CN1174991A - Microwave plasma torch atomic emission spectrometer - Google Patents
Microwave plasma torch atomic emission spectrometer Download PDFInfo
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- CN1174991A CN1174991A CN 97111970 CN97111970A CN1174991A CN 1174991 A CN1174991 A CN 1174991A CN 97111970 CN97111970 CN 97111970 CN 97111970 A CN97111970 A CN 97111970A CN 1174991 A CN1174991 A CN 1174991A
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Abstract
The present invention belongs to an atomic emission spectrograph for detecting elemental components in sample. Said spectrograph uses oxygen screened microwave plasma torch as light source. Said light source is formed from inner tube introducing carrier and sample, intermediate tube introducing working gas and outer tube introducing screening gas. A tuning screw bolt is coaxially installed on the bottom of the outer tube, and on the outer tube wall over the end face of the tuning screw bolt there is coaxially installed on the end face of the tuning screw bolt there is a tangential gas-introducing channel. Said invented spectrograph can betermine all elements included in periodic table of chemical elements with remarkable price performance.
Description
The present invention is the spectrometer of elemental composition in the test sample, particularly makes the Atomic Emission Spectrometer AES of light source with microwave plasma.
Successful and the most the most frequently used Atomic Emission Spectrometer AES is the Atomic Emission Spectrometer AES that inductively coupled plasma is made light source at present.Its structure mainly includes inductance coupling plasma light source, solution sampling system, beam splitting system and spectral signal detection system.Inductively coupled plasma has good analytical performance, but significant limitation is also arranged.This mainly shows two aspects: (1) is difficult to form helium plasma, thereby surveys nonmetalloid such as bad halogen, and this is a very big defective as chromatographic atomic emissions detecting device the time; (2) cost and standing charges are too big, and the gas consumption amount is more than 15L/min, and power consumption is more than 800W.Therefore, inductively coupled plasma atomic emission spectrometer also has been subjected to very big restriction in actual applications.The microwave plasma physical efficiency forms helium plasma under lower power and plasma gas flow amount, thereby can remedy above-mentioned two defectives of inductively coupled plasma well, but traditional microwave plasma has the low significant drawback of sample holding capacity again.This shortcoming has become the traditional microwave plasma to fail so far by commercial most important reason successfully.
The objective of the invention is to overcome the deficiencies in the prior art, the microwave plasma light source that design makes new advances, improved the ability to bear of microwave plasma greatly, spectrometer has been reached under lower-wattage and gas flow, can measure to comprise that inductively coupled plasma atomic emission spectrometer surveys nearly all element in the periodic table of bad nonmetalloids such as halogen sample.
Microwave plasma torch atomic emission spectrometer of the present invention by the solution sampling system, contains parts such as sample, carrier gas source, atomization system and dissolving system, plasma source, and beam splitting system mainly contains monochromator, and the spectral signal detection system is formed.Said plasma source is the microwave plasma torch light source, and it mainly is made of three coaxial pipes.Coaxial pipe comprises the interior pipe of introducing carrier gas and sample, introduces the middle pipe of work gas and the outer tube of introducing shielding gas.The inner wire of microwave transmission wire terminal and outer conductor respectively with middle pipe and outer tube short circuit.Said solution sampling system contains dissolving system, and dissolving system is made of heating vaporization water condensation unit, back and concentrated sulphuric acid absorptive unit.Solution example transfers to the solution atomization system through the solution transmission system and becomes aqueous aerosol, after removing most solvents, dissolving system enters the effect that plasma is accepted plasma by the interior pipe of microwave plasma torch with carrier gas, the emission of feature that tested element produces in plasma is focused to the entrance slit of monochromator through condenser system, and enters beam splitting system thus and by chromatic dispersion.Step motor drive grating rotating in the monochromator, make each spectral line of opening through grating dispersion penetrate the light inlet electric-examination switching device of going forward side by side through exit slit in turn and be converted into electric signal, handle these electric signal by photodetector system again, thereby realize qualitative and quantitative analysis elemental composition in the sample.
