CN1474176A - Mirowave plasma torch full spectometer - Google Patents

Mirowave plasma torch full spectometer Download PDF

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Publication number
CN1474176A
CN1474176A CNA031276725A CN03127672A CN1474176A CN 1474176 A CN1474176 A CN 1474176A CN A031276725 A CNA031276725 A CN A031276725A CN 03127672 A CN03127672 A CN 03127672A CN 1474176 A CN1474176 A CN 1474176A
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China
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plasma torch
grating
array detector
microwave plasma
concave mirror
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CN1230672C (en
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金钦汉
曹彦波
郇延富
冯国栋
费强
姜杰
汪淑华
王兴华
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Jilin University
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Jilin University
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Abstract

The microwave plasma torch full spectrometer is a kind of spectral instrument for simultaneous multispectral detection in atomic emission spectrum analysis. The structure includes built-in water cooled microwave power source system, microwave plasma torch system, optical path system comprise concave reflector and optical fiber, spectroscopic detection system with spectroscopic detection module comprising flattening grating and ultraviolet enhanced array detector, and computer system. The present invention has small volume, small stable microwave power, conveniently altered spectral range, simultaneous detection of multiple elements, and other advantages.

Description

Simultaneous microwave plasma torch-atomic emission spectrometry
Technical field
The invention belongs to a kind of Atomic Emission Spectral Analysis and detect the device of atomic emission spectrum with multielement (multi-wavelength) simultaneously
Background technology
Current, in the used instrument in atomic emission spectrum field, mainly contain inductively-coupled plasma spectrometer and the sequential scanning ripple plasma torch spectrometer that declines.The commercialization inductively-coupled plasma spectrometer is in having experienced nearly 30 years evolution, and its technology is very ripe.The instrument type is also very perfect, comprises polytypes such as sequential scanning type, multi-channel type and full spectral pattern.Yet, inductively-coupled plasma spectrometer purchase and running, maintenance cost all very high.And not exclusively suitable developing country, medium-sized and small enterprises and institution of higher learning use.Commercial in recent years microwave plasma torch spectrometer has solved the costly problem of inductively-coupled plasma spectrometer to a certain extent.What but current microwave plasma torch spectrometer adopted is the scan-type driving mechanism, and instrumental analysis speed is slower, and the sample consumption is bigger.And there is the mechanical wear problem in Scan Architecture, and long-time stability are unsatisfactory.
With the close prior art of the present invention is a Chinese invention patent, and name is called " microwave plasma torch atomic emission spectrometer ", publication number CN1174991A, open day on March 4th, 1998.The structure of the disclosed spectrometer of this patent of invention comprises the microwave power origin system; Sample drawing-in system (solution sampling system)---contain sample, carrier gas source, atomizer, go to molten unit; Microwave plasma torch system (plasma source)---the interior pipe introduced for sample and carrier gas, 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, outer conductor and outer tube short circuit; Beam splitting system---mainly contain monochromator, what beam splitting system adopted is motor-driven grating monochromator beam split, and the instrument volume is big, sweep velocity is slow, and the sample consumption is bigger; The spectral signal detection system---mainly contain electrooptical device.Can also comprise computer system, be used for controlling the solution sample introduction, remove solubility temperature, work such as the step motor drive of monochromator and spectral signal detection.
Summary of the invention
The technical problem to be solved in the present invention is, overcome existing foregoing shortcoming of current commercialization microwave plasma torch spectrometer and deficiency, adopt modular design, use the ultraviolet enhanced linear array detecting device, realized that multielement, multi-wavelength detect simultaneously, it is slow fundamentally to eliminate the sequential scanning analysis speed that ripple plasma torch spectrometer exists that declines, the problem that the sample consumption is big; Design new spectral detection system, eliminate the mechanical wear problem that Scan Architecture exists, increase the reliability of analysis result.
The structure of simultaneous microwave plasma torch-atomic emission spectrometry of the present invention comprises the microwave power origin system; The sample drawing-in system---mainly contain sample, carrier gas source, atomizer, go to molten unit; The microwave plasma torch system---supply outer tube and shielding source of the gas that sample and the carrier gas interior pipe of introducing and the middle pipe and the work source of the gas that go the sulfuric acid pond exsiccator of molten unit to join, to introduce for work gas join, introduce for shielding gas to join, in pipe, middle pipe, outer tube be coaxial package successively, the inner wire of the microwave transmission wire terminal that one end is connected with microwave power source and middle pipe short circuit, outer conductor and outer tube short circuit; Can also comprise computer system, computer system also connects the input of sample drawing-in system control sample.With background technology different be that said microwave power origin system is built-in, uses the water cooling magnetron; Light path system is equipped with at torch flame place at microwave plasma torch, and said light path system is made up of the optical fiber of concave mirror that is installed in torch flame one side and torch flame opposite side; The other end of optical fiber is relative with the light entrance of spectral detection system, and said spectral detection system is light entrance, parallel light concave mirror, grating, optical convergence concave mirror and array detector by the optical propagation direction order; Array detector is realized the electric signal input computer system after the opto-electronic conversion.
Spectral detection system can adopt the flat field grating to strengthen the design proposal that array detector matches with ultraviolet.That is, said grating is the flat field grating; Said array detector is that ultraviolet strengthens array detector.
Spectral detection system can be made into the form of beam split detection module.Said beam split detection module is installed together by stationkeeping separately by parallel light concave mirror, grating, optical convergence concave mirror and array detector and constitutes; Each beam split detection module is selected the detection wavelength of different sections, thereby forms the beam split detection module of one group of series wavelength.During use, can pass through to change different beam split detection modules, and realize the detection of different wavelength range spectrum.The beam split detection module both can adopt concave grating to cooperate with the linear array detecting device, can adopt echelle grating to cooperate with two-dimensional array detector again.
