B CN 105136749 B CN105136749 B CN 105136749B CN 201510514458 A CN201510514458 A CN 201510514458A CN 105136749 B CN105136749 B CN 105136749B
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Abstract
The present invention proposes a kind of microwave plasma torch atomic emission spectrometer, the microwave source system of microwave plasma torch atomic emission spectrometer can produce high-power and continuous-stable microwave, power is adjustable in the range of 0 1500W, microwave output stability is high, by in the high power microwave plasma torch light-source system of powerful microwave coupling to matching, excite the ability of plasma stronger, plasma is not easy by solvent damage, can be by the direct nebulization sampling of sample solution, dissolving device is removed so as to save heating, greatly simplify instrument sampling system, improve the reliability of instrument, caused plasma source is more conducive to Acquisition Detection in spectral detection system, it is more preferable that the spectral analysis data of generation is used for effect during elementary analysis, overall performance is improved.
Description
Technical field
The invention belongs to sample elemental composition detection field, and in particular to one kind is used to form plasma source progress light
The microwave plasma torch atomic emission spectrometer of spectral analysis technology.
Background technology
In Atomic Emission Spectral Analysis field, currently used technology is inductively coupled plasma (ICP) atomic emissions
Spectroscopic methodology, the spectrometer using the technology as core have been widely used, and instrument species and model are also very various, including
Sequential scanning-type, full spectrum direct-reading type etc., overall performance meets scientific research and application demand.But inductively coupled plasma spectrometry
Instrument is expensive, and operating and maintenance cost are higher, is not applicable very much in general institution of higher learning and medium-sized and small enterprises.This
Outside, inductively coupled plasma atomic emission spectrum technology is more difficult to the measure of the nonmetalloids such as halogen.Therefore, find
Not only the advantages of having kept inductively-coupled plasma spectrometer but also its insufficient new type ideal spectrometer is overcome to turn into a focus.
It is expensive that microwave plasma torch spectrometer solves inductively-coupled plasma spectrometer to a certain extent
The problem of.A kind of " microwave plasma torch original is proposed in Patent Office of the People's Republic of China Publication No. CN1174991A application for a patent for invention
Sub- emission spectrometer ", its spectrometer being related to include sampling system, atomization system, dissolving system, plasma source, light splitting
System etc., it is therefore intended that improve ability to bear of the microwave plasma to sample.Patent Office of the People's Republic of China Publication No. CN1474176A
Application for a patent for invention in propose a kind of " simultaneous microwave plasma torch-atomic emission spectrometry ", its spectrometer being related to includes microwave power source system
System, sample introduction system, microwave plasma torch system, computer system etc., it is a kind of full spectrometer, realizes multielement, more
The effect that wavelength detects simultaneously.
But the microwave source system power scope of above two spectrometer belongs to low-power category between 0-300W, with
Multikilowatt ICP is compared, and its plasma exciatiaon ability is still limited, and the plasma under low-power is to the tolerance of aqueous solvent
It is low to incite somebody to action moisture removal contained in aqueous aerosol, conventional sampling system, it is necessary to increase dissolving system in sampling system
After sample atomization heating and gasifying again water cooled solidifying+concentrated sulfuric acid realize go it is molten.Concentrated sulfuric acid operation, inconvenience is changed, glass condenser is easy
Broken, building also must be careful, and air-tightness is bad, can not ensure the long-time stability of sample analysis, and overall performance is relatively low.
The content of the invention
Purpose to be solved by this invention is to provide a kind of microwave plasma torch atomic emission spectrometer, can be operated in
High-power state, plasma excite ability stronger, and sampling system can require no molten and direct after sample atomization
Sample introduction improves overall performance into torch pipe.
To solve the above problems, the present invention proposes a kind of microwave plasma torch atomic emission spectrometer, including：It is high-power
Microwave Plasma Torch Source system, its torch pipe are three pipe coaxial configurations of one end open；Air-path control system, it is controlling
Air inlet of each gas cylinder to high power microwave plasma torch light-source system；Sampling system, the air-path control system control output
Gas of carrier gas sample is also formed by the processing of sampling system sample introduction, sampling system exports sample to HIGH-POWERED MICROWAVES plasma
In the inner tube of body torch light-source system；Microwave source system, it produces the output of adjustable in high-power scope and continuous microwave；Microwave
Transmission system, it is to receive and transmit the microwave, and by microwave coupling to high power microwave plasma torch light-source system；
Spectral detection system, it is capturing the plasma after the plasma exciatiaon of high power microwave plasma torch light-source system
Light source, and generate spectral analysis data；And detecting and controlling system, its to each system is controlled and reception processing described in
Spectral analysis data.
