CN102269707B - Portable element spectrograph for online detection of liquid/gas phase sample - Google Patents
Portable element spectrograph for online detection of liquid/gas phase sample Download PDFInfo
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Abstract
The invention discloses a portable element spectrograph for online detection of a liquid/gas phase sample. The portable element spectrograph comprises a sample leading-in system, a plasma atomization system and a spectral measurement processing system, wherein the plasma atomization system mainly comprises a plasma torch tube, a microwave energy exertion device, and a plasma triggering device and a plasma torch stabilizing chamber; the plasma torch tube is composed of a sample conveying inner tube, a middle tube which is coaxially sleeved on the inner tube and uses a conducting metal as an outer material, and an outer tube shell coaxially sleeved out of the middle tube; the microwave energy exertion device is composed of a microwave source and an antenna connected with the microwave source through a microwave transmission conducting wire; and the antenna is arranged out of the tube wall of the middle tube to close to an outlet. The element spectrograph is suitable for the liquid phase sample as well as the gas phase sample, can realize the online detection in real time, has the advantages of high detection sensitivity, low power, less gas consumption, small volume and light weight, and can be used for detecting almost all elements in the periodic table.
Description
Technical field
The present invention relates to a kind of ultimate analysis instrument, be specifically related to a kind of portable spectrometer of the liquid/gas phase sample on-line real time monitoring based on microwave induced plasma, particularly the spectral detection of transition metal, rare earth element, actinide, alkaline metal and alkali earth metal microwave plasma source.
Background technology
Along with development and the progress of industrial technology, transition metal, rare earth element, actinide, alkaline metal and alkali earth metal are used also more and more widely, and be simultaneously also more and more serious by its pollution that causes.Preparation technology with beryllium is example, and beryllium is by extracting and be converted into beryllium hydroxide in the beryl, is used for realizing synthetic, the ceramic production of metal alloy and oxide, industry and the military uses such as preparation of pure beryllium.Because the increasing of supervision and to the lifting of beryllium recognizing dangers, at production, purification and the beryllium product of beryllium in industry, commercial use, to beryllium content in the context carry out in time, exactly mensuration seems particularly important.
Along with the enhancing of people's social enviroment protection consciousness with to the lifting of labourer's due care degree, countries in the world are strong day by day for the demand that realizes transition metal, rare earth element, actinide, alkaline metal and alkali earth metal in the monitoring air and water sample in real time.In addition, in industrial processes, can carry out quality control by the detection to some element, can save production cost in a large number, reduce or eliminate the generation of waste product, as the coating process in the semi-conductor industry production, and biomedicine field, environmental area, metallurgical Exploration Domain, space industry etc., all can carry out quality of production control by some element is detected.Therefore, develop highly sensitive, and can be fast, the portable checkout equipment of above-mentioned element in the on-line real time monitoring industrial emissions, become the task of top priority of various countries and the target of chasing for a long time.
United States Patent (USP) (U.S. Pat. No. 4,844,612 (Durr and Rozain, Jul. 4,1989)) disclose and a kind ofly applied excitation energy by electromagnetic field article on plasma body, utilize electro-induction coupled plasma emission spectrum to realize the sample element is carried out the method for analyzing and testing, can be used for beryllium or other trace elements in the tracer liquid sample.Be used for implementing the detector that element detects, comprise that mainly detected sample and plasma keep the gas drawing-in system, plasma atomization system and spectral measurement disposal system, wherein plasma atomization system applies electromagnetic field with radio frequency (RF) as the energy that forms plasma, the frequency of RF is 27-28MHz, because the frequency of RF is low, penetration capacity is not strong, in order to obtain stable plasma torch, need to use powerful RF to build electromagnetic field, its power generally must reach 1000-2000W, the airshed of keeping of plasma also must be big simultaneously, reach 15-25L/min.In view of radio frequency (RF) power of this elements are contained instrument big, need to be equipped with special-purpose power power-line, it is big that plasma is kept gas flow, the drawing-in system device volume is big, and need the special ventilating system of configuration, therefore, this measuring instrument is the desk-top fixed equipment that use in a kind of laboratory, people can only deliver to sample the measurement that trace element is carried out in the laboratory, can not be used for online or on-the-spot test sample being detected in real time.