Concrete structure is provided by the block scheme of Fig. 1.The solution sampling system comprises carrier gas source 9, and carrier gas can be inert gases such as argon, helium, enters atomization system 15 through carrier gas air pressure and flow control system 12, and sample 13 enters atomization system 15 atomizings through transfusion system 14.Sample after the atomizing and carrier gas are introduced in the interior pipe of microwave plasma torch light source 2 through dissolving system 16, go solubility temperature by temperature control system 17 controls.7 are the work source of the gas, working gas are introduced the middle pipe of microwave plasma torch light source 2 by operating air pressure power and flow control system 10.The 1st, microwave source.3 is condenser system.Beam splitting system is mainly by monochromator 4, and motor scans compositions such as spacing protection system 18, stepper motor 19, stepper motor driver 20.The spectral signal detection system comprises electrooptical device 5, photoelectric commutator drive system 21, I/V converter 6, program control signal amplification and regulating system 22, programmable filter 23 etc.Multi-action computer plug-in card 24 and computer system 25 are used for controlling transfusion system, go the solubility temperature TT﹠C system, the work of driving system of stepping motor and spectral signal detection system, and 26 are additional registering instrument, can.
When microwave plasma torch light source 2 shielded the microwave plasma torch light source of gas for band, instrument system should increase shielding source of the gas 8 and shielding gas air pressure and flow control system 11.Shielding gas is oxygen among the present invention, also can differently according to circumstances make shielding gas with other gases such as nitrogen.
The solution sampling system of microwave plasma torch atomic emission spectrometer of the present invention can adopt various solution atomization methods, comprises pneumatic nebulization, ultrasonic atomizatio and heat atomizing etc.; Can pump into solution with peristaltic pump during pneumatic nebulization, also the lifting force of reliable pneumatic nebulizer self promotes solution; But continuous sample introduction also can intermittently or adopt flow injection mode sample introduction, also can carry out the ON-LINE SEPARATION enrichment; Can manually control sample introduction, also program-controlled sample introduction.Beam splitting system can be a single track sequential scanning monochromator, and its physical construction can adopt sinusoidal structured, also can adopt the turbine worm structure.The electrooptical device 5 of spectral signal detection system is except that available photomultiplier, also can adopt photodiode array and charge transfer device to comprise charge-coupled image sensor and charge injection device, its analog to digital conversion can adopt successive comparison analog to digital conversion mode, also can adopt voltage-frequency analog to digital conversion mode.
The structure of oxygen shield microwaves plasma torch light source 2 of the present invention is as follows: the interior pipe of introducing for carrier gas and sample, the middle pipe of introducing for work gas and be coaxial package successively for the outer tube that shielding gas is introduced.The inner wire of microwave transmission wire terminal and middle pipe short circuit can be to adorn an inner wire short circuit that can slide up and down conductor loops and microwave transmission wire terminal on the outer wall of middle pipe, also can be that middle pipe directly is connected with the inner wire of microwave transmission wire terminal.Have one to contact tuning bolt good and that be connected by accurate thread with the bottom of outer tube respectively between outer tube and the middle pipe with them.On the outer tube wall on the tuning bolt end face, there is a gas to introduce passage.
Concrete structure is provided by Fig. 2.Among Fig. 2,27 is interior pipe, links to each other with dissolving system 16 in the solution sampling system, is used to introduce carrier gas and sample; 28 is middle pipe, links to each other with operating air pressure power and flow control system 10, is used to introduce working gas; 29 is outer tube, links to each other with shielding atmospheric pressure and flow control system 11 by the tangential gas introducing passage of opening on its tube wall 30, is used for introducing shielding gas; The inner wire 31 of microwave transmission wire terminal is by conductor loops 32 and middle pipe 28 short circuits, and conductor loops 32 can slide up and down at middle pipe 28 outer walls; The outer conductor of microwave transmission wire terminal is by fixed cover 33 and outer tube 29 short circuits, and fixed cover 33 is enclosed within outer tube 29 outsides, and short circuit can slide up and down and can be fixed by screw 34 with it.35 is tuning bolt, is installed between outer tube 29 and the middle pipe 28, can introduce between the passage 30 adjustable up and down in outer tube 29 bottoms and tangential gas by the accurate thread of outer tube 29 bottoms.36,37,38 are respectively root, plasma nuclear and the plasma tail flame of plasma.
Oxygen shield microwaves plasma torch light source 2 among the present invention, interior pipe 27 internal diameters can be 0.1-5mm, and thickness of pipe 0.1-2mm can be a metal tube, as copper pipe or stainless-steel tube, can be nonmetallic pipe also, as quartz ampoule.Middle pipe 28 internal diameters can be 6-25mm, and thickness of pipe 1-3mm is a metal tube, as copper pipe, aluminum pipe or stainless-steel tube.Outer tube 29 internal diameters can be 10-100mm, and thickness of pipe 1-8mm also is a metal tube.Tuning bolt 35 upper surfaces can be 30-300mm apart from the distance at torch pipe top, but and free adjustment.The internal diameter that gas is introduced passage 30 can be 1-10mm, can tangentially install with outer tube 29, also can non-tangential installation.