According to one embodiment of present invention, the high power microwave plasma torch light-source system includes：Inner tube, in
Pipe, outer tube, coupling pin, coupling ring, reflecting mechanism, spacer ring；Said inner tube, middle pipe, outer coaxial tube are set, and the reflecting mechanism connects
The bottom for being connected on middle pipe and outer tube is arranged in middle pipe outer wall as microwave reflection end, the coupling ring, the coupling pin connection
Microwave coupling is simultaneously played co-axially fixed work by coupling ring between middle pipe and outer tube, the spacer ring is arranged between inner tube and middle pipe
With said inner tube, middle pipe, outer tube and spacer ring are metal material；In the torch pipe of high power microwave plasma torch light-source system
Open end face excites to form plasma.
According to one embodiment of present invention, the reflecting mechanism is configured to untunable mechanism, configures the reflection machine
The position of structure make it that the cavity depth of high power microwave plasma torch light-source system is the odd-multiple of 1/4 microwave wavelength.
According to one embodiment of present invention, in addition to three-dimensional regulating mechanism, it is arranged on the microwave transmission system,
Three-dimensional regulating mechanism is described high-power by the three-dimensional motion of X-axis motor, y-axis motor, Z axis motor control microwave transmission system
Microwave Plasma Torch Source system is rigidly connected with microwave transmission system.
According to one embodiment of present invention, the microwave transmission system includes circulator, three pin adjusters, and waveguide is same
Axle converter；Circulator and the connection of three pin adjusters, three pin adjusters connect with waveguide coaxial converter；Circulator to
The microwave received is adjusted so that microwave is converted to the output of unidirectional loop transmission form；Three pin adjusters export to adjust microwave
The degree of coupling；Torch of the waveguide coaxial converter by L29 joints by microwave coupling to high power microwave plasma torch light-source system
Guan Zhong.
According to one embodiment of present invention, the microwave source system is the adjustable high power solid state microwave of continuous wave power
Source system, the microwave transmission system are a L29 joints, the microwave delivery outlet of microwave source system by L29 joints with it is high-power
The torch pipe of Microwave Plasma Torch Source system is of coupled connections.
According to one embodiment of present invention, the microwave source system includes high power CW ripple magnetron and linear electricity
Source, the linear power supply to high power CW ripple magnetron carry out high power power supply；Change high power CW ripple magnetron
To adjust the output microwave, high power CW ripple magnetron is coupled interior magnetic field intensity by waveguide and microwave transmission system.
According to one embodiment of present invention, the sampling system includes atomizer, fog chamber, peristaltic pump；Atomizer and mist
Room is tightly connected, and fog chamber lower end is connected with peristaltic pump, and the gas access of the atomizer inputs the gas of carrier gas, sample solution
In atomizer atomization and mixed carrier gas gas formed sample aerosol enter fog chamber in, sample aerosol by fog chamber above
Ground enters in inner tube.
According to one embodiment of present invention, the sampling system includes atomizer, fog chamber, heating tube, Nafion dryings
Pipe, warm bath case；Atomizer and fog chamber are tightly connected, and the gas access of the atomizer inputs the gas of carrier gas, sample solution
Atomization and mixed carrier gas gas form sample aerosol and entered in fog chamber in atomizer, and sample aerosol above fog chamber by going out
Mouth, which is entered in heating tube, to be heated, and the sample aerosol after heating enters in inner tube after being dried via Nafion drying tubes, described
Heating tube and Nafion drying tubes, which are arranged in warm bath case, keeps constant temperature working condition.
According to one embodiment of present invention, the sampling system include the first triple valve, the second triple valve, sample cell,
Reaction tank, pond is dried, for the entrance of first triple valve to be passed through gas of carrier gas, the first outlet of the first triple valve connects institute
State the first entrance of the second triple valve, the second outlet of the first triple valve is connected to the gas access of reaction tank, sample cell to
There is provided sample solution to be reacted into reaction tank to form sample aerosol, the delivery outlet output sample aerosol of reaction tank is extremely
Dry in pond and dry, dry pond delivery outlet and export dried sample gas to the second entrance of the second triple valve, the second triple valve
Outlet be connected to inner tube.