The sample drawing-in system both can adopt the continuous sample introduction mode, can adopt the flow injection input mode again.Adopting the flow injection input mode can further reduce and eliminate matrix disturbs.Atomizer wherein can adopt concentric atomizer, the atomic spectroscopic analysis such as atomizer, ultrasonic atomizer that intersect atomizer commonly used.
The microwave plasma torch system can adopt the plasma torch pipe with oxygen function of shielding of 1/4 or 3/4 resonance wavelength.
Simultaneous microwave plasma torch-atomic emission spectrometry of the present invention has saved fan because microwave power source adopts the built-in form of water-cooled, owing to use Optical Fiber Transmission in the light path, make installation more random, therefore volume is little and compact, and it is low to consume microwave power, has strengthened the stability of energy output.Owing to partly increased a concave mirror, strengthened the ray-collecting ability, to improve analytical performance at light path system.Owing to adopt modular design, spectral detection system does not have movable member, change spectral range freedom, convenience, can realize that multielement (multi-wavelength) detects simultaneously, improved analysis speed, saved the sample consumption, Instrument purchase and running, maintenance cost are cheap, eliminate the mechanical wear problem that Scan Architecture exists, increased the reliability of analysis result.In a word, the present invention has solved fundamentally that inductively-coupled plasma spectrometer exists purchasing and running, maintenance cost high problem, it is slow also to have solved the sequential scanning analysis speed that ripple plasma torch spectrometer exists that declines, the sample consumption reaches the problem of mechanical wear greatly, has good practical values and market application foreground.
Description of drawings
Fig. 1 is the structured flowchart of simultaneous microwave plasma torch-atomic emission spectrometry of the present invention.
Fig. 2 is a sample drawing-in system synoptic diagram of the present invention.
Fig. 3 is a spectral detection system synoptic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the concrete structure of the present invention and the course of work are described.
The one-piece construction of embodiment 1 simultaneous microwave plasma torch-atomic emission spectrometry of the present invention.
See Fig. 1, one-piece construction of the present invention is divided into six parts, comprises sample drawing-in system 1, microwave power origin system 2, microwave plasma torch system 3, light path system 4, spectral detection system 5 and computer system 6.
Carrier gas source 21 is connected with the carrier gas inlet of sample drawing-in system 1; Shielding source of the gas 22 is connected with the outer tube of microwave plasma torch system 3.The inner wire of the microwave transmission wire terminal of microwave power origin system 2 and outer conductor respectively with the middle pipe and the outer tube short circuit of microwave plasma torch system 3.Microwave power origin system 2 is coupled to plasma torch system 3 with microwave energy, and carrier gas (be generally argon gas, also can use air or helium) under the effect of microwave energy, is ionized, excites the formation plasma.The be placed in torch flame both sides of microwave plasma torch system 3 of the concave mirror 23 of light path system 4 and an end of optical fiber 24.The other end of optical fiber 24 is relative with the light entrance of spectral detection system 5; Spectral detection system 5 adopts modular design, each parts fixed installation.Computer system 6 contains computer control 25 and shows 26, prints parts such as 27.Computer system control 25 also connects the input of sample drawing-in system 1 control sample.
The sample drawing-in system of embodiment 2 simultaneous microwave plasma torch-atomic emission spectrometries of the present invention.
Sample drawing-in system of the present invention 1 is basic identical in background technology, introduces by accompanying drawing at this, can help the understanding of the present invention.
Among Fig. 2,12 is carrier gas inlet, 13 are the sample solution inlet, sample solution (perhaps is thus lifted to atomizer 7 under the effect of peristaltic pump in carrier gas, through behind the atomizer 7, sample solution forms the sample aqueous aerosol, aqueous aerosol under the carrier band of carrier gas through fog chamber 8, oarse-grained here gasoloid deposits because of gravity and is rejected to outside the system by waste discharge mouth 14, residue granule aqueous aerosol removes pipe 9 through heating, here be heated to more than 100 degrees centigrade and make particles of solute and separated from solvent, high-temperature aerosol is by condenser pipe 10, here the major part of solvent is removed, next remaining gasoloid is through persulfuric acid pond exsiccator 11, most of here remaining solvent (water) is absorbed, and finally dried gasoloid is incorporated into the plasma torch flame by the interior pipe of microwave plasma torch system 3 and is excited, and contained various elements are launched characteristic spectral line separately in the sample solution.Among Fig. 2,15 is the water inlet of condenser pipe 10, and 16 is the water delivering orifice of condenser pipe 10.
The spectral detection system of embodiment 3 simultaneous microwave plasma torch-atomic emission spectrometries of the present invention.
See Fig. 3,31 is light entrance, corresponding with an end of optical fiber 24; 32 is the parallel light concave mirror, optical fiber 24 is passed the light of coming be reflected into directional light, shines on the grating 33 again, and grating 33 can be the flat field grating; Here complex light through projecting on the ultraviolet enhanced linear array detecting device 44 behind the optical convergence concave mirror 34, is realized the opto-electronic conversion of whole wavelength coverage by the monochromatic light of grating 33 beam split one-tenth according to Wavelength distribution.Electric signal after the conversion is shown by computer-controlled demonstration and print system 6 and prints, measures when finishing multielement in the sample solution (multi-wavelength).
Beam split detection module 5 is key components of instrument.What adopt among the present invention is the one-dimensional linear array detector.In addition, also can cooperate the cross dispersion element to replace, realize the two-dimensional detection of spectrum in order to echelle grating with the design module that the two-dimensional array detecting device combines.Instrument can pass through to change different beam split detection modules, and realizes the detection of different wavelength range spectrum.