Oxygen shield microwaves plasma torch light source 2 used conductive material surfaces among the present invention all can plate the better metal material of one deck electric conductivity, as silver etc.; Under the outer tube bottom interior surface situation suitable, promptly when no tuning needs, also tuning bolt can be arranged apart from the distance of port; Introduce the vapour lock that passage 30 to middle pipe 28 between the torch pipe top and 29 of outer tubes can be filled an insulation at shielding gas, to increase the linear flow speed that shields gas and to reduce its flow; Can add the effect of a radome in the inboard or the outside of outer tube upper end with disturbance, increase shielding gas shield and the constriction of further minimizing air article on plasma body.Different according to circumstances, remove available O
2Make outside the shielding gas also available N
2Or other gas do shielding gas, even use shielding gas; Except that inert gases such as available Ar and He are working gas and the carrier gas, also available N
2Equimolecular gas is done work gas or carrier gas; Except that available pure gas is done work gas and carrier gas, and combination gass such as available air are done work gas or carrier gas.
During work, microwave power gets final product more than 50W; Carrier gas flux gets final product more than 10mL/min, and working gas and shroud gas flow get final product at 40mL/min with more than the 500mL/min respectively.
Microwave plasma torch of the present invention is compared with traditional microwave plasma, and the solvable ability of aqueous aerosol and molecular components has been improved 2-3 the order of magnitude.Oxygen shield microwaves plasma torch light source of the present invention is compared with traditional microwave plasma torch; owing to form a gas shield layer between plasma and the air; effectively stoped air be involved in and the article on plasma body played the constriction effect, thereby all significantly improved the analytical performance of microwave plasma torch in many aspects.Be embodied in: (1) uses O
2After the shielding, the argon microwave plasma becomes brighter, and is whiter, moves on the plasma nuclear, this means that increase the preheating time of the tested component in best area of observation coverage place, and the plasma profile is more clear, and whole plasma slightly reduces, and lengthening is more stable; (2) change has taken place in plasma parameter, increase about 200K as excitation temperature, rotational temperature increases 200-400K, and plasma parameter all reduces relatively to the dependence of height of observation, optimized analysis is observed the district and is further enlarged, and plasma relatively more approaches local thermodynamic equilibrium; (3) background emission and noise greatly reduce, significant change does not take place in transmitting of tested element, signal-to-background ratio and signal to noise ratio (S/N ratio) are then general obviously to be improved, thereby make detection limit and mensuration precision all obtain considerable improvement to element, as, do to have improved respectively when the light source atomic emission spectrometry is made light source to the detection limit of elements such as Ti and Tl than with the traditional microwave plasma torch nearly 10 times and nearly 20 times with oxygen shield microwaves plasma torch, the mensuration precision of element has then generally been improved 1.1-3.5 doubly, the range of linearity further enlarges, and makes microwave plasma torch do to have bigger potentiality aspect the qualitative and quantitative analysis of elemental composition; (4) oxygen shielding also makes the matrix effect of microwave plasma torch light source obtain to a certain degree alleviation.Oxygen shield microwaves plasma torch atomic emission spectrometer of the present invention is compared with inductively coupled plasma atomic emission spectrometer, and power demand only is about 1/10th of an inductively-coupled plasma spectrometer.The plasma gas flow amount also only is the about 1/10th of inductively-coupled plasma spectrometer, can survey bad nonmetalloids such as halogen by inductance measuring coupled plasma spectrometer, thereby have the remarkable ratio of performance to price.Oxygen shield microwaves plasma torch atomic emission spectrometer of the present invention can be widely used in departments such as industry, agricultural, national defence, scientific research, health care, quality detection, exploration and criminal investigation, the qualitative and quantitative analysis that is used for the actual sample elemental composition also can be for the instruments used for education of each universities and colleges as modern atomic spectroscopic analysis.Microwave plasma torch light source of the present invention is except that the excitation source that can be used as Atomic Emission Spectrometer AES of the present invention, also can be used as chromatogram, comprise the excitation source of atomic emission spectrum detecting device such as gas chromatography, liquid chromatography and supercritical fluid chromatography, the atomizer and the mass spectrometric ionization source of atom of atomic fluorescence spectrometer.In addition, microwave plasma torch also has many non-spectroscopy purposes, as the plasma of its formation being used for the harmless treatment of gaseous contaminant, coal gasification etc.