According to one embodiment of present invention, the spectral detection system include convex lens, slit, collimating mirror, prism, in
Echelon, focus lamp, CCD or ICCD detectors；Plasma source enters slit by convex lens, and successively by collimation
It is transmitted to after mirror, prism, echelle grating, focus lamp on CCD or ICCD detectors, CCD or ICCD detectors carry out all-wave model
Opto-electronic conversion in enclosing generates the spectral analysis data.
According to one embodiment of present invention, the spectral detection system includes convex lens, slit, collimating mirror, grating, gathers
Jiao Jing, photomultiplier or photodiode array or charge coupling device or CID；Plasma source is passed through
Convex lens enter slit, and are transmitted to photomultiplier or photodiode array after collimating mirror, grating, focus lamp successively
Or charge coupling device or CID, photomultiplier or photodiode array or charge coupling device or electric charge note
Enter device and scan the progress opto-electronic conversion generation spectral analysis data in order.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art：Microwave plasma torch
The microwave source system of Atomic Emission Spectrometer AES can produce high-power and continuous-stable microwave, and power can in the range of 0-1500W
Adjust, microwave source system output stability is high, the high power microwave plasma torch light source by powerful microwave coupling to matching
In system, excite the ability of plasma stronger, plasma is not easy by solvent damage, sample solution can be directly atomized into
Sample, dissolving device is removed so as to save heating, greatly simplifies instrument sampling system, improve the reliability of instrument, caused grade from
Daughter light source is more conducive to Acquisition Detection in spectral detection system, and the spectral analysis data of generation is used for during elementary analysis effect more
Good, overall performance is improved.
High-power lower microwave plasma torch atomic emission spectrometer overall performance is improved, micro- compared under low-power
For ripple plasma torch atomic emission spectrometer, the detection of halogen has clear improvement.
Three-dimensional motion is carried out using three-dimensional regulating mechanism control microwave transmission system, can be to microwave coupling to high-power micro-
The spatial coordinate location (X, Y, Z) of ripple plasma torch light-source system is adjusted, and divides beneficial to plasma space energy is carried out
Cloth is measured, and possibility is provided for Optimal Experimental condition and research plasma substrate physical chemistry characteristic.
Brief description of the drawings
Fig. 1 is the structured flowchart of the microwave plasma torch atomic emission spectrometer of one embodiment of the invention；
Fig. 2 is the structural representation of the air-path control system of one embodiment of the invention；
Fig. 3 is the structured flowchart of the high power microwave plasma torch light-source system of one embodiment of the invention；
Fig. 4 is the structured flowchart of the three-dimensional regulating mechanism of one embodiment of the invention；
Fig. 5 is the structured flowchart of the microwave transmission system of one embodiment of the invention；
Fig. 6 is the structured flowchart of the sampling system of one embodiment of the invention；
Fig. 7 is the structured flowchart of the sampling system of another embodiment of the present invention；
Fig. 8 is the structured flowchart of the sampling system of another embodiment of the invention；
Fig. 9 is the structured flowchart of the full spectrum direct-reading type spectral detection system of one embodiment of the invention；
Figure 10 is the structured flowchart of the sequential scanning-type spectral detection system of one embodiment of the invention.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below in conjunction with the accompanying drawings to the present invention
Embodiment be described in detail.
Many details are elaborated in the following description in order to fully understand the present invention.But the present invention can be with
Much it is different from other manner described here to implement, those skilled in the art can be in the situation without prejudice to intension of the present invention
Under do similar popularization, therefore the present invention is not limited to the specific embodiments disclosed below.
Referring to Fig. 1, microwave plasma torch atomic emission spectrometer of the invention includes high power microwave plasma torch
Light-source system 1, air-path control system 7, sampling system 5, microwave source system 2, microwave transmission system 3, spectral detection system 8, inspection
Survey control system 6.
The power for the microwave source system that the microwave plasma torch atomic emission spectrometer of the present invention uses can be in 300W
More than, microwave source system output stability is high, and output offset error is small, ensure that high power microwave plasma torch light-source system
The stability of 1 work.