Claims (3)

1, a kind of simultaneous microwave plasma torch-atomic emission spectrometry, its structure comprise microwave power origin system (2); Sample drawing-in system (1); Microwave plasma torch system (3) is by interior pipe, middle pipe, the outer tube of coaxial package constitute computer system (6), the input of computer system (6) connection sample drawing-in system (1) control sample successively; It is characterized in that said microwave power origin system (2) is built-in, use the water cooling magnetron; Light path system (4) is equipped with at torch flame place in microwave plasma torch system (3), and said light path system (4) has the optical fiber (24) of the concave mirror (23) that is installed in torch flame one side and torch flame opposite side to form; The other end of optical fiber (24) is relative with the light entrance (31) of spectral detection system (5); Said spectral detection system (5) is light entrance (31), parallel light concave mirror (32), grating (33), optical convergence concave mirror (34) and array detector (35) by the optical propagation direction order; Array detector (35) is realized the electric signal input computer system (6) after the opto-electronic conversion.
According to the described simultaneous microwave plasma torch-atomic emission spectrometry of claim 1, it is characterized in that 2, spectral detection system (5) adopts flat field grating and ultraviolet to strengthen array detector and matches, promptly said grating (33) is the flat field grating; Said array detector (35) is that ultraviolet strengthens array detector; Spectral detection system (5) is made into the form of beam split detection module, said beam split detection module is installed together formation by parallel light concave mirror (32), grating (33), optical convergence concave mirror (34) and array detector (35) by stationkeeping separately, and each beam split detection module is selected the detection wavelength of different sections.
According to claim 1 or 2 described simultaneous microwave plasma torch-atomic emission spectrometries, it is characterized in that 3, the beam split detection module adopts concave grating to cooperate with the linear array detecting device or adopts echelle grating to cooperate with two-dimensional array detector.
CN 03127672 2003-08-08 2003-08-08 Mirowave plasma torch full spectometer Expired - Fee Related CN1230672C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101865848A (en) * 2010-05-21 2010-10-20 北京泰科诺科技有限公司 Method and device for measuring monobromethane concentration in fumigation tank by plasma emission spectroscopy
CN104602437A (en) * 2015-01-13 2015-05-06 吉林大学 Energy field generating device and control method thereof
CN105136749A (en) * 2015-08-20 2015-12-09 浙江中控研究院有限公司 Microwave plasma torch atomic emission spectrometer
CN105277906A (en) * 2014-06-05 2016-01-27 核工业西南物理研究院 High-precision magnetic field inclination angle measuring system applied to magnetic confinement fusion device
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
CN115791713A (en) * 2022-03-04 2023-03-14 成都艾立本科技有限公司 Aerosol element analysis device

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101865848A (en) * 2010-05-21 2010-10-20 北京泰科诺科技有限公司 Method and device for measuring monobromethane concentration in fumigation tank by plasma emission spectroscopy
CN101865848B (en) * 2010-05-21 2012-05-30 北京泰科诺科技有限公司 Method and device for measuring monobromethane concentration in fumigation tank by plasma emission spectroscopy
CN105277906A (en) * 2014-06-05 2016-01-27 核工业西南物理研究院 High-precision magnetic field inclination angle measuring system applied to magnetic confinement fusion device
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
CN105136749A (en) * 2015-08-20 2015-12-09 浙江中控研究院有限公司 Microwave plasma torch atomic emission spectrometer
CN105136749B (en) * 2015-08-20 2017-12-22 浙江全世科技有限公司 A kind of microwave plasma torch atomic emission spectrometer
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
CN115791713A (en) * 2022-03-04 2023-03-14 成都艾立本科技有限公司 Aerosol element analysis device

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