Description of drawings: Fig. 1 is the structural representation of oxygen shield microwaves plasma torch atomic emission spectrometer of the present invention.Fig. 2 is the structural representation of the oxygen shield microwaves plasma torch among the present invention.
Claims (2)
1. microwave plasma torch atomic emission spectrometer, mainly, contain sample (13), carrier gas source (9), atomization system (15), dissolving system parts such as (16), plasma source by the solution sampling system, beam splitting system mainly contains monochromator (4) and spectral signal detection system and forms; It is characterized in that, said plasma source is microwave plasma torch light source (2), the torch pipe and the microwave source (1) that are made of three coaxial pipes constitute, coaxial pipe comprises the interior pipe (29) of introducing sample and carrier gas, the middle pipe (28) of introducing work gas, and outer tube (29), the inner wire of microwave transmission wire terminal and outer conductor difference short circuit are on middle pipe (28) and outer tube (29) outer wall; Said solution sampling system contains dissolving system, and dissolving system is made of heating vaporization water condensation unit, back and concentrated sulphuric acid absorptive unit.
2. according to the described microwave plasma torch atomic emission spectrometer of claim 1, it is characterized in that, said microwave plasma torch light source (2) is an oxygen shield microwaves plasma torch light source, its structure is to have a tangential gas to introduce passage (30) on outer tube (29) tube wall, inner wire of microwave transmission wire terminal (31) and middle pipe (28) short circuit, the outer conductor of microwave transmission wire terminal is by fixed cover (33) and outer tube (29) short circuit; Between outer tube (29) and middle pipe (28), there is one to contact tuning bolt (35) good and that be connected by accurate thread with the outer tube bottom respectively with them.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 97111970 CN1049286C (en) | 1997-07-08 | 1997-07-08 | Microwave plasma torch atomic emission spectrometer |
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| CN 97111970 CN1049286C (en) | 1997-07-08 | 1997-07-08 | Microwave plasma torch atomic emission spectrometer |
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| CN1174991A true CN1174991A (en) | 1998-03-04 |
| CN1049286C CN1049286C (en) | 2000-02-09 |
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| CN102269707A (en) * | 2011-07-13 | 2011-12-07 | 段忆翔 | Portable element spectrograph for online detection of liquid/gas phase sample |
| CN103269561A (en) * | 2013-05-15 | 2013-08-28 | 浙江大学 | Waveguide direct-feed-type microwave plasma torch device |
| CN103945631A (en) * | 2014-04-06 | 2014-07-23 | 浙江大学 | Improved microwave plasma torch device and application |
| CN104470183A (en) * | 2014-12-04 | 2015-03-25 | 浙江中控研究院有限公司 | Self-tuning magnetron microwave source MPT, self-tuning device and control method |
| CN104602437A (en) * | 2015-01-13 | 2015-05-06 | 吉林大学 | Energy field generating device and control method thereof |
| CN104949962A (en) * | 2014-03-25 | 2015-09-30 | 日本株式会社日立高新技术科学 | ICP atomic emission spectrophotometer |
| CN105148693A (en) * | 2015-08-27 | 2015-12-16 | 浙江中控研究院有限公司 | Method for purifying cooking fume organic matter |
| CN105957793A (en) * | 2016-06-21 | 2016-09-21 | 东华理工大学 | Microwave plasma torch ionization source and ionization mass spectrometry analysis method |
| CN106222711A (en) * | 2016-08-11 | 2016-12-14 | 浙江全世科技有限公司 | The surface treatment method of microwave plasma torch instrument torch pipe |
| CN106323923A (en) * | 2015-07-08 | 2017-01-11 | 北京瑞利分析仪器有限公司 | Two-zone temperature controlled shield type quartz furnace atomizer |
| CN107422025A (en) * | 2017-07-17 | 2017-12-01 | 大连理工大学 | A kind of trace element detection means excited based on plasma surface ripple |
| CN107576524A (en) * | 2017-08-31 | 2018-01-12 | 北京理工大学 | Solid sample microplasma sampler in a kind of open environment |