Wherein, the torch pipe of high power microwave plasma torch light-source system 1 is three pipe coaxial configurations of one end open, and this is big
Power microwave plasma torch light-source system 1 can be coupled to receive the microwave of high-power state, torch pipe middle pipe and outer tube it
Between form electromagnetic field standing wave, in torch pipe openend, electric field most excites by force plasma, and plasma exciatiaon ability is stronger.Gas circuit control
System 7 processed is for controlling each gas cylinder to include carrier gas bottle 10 to the air inlet of high power microwave plasma torch light-source system 1, each gas cylinder
(built-in gas of carrier gas), work gas cylinder 11 (built-in maintenance gas) and shielding gas oxygen cylinder 12 (built-in shroud gas), in a reality
Apply in example, when high power microwave plasma torch light-source system 1 can not need shroud gas, the gas oxygen that deshields can also be saved
Bottle 12, each gas cylinder connects for example, by the pipeline such as metal tube or PU (Polyurethane) pipe and air-path control system 7, air-path control system
7 receive the operational orders control gas flow rate of detecting and controlling systems 6, air-path control system 7 export after through metal tube or PU pipes
Gas of carrier gas, plasma gas, shroud gas are passed through the inner tube, the tube and the outer tube of torch pipe by transmission respectively.Wherein gas circuit controls
System 7 control output gas of carrier gas also by the processing of sampling system 5 formed sample after enter or be sent into HIGH-POWERED MICROWAVES etc. from
In the inner tube of daughter torch light-source system 1.Microwave source system 2 provides adjustable in high-power scope and continuous microwave.Microwave passes
Defeated system 3 receives and changes microwave so that the coupling that microwave and torch pipe more match, by the microwave coupling after conversion to high-power micro-
Ripple plasma torch light-source system 1, after microwave coupling to torch pipe, plasma is excited in torch pipe open end, forms plasma
Light source.Spectral detection system 4 captures the plasma after the plasma exciatiaon of high power microwave plasma torch light-source system 1
Light source, and generate spectral analysis data.Detecting and controlling system 6 plays control action in spectrometer, controls the normal of each system
Work, detecting and controlling system 6 also receive and handle the spectral analysis data of the output of spectral detection system 4.
Referring to Fig. 2, air-path control system 7 include carrier gas mass flow controller 29, maintain gas mass flow controller 30,
Oxygen shielding gas mass flow controller 31, receives the control signal from control system 9, each road gas flow is controlled
System, is controlled to gas flow using gas motion fuel factor, is connected using adapter with each pipeline, it is preferred that each pipeline
Using external diameter 6mm metal or PU tracheaes, when entering sample, carrier gas mass flow controller 29 connects with sampling system 5, carrier gas
Mass flow controller 29 is handled after exporting gas of carrier gas by sampling system 5, and carrier gas is provided for sample solution sample introduction.
In one embodiment, detecting and controlling system 6 includes control system 9 and host computer 14, and host computer 14 facilitates user
Using operation software control spectrometer, control system 9 can by the transmission lines such as netting twine and the communication receiving/transmission operational order of host computer 14,
It is connected by connection with each system, realizes transmitting-receiving command function control execution unit, control system 9 exports operational order to gas
So as to control gas flow rate, electric signal (spectral analysis data) of the spectral detection system after opto-electronic conversion passes path control system 7
Data processing is carried out to host computer 14, shows and generates spectrogram, completes element measurement.
Referring to Fig. 3, in one embodiment, high power microwave plasma torch light-source system 1 includes inner tube 15, middle pipe
16th, outer tube 17, coupling pin 18, coupling ring 19, reflecting mechanism 20, spacer ring 24.Inner tube 15, middle pipe 16, outer tube 17 coaxially assemble, interior
Pipe 15 is passed through carrier gas, and middle pipe 16 is passed through maintenance gas, and outer tube 17 is passed through shielding gas, and reflecting mechanism 20 is connected to middle pipe 16 and outer tube 17
Bottom as microwave reflection end, coupling ring 19 is fitted tightly on the outer wall of middle pipe 16, coupling pin 18 connect coupling ring 19 simultaneously will
For microwave coupling between middle pipe 16 and outer tube 17, microwave frequency is, for example, 2.45GHz, spacer ring be arranged on inner tube 15 and middle pipe 16 it
Between serve co-axially fixed, also act as the effect of the reflection end face of microwave between middle pipe 16 and inner tube 15, inner tube 15, middle pipe in addition
16th, outer tube 17 and spacer ring 24 are metal material, the interior electromagnetic field stationary field formed with double resonance of torch pipe of the structure, are applied to
High-power and low power occasion, in the present embodiment, the one of the torch pipe opening of high power microwave plasma torch light-source system 1
End excites plasma, and plasma 28 excites ability stronger, and plasma 28 is made up of flame root 21, flame core 22, flame tail 23；Flame
Core 22 is generally optimized analysis area, and sample aerosol is launched respectively in flame root 21 through gasifying to be stimulated with flame core 22 after atomization
The characteristic emission of element.
In one embodiment, inner tube 15 can also be used as quartz material, middle pipe 16 and outer tube 17 are metal material
High power microwave plasma torch light-source system 1.The high power microwave plasma torch light-source system 1 of the present embodiment is to realize torch
Pipe HIGH-POWERED MICROWAVES is coupled so as to obtain a specific embodiment of the stronger arousal function of plasma 28, it will be understood that its
He can realize that the high power microwave plasma torch light-source system of the function can also be used in the present invention, microwave coupling side
Formula is also not limited to couple the mode of pin 18 and coupling ring 19, microwave can also be for example coupled to by waveguide middle pipe and outer tube it
Between.
Preferably, the reflecting mechanism 20 of high power microwave plasma torch light-source system 1 is configured to untunable mechanism, match somebody with somebody
The position for putting reflecting mechanism 20 make it that the cavity depth of high power microwave plasma torch light-source system 1 is 1/4 microwave wavelength
Odd-multiple so that the electric-field intensity in torch pipe opening end face is most strong, realizes most strong plasma exciatiaon, it is ensured that plasma
Work repeatability, and the torch pipe of the structure is more conducive to radiate, and improves plasma operation performance.In addition, to avoid treating test sample
Product sample introduction solution remains the corrosion to torch pipe, improves the service life of torch pipe, unique anti-corrosion treatment is also carried out to torch pipe.
Referring to Fig. 4, in a further embodiment, spectrometer also includes three-dimensional regulating mechanism 13, is arranged on the microwave
In Transmission system 3 and by X-axis motor 37, y-axis motor 38, the adjustment control microwave transmission system 3 of Z axis motor 39 three maintenance and operations
Dynamic, high power microwave plasma torch light-source system 1 is rigidly connected with microwave transmission system 3.Due to the sky of spectral detection system 4
Between position fix, the form of plasma 28 adjusts because sample is different, in order to ensure the optimization of testing conditions, in microwave transmission
The lower section of system 3 installs three-dimensional regulating mechanism 13 additional, is not restricted to lower section certainly, and three-dimensional regulating mechanism 13 is micro- installed in that can cause
Ripple Transmission system 3 carry out three-dimensional motion arbitrary orientation on can, using high power microwave plasma torch light-source system 1 with
The disjunctor of microwave transmission system 3 realizes the three-dimensional regulation of torch pipe.Three-dimensional regulating mechanism 13 can carry out torch pipe space coordinates position
(X, Y, Z) regulation is put, is Optimal Experimental condition and research plasma substrate beneficial to plasma space energy distribution measurement is carried out
Physical chemistry characteristic provides possibility.
In one embodiment, microwave source system 2 includes high power CW ripple magnetron and linear power supply (does not show in figure
Go out), linear power supply is that high power CW ripple magnetron carries out high power power supply, and optionally, linear power supply is Switching Power Supply, is used
Water-cooling apparatus cooling magnetron ensures job stability；The magnetic field intensity changed in high power CW ripple magnetron is defeated to adjust
Go out microwave, high power CW ripple magnetron is coupled by waveguide and microwave transmission system, and microwave power system output power can be in 0-
1500W continuously adjustabes, stability are better than ± 0.5%, and microwave source system is continuous wave output mode, and output microwave frequency is
2.45GHz.The microwave transmission system 3 coupled referring to Fig. 5, and the present embodiment microwave source system 2 can for example include circulator
25th, three pin adjusters 26, waveguide coaxial converter 27.The connected mode of the pin adjuster 26 of circulator 25 and three is preferably firm
Property connection, the connected mode of three pin adjusters 26 and waveguide coaxial converter 27 is preferably to be rigidly connected；Circulator 25 to
Regulation makes the microwave of reception so that microwave is converted to the output of unidirectional loop transmission form；Three pin adjusters 26 are adjusting microwave
Output coupling degree；Waveguide coaxial converter 27 by a kind of L29 (model of radio frequency (RF) coaxial connector) joint by microwave coupling extremely
In the torch pipe of high power microwave plasma torch light-source system 1.Microwave source system produces microwave signal and is passed to microwave transmission system
3, ensure to load (torch pipe) and the impedance matching of microwave transmission system 3, waveguide coaxial converter by adjusting three pin adjusters 26
27 are coupled into microwave signal in torch pipe by L29 joints, are led to after torch pipe internal reflection, the preferably plane fitting that is rigidly connected
Screw perforation is crossed to screw.Certainly, the microwave transmission system shown in Fig. 5 can be used for transmitting other combinable power adjustables
Microwave caused by microwave source system.