| CN107991289A (en) * | 2017-11-17 | 2018-05-04 | 浙江全世科技有限公司 | A kind of plasma height adjuster and method |
| CN108387567A (en) * | 2018-05-30 | 2018-08-10 | 吉林大学 | A kind of microwave coupling Plasma-Atomic device for Atomic Fluorescence Spectrometer |
| CN108732234A (en) * | 2017-04-24 | 2018-11-02 | 上海新昇半导体科技有限公司 | Plasma producing apparatus |
| CN110487775A (en) * | 2019-07-25 | 2019-11-22 | 电子科技大学 | A kind of portable spectral analysis device based on plasma |
| CN113906828A (en) * | 2019-04-01 | 2022-01-07 | 珀金埃尔默健康科学加拿大股份有限公司 | Apparatus and method for improving background normality of elemental morphology |
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1997
- 1997-07-08 CN CN 97111970 patent/CN1049286C/en not_active Expired - Lifetime
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| CN102269707A (en) * | 2011-07-13 | 2011-12-07 | 段忆翔 | Portable element spectrograph for online detection of liquid/gas phase sample |
| CN102269707B (en) * | 2011-07-13 | 2013-08-14 | 段忆翔 | Portable element spectrograph for online detection of liquid/gas phase sample |
| CN103269561A (en) * | 2013-05-15 | 2013-08-28 | 浙江大学 | Waveguide direct-feed-type microwave plasma torch device |
| CN104949962A (en) * | 2014-03-25 | 2015-09-30 | 日本株式会社日立高新技术科学 | ICP atomic emission spectrophotometer |
| CN103945631A (en) * | 2014-04-06 | 2014-07-23 | 浙江大学 | Improved microwave plasma torch device and application |
| CN103945631B (en) * | 2014-04-06 | 2016-04-13 | 浙江大学 | A kind of microwave plasma torch device of improvement and application |
| CN104470183A (en) * | 2014-12-04 | 2015-03-25 | 浙江中控研究院有限公司 | Self-tuning magnetron microwave source MPT, self-tuning device and control method |
| CN104470183B (en) * | 2014-12-04 | 2017-11-21 | 浙江全世科技有限公司 | Can self-tuning microwave magnetron source MPT, self-tuning device and control method |
| CN104602437A (en) * | 2015-01-13 | 2015-05-06 | 吉林大学 | Energy field generating device and control method thereof |
| CN104602437B (en) * | 2015-01-13 | 2017-11-14 | 吉林大学 | A kind of energy field generating means and its control method |
| CN106323923B (en) * | 2015-07-08 | 2023-07-14 | 北京北分瑞利分析仪器(集团)有限责任公司 | Double-zone temperature control shielding type quartz furnace atomizer |
| CN106323923A (en) * | 2015-07-08 | 2017-01-11 | 北京瑞利分析仪器有限公司 | Two-zone temperature controlled shield type quartz furnace atomizer |
| CN105148693B (en) * | 2015-08-27 | 2017-11-10 | 浙江中控研究院有限公司 | A kind of oil smoke organic matter purification method |
| CN105148693A (en) * | 2015-08-27 | 2015-12-16 | 浙江中控研究院有限公司 | Method for purifying cooking fume organic matter |
| CN105957793A (en) * | 2016-06-21 | 2016-09-21 | 东华理工大学 | Microwave plasma torch ionization source and ionization mass spectrometry analysis method |
| CN106222711A (en) * | 2016-08-11 | 2016-12-14 | 浙江全世科技有限公司 | The surface treatment method of microwave plasma torch instrument torch pipe |
| CN106222711B (en) * | 2016-08-11 | 2018-05-11 | 浙江全世科技有限公司 | The surface treatment method of microwave plasma torch instrument torch pipe |
| CN108732234A (en) * | 2017-04-24 | 2018-11-02 | 上海新昇半导体科技有限公司 | Plasma producing apparatus |
| CN107422025A (en) * | 2017-07-17 | 2017-12-01 | 大连理工大学 | A kind of trace element detection means excited based on plasma surface ripple |
| CN107422025B (en) * | 2017-07-17 | 2023-08-04 | 大连理工大学 | Trace element detection device based on plasma surface wave excitation |
| CN107576524A (en) * | 2017-08-31 | 2018-01-12 | 北京理工大学 | Solid sample microplasma sampler in a kind of open environment |
| CN107991289A (en) * | 2017-11-17 | 2018-05-04 | 浙江全世科技有限公司 | A kind of plasma height adjuster and method |
| CN108387567A (en) * | 2018-05-30 | 2018-08-10 | 吉林大学 | A kind of microwave coupling Plasma-Atomic device for Atomic Fluorescence Spectrometer |
| CN113906828A (en) * | 2019-04-01 | 2022-01-07 | 珀金埃尔默健康科学加拿大股份有限公司 | Apparatus and method for improving background normality of elemental morphology |
| CN110487775A (en) * | 2019-07-25 | 2019-11-22 | 电子科技大学 | A kind of portable spectral analysis device based on plasma |
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