In one embodiment, microwave source system 2 is the adjustable high power solid state microwave source system of continuous wave power (in figure
It is not shown), the microwave transmission system 3 is a L29 joints, and the microwave delivery outlet of microwave source system 2 passes through L29 joints and big work(
The torch pipe of rate Microwave Plasma Torch Source system is of coupled connections.Using LDMOS, (horizontal proliferation metal aoxidizes microwave source system 2
Thing semiconductor) high power solid state power device progress multichannel synthesis output microwave, use high-precision directional coupler and wave detector
Ensure the accuracy of output signal, temperature in use feedback compensation circuit ensures the stability of power output, the output of microwave source system
Power can be better than ± 0.5% in 0-1500W continuously adjustabes, stability, and microwave source system is continuous wave output mode, exports microwave
Frequency is 2.45GHz.Solid state microwave sources are coupled to the torch pipe of high power microwave plasma torch light-source system, torch pipe can lead to
Cross L29 joints to be connected with solid state microwave sources system direct-coupling, solve the situation of microwave transmission cable heating in the prior art,
Instrument space is saved, while without water-cooling apparatus, it is more convenient that instrument puts carrying.
Referring to Fig. 6, in one embodiment, sampling system 5 includes mist for a kind of directly nebulization sampling device, sampling system
Change device 41, fog chamber 40, peristaltic pump 43, atomizer 41 is, for example, pneumatic nebulizer or OneNeb atomizers (based on scattered stream skill
A kind of atomizer of art), fog chamber 40 can be the gas access connection gas circuit control of single track or two pass eddy flow, wherein atomizer 41
The gas of carrier gas pipeline of system 7 processed receives gas of carrier gas, and it is atomization and enter fog chamber 40 that sample solution is promoted into atomizer 41
In, atomizer 41 preferably screws to be connected with fog chamber 40 using buckle ensures air-tightness, and the top of fog chamber 40 is for example configured to No. 12 balls
42, No. 12 spherical grounds 42 of shape ground connect with the lower section interface of inner tube 15, and the sample solution aerosol after atomization is passed through into inner tube
15, the lower end of fog chamber 40 is connected by pump line with peristaltic pump 43, and in fog chamber 40, bulky grain sample liquids slide to be formed along wall
Waste liquid is discharged through peristaltic pump 43, and according to OneNeb atomizers, sample solution lifting needs to be driven into atomization by peristaltic pump 43
In device.Compared with background technology, spectrometer of the present invention simplifies sampling system, and pond and heating condensation dress are dried without the concentrated sulfuric acid
Put, improve device portability.
Referring to Fig. 7, in one embodiment, sampling system is done including atomizer 41, fog chamber 40, heating tube 59, Nafion
Dry pipe (drying tube of Nafion material) 60 and warm bath case 61, sample solution are atomized and mixed in atomizer 41
After conjunction gas of carrier gas formation sample aerosol enters fog chamber 40, little particle aerosol rises the outlet of the top of fog chamber 40, passes through glass
Pipeline enters heating tube 59, and heating tube 59 is preferably quartz material, and by heater strip and heat insulation foam temperature control, warm bath case 61 is Nafion
Drying tube 60 provides optimal operating temperature, and heating tube 59 and Nafion drying tubes 60 are positioned over holding constant temperature work in warm bath case 61
Make state, the sample aerosol after heating removes steam therein through Nafion drying tubes 60, and dried sample enters big work(
In rate Microwave Plasma Torch Source system 1.
Referring to Fig. 8, in one embodiment, sampling system 5 is a kind of gas generating unit, including triple valve 32, threeway
Valve 33, sample cell 34, reaction tank 35, dry pond 36, the entrance of triple valve 32 is to be passed through gas of carrier gas, and the first of triple valve 32
The first entrance of outlet connection triple valve 33, the second outlet of triple valve 32 are connected to the gas access of reaction tank 35, sample cell
34 are reacted to form sample aerosol, the delivery outlet output sample of reaction tank 35 to provide sample solution into reaction tank 35
Product aerosol is dry in pond 36 to drying, and the dried sample gas of the dry delivery outlet of pond 36 output to the second of triple valve 33 enters
Mouthful, the outlet of triple valve 33 is connected to inner tube.Sample cell 34 preferably uses glassware, such as can be syringe, for storing
Deposit sample solution；Reaction tank 35 preferably uses glassware, is the reacting environment of sample solution, has a stirring in reaction tank 35
Rod, and heating stirring is carried out in constant-temperature heating magnetic stirring apparatus, sample cell 34 passes through the rubber on the surface of reaction tank 35 by syringe
Glue closure connects, and reaction tank 35 reacts caused gas and is passed through drying tube 36 by glass tube, can be dense in drying tube 36
Sulfuric acid, gas after drying are analyzed by triple valve 33 into inner tube 15.The sampling system of the present embodiment is used in the present invention
Spectrometer in, for detecting halogen (gas form), compared to low-power spectrometer, spectrometer of the invention to halogen examine
Go out to have clear improvement, while as carrier gas and maintain gas can be to gas and Dry aerosol sample using helium or other inert gases
Product do full elemental analysis detection, and a kind of easily analysis detection and platform of tracing to the source are provided for food security and environment measuring.
Referring to Fig. 9, in one embodiment, spectral detection system 3 includes convex lens 52, slit 53, collimating mirror 58, prism
57th, echelle grating 55, focus lamp 56, CCD (Charge-coupled Device, charge coupled cell, a kind of image sensing
Device)/ICCD (reinforcing charge coupling device) detector 54.The flame of optical fiber or light cylinder 8 the alignment plasma of spectral detection system 4
The optimized analysis area of core 22, optical fiber or light cylinder 8 are fixed using optical table or mechanical structure, are excited for gathering tested element
Caused light, that is, plasma source 51 are relative with the fiber entrance of spectral detection system 4, and plasma source 51 is passed through
Convex lens 52 enter slit 53, by collimating mirror 58 beam collimation adjust beam quality, afterwards by prism 57 dispersion again
It is irradiated in echelle grating 55, light beam line focus mirror 56 is transmitted on CCD or ICCD detectors 54 after converging, CCD or ICCD
Detector 54 realizes the opto-electronic conversion in the range of all-wave, and the electric signal (spectral analysis data) after opto-electronic conversion reaches host computer
14 carry out data processing, show and generate spectrogram, complete element measurement, can obtain the full modal data of element to be measured simultaneously, greatly
Reduce testing time and testing cost greatly.
Referring to Figure 10, in one embodiment, spectral detection system 4 includes convex lens 45, slit 46, collimating mirror 50, light
Grid 48, focus lamp 49, photomultiplier or photodiode array or charge coupling device or CID 54.Plasma
Body light source 44 and the face of convex lens 45, enter slit 46 by convex lens 45, light beam is adjusted by the beam collimation of collimating mirror 50
Quality, then be irradiated on grating 48, light beam line focus mirror 49 be transmitted to after converging photomultiplier or photodiode array or
On charge coupling device or CID 47, photomultiplier or photodiode array or charge coupling device or electric charge
Injection device 47 scans in order carries out opto-electronic conversion, and the electric signal (spectral analysis data) after opto-electronic conversion reaches host computer
14 carry out data processing, show and generate spectrogram, complete element measurement.
Although the present invention is disclosed as above with preferred embodiment, it is not for limiting claim, any this area
Technical staff without departing from the spirit and scope of the present invention, can make possible variation and modification, therefore the present invention
Protection domain should be defined by the scope that the claims in the present invention are defined.
Claims (10)
- A kind of 1. microwave plasma torch atomic emission spectrometer, it is characterised in that including：High power microwave plasma torch light Source system, its torch pipe are three pipe coaxial configurations of one end open；Air-path control system, it is controlling each gas cylinder to high-power micro- The air inlet of ripple plasma torch light-source system；Sampling system, the gas of carrier gas of the air-path control system control output also pass through The processing of sampling system sample introduction forms sample, and sampling system exports sample to high power microwave plasma torch light-source system Guan Zhong；Microwave source system, it produces the output of adjustable in high-power scope and continuous microwave；Microwave transmission system, its to Receive and transmit the microwave, and by microwave coupling to high power microwave plasma torch light-source system；Spectral detection system, its To capture the plasma source after the plasma exciatiaon of high power microwave plasma torch light-source system, and generate spectrum Analyze data；And detecting and controlling system, it to each system being controlled and spectral analysis data described in reception processing；The high power microwave plasma torch light-source system includes：Inner tube, middle pipe, outer tube, coupling pin, coupling ring, reflection machine Structure, spacer ring；Said inner tube, middle pipe, outer coaxial tube are set, and the reflecting mechanism is connected to the bottom of middle pipe and outer tube as microwave Reflection end, the coupling ring are arranged in middle pipe outer wall, and the coupling pin connects coupling ring and by microwave coupling to middle pipe and outside Between pipe, the spacer ring, which is arranged between inner tube and middle pipe, plays co-axially fixed, said inner tube, middle pipe, outer tube and spacer ring It is metal material；Excite to form plasma in the end face that the torch pipe of high power microwave plasma torch light-source system opens；The reflecting mechanism is configured to untunable mechanism, and the position for configuring the reflecting mechanism causes HIGH-POWERED MICROWAVES plasma The cavity depth of body torch light-source system is the odd-multiple of 1/4 microwave wavelength.
- 2. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that also including three-dimensional regulation Device, it is arranged on the microwave transmission system, and three-dimensional regulating mechanism is micro- by X-axis motor, y-axis motor, Z axis motor control The three-dimensional motion of ripple Transmission system, the high power microwave plasma torch light-source system are rigidly connected with microwave transmission system.
- 3. microwave plasma torch atomic emission spectrometer as claimed in claim 2, it is characterised in that the microwave transmission system System includes circulator, three pin adjusters, waveguide coaxial converter；Circulator and the connection of three pin adjusters, the regulation of three pins Device connects with waveguide coaxial converter；Circulator is adjusting the microwave of reception so that microwave is converted to unidirectional loop transmission form Output；Three pin adjusters are adjusting microwave output coupling degree；Waveguide coaxial converter by L29 joints by microwave coupling extremely In the torch pipe cavity of high power microwave plasma torch light-source system.
- 4. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that the microwave source system For the adjustable high power solid state microwave source system of continuous wave power, the microwave transmission system is a L29 joints, microwave source system Microwave delivery outlet be of coupled connections by the torch pipe of L29 joints and high power microwave plasma torch light-source system.
- 5. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that the microwave source system Including high power CW ripple magnetron and linear power supply, the linear power supply to high power CW ripple magnetron carry out Gao Gong Rate is powered；Change the magnetic field intensity in high power CW ripple magnetron to adjust the output microwave, high power CW ripple magnetic control Pipe is coupled by waveguide and microwave transmission system.
- 6. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that the sampling system bag Include atomizer, fog chamber, peristaltic pump；Atomizer and fog chamber are tightly connected, and fog chamber lower end is connected with peristaltic pump, the gas of the atomizer Body entrance inputs the gas of carrier gas, and sample solution is atomized in atomizer and mixed carrier gas gas forms sample aerosol and entered In fog chamber, sample aerosol is entered in inner tube by the ground above fog chamber.
- 7. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that the sampling system bag Include atomizer, fog chamber, heating tube, Nafion drying tubes, warm bath case；Atomizer and fog chamber are tightly connected, the gas of the atomizer Body entrance inputs the gas of carrier gas, and sample solution is atomized in atomizer and mixed carrier gas gas forms sample aerosol and entered In fog chamber, sample aerosol is entered in heating tube by outlet above fog chamber and heated, the sample aerosol after heating via Nafion drying tubes enter in inner tube after drying, and the heating tube and Nafion drying tubes are arranged in warm bath case and keep constant temperature work Make state.
- 8. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that the sampling system bag Include the first triple valve, the second triple valve, sample cell, reaction tank, dry pond, the entrance of first triple valve is being passed through carrier gas Gas, the first outlet of the first triple valve connect the first entrance of second triple valve, and the second outlet of the first triple valve connects The gas access of reaction tank is connected to, sample cell is reacted molten to form sample gas to provide sample solution into reaction tank Glue, the delivery outlet of reaction tank export sample aerosol and dried into dry pond, dry pond delivery outlet and export dried sample gas To the second entrance of the second triple valve, the outlet of the second triple valve is connected to inner tube.
- 9. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that the light splitting detection system System includes convex lens, slit, collimating mirror, prism, echelle grating, focus lamp, CCD or ICCD detectors；Plasma source Enter slit by convex lens, and be transmitted to CCD or ICCD after collimating mirror, prism, echelle grating, focus lamp successively and visit Survey on device, the opto-electronic conversion that CCD or ICCD detectors carry out in the range of all-wave generates the spectral analysis data.
- 10. microwave plasma torch atomic emission spectrometer as claimed in claim 1, it is characterised in that the light splitting detection System includes convex lens, slit, collimating mirror, grating, focus lamp, photomultiplier or photodiode array or charge-coupled device Part or CID；Plasma source enters slit by convex lens, and successively by collimating mirror, grating, focus lamp After be transmitted to photomultiplier or photodiode array or charge coupling device or CID, photomultiplier or light Electric diode array or charge coupling device or CID scan in order carries out the opto-electronic conversion generation spectrum point Analyse data.
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