Summary of the invention
The all restrictions of element detector based on prior art, what purpose of the present invention aimed to provide a kind of small portable not only detected spectrometer applicable to liquid phase sample but also applicable to the element of gas phase sample, to satisfy people to realizing online real-time detection, the detection sensitivity height, economical and practical, energy consumes the tight demand of low novel element detector again.
The portable element spectrometer that is applicable to the online detection of liquid/gas phase sample provided by the invention, comprise the sample drawing-in system, plasma atomization system and spectral measurement disposal system, wherein plasma atomization system comprises the plasma torch pipe again, the microwave energy bringing device, plasma initiating device and plasma torch equalization chamber, described plasma torch pipe is by managing in the sample delivery, coaxially be nested with middle pipe and the coaxial outer pipe shell that is nested with outside middle pipe that outside interior pipe material is conducting metal and constitute, perimetrical lumen between the interior Guan Yuzhong pipe is that plasma is kept the letter shoot road, its import is kept the gas outlet with the plasma in the sample drawing-in system and is connected, testing sample outlet in the import of interior pipe and the sample drawing-in system is connected, described microwave energy bringing device is made of with the antenna that is connected with microwave source by the microwave transmission lead microwave source, the tube wall of pipe was outward near the exit during antenna was arranged on, described plasma initiating device connects the plasma torch district by lead, described torch equalization chamber is arranged on the plasma torch pipe port, and locular wall is arranged on the trough place of microwave propagation direction, and the locular wall design has outlet port and is used for being provided as the window of the light collecting device of a spectral measurement disposal system part.
In technique scheme, when testing sample is fluid sample, testing sample in the described sample drawing-in system is introduced Subsystem Design interconnective fluid sample discharge pump, atomizer and removal of solvents device, and atomizer is connected with the air shooter of atomized liquid sample.Any suitable atomising device all can be used for the atomizing of liquid sample, as ultrasonic atomizer.When excessive being not suitable for of sample humidity of being come out by the removal of solvents device, can behind the removal of solvents device, set up exsiccator atomized sample is carried out drying, the outlet of the import of exsiccator and removal of solvents device is connected, exports with the interior pipe import of plasma torch pipe in the plasma atomization system to be connected.For fluid test sample, plasma in the sample drawing-in system is kept gas introducing subsystem can be provided with two introducing branch roads, the meter of leading up to is connected with the atomizer that testing sample is introduced in the subsystem, fluid sample is atomized, another road is kept the conduit entrance of gas conveying annular by meter with the plasma in the plasma atomization system and is connected, and keeps gas for plasma provides.The flow velocity that plasma is kept gas is adjustable, and range of adjustment is 0.1 L/min to 10 L/min, and specifically the factors such as gaseous species, pipe diameter, testing sample concentration of keeping gas by required plasma shape, plasma determine.Usually flow velocity is between 0.5 L/min to 4 L/min.
In technique scheme, when testing sample is gaseous sample, sample in the drawing-in system is introduced subsystem does not then need to arrange atomizer, generally do not need to arrange removal of solvents device and exsiccator yet, the pressure of gaseous sample is enough big, can be introduced directly into the interior pipe of the plasma torch pipe in the plasma atomization system, when the pressure of gaseous sample was enough big, gaseous sample can be sent into plasma atomization system by air pump.When the quantity not sufficient of gaseous sample is enough big, also can introduce a part of plasma and keep gas, enter plasma atomization system in the lump.
In order to obtain better technique effect, on the basis of technique scheme, the present invention also can further take following technical measures.Following technique measures can be taked separately respectively, also can a plurality of measure combinations take, or takes simultaneously in the lump.
Torch equalization chamber in the plasma atomization system, its locular wall is preferably disposed on the trough place of microwave propagation direction, and chamber radial dimension and axial dimension all are not more than 5 wavelength.According to this characteristics design torch equalization chamber.
Be provided with the microwave reflection mirror in the middle pipe of plasma torch pipe and the perimetrical lumen between the outer pipe shell, the microwave reflection mirror is positioned at the microwave antenna below, in order to the microwave energy of antenna emission is reflexed to the plasma torch zone.In the perimetrical lumen in the microwave reflection mirror preferably can move up and down and be arranged on with regulating between pipe and the outer pipe shell.The distance of microwave antenna and microwave reflection mirror is preferably the odd multiple of microwave 1/4 wavelength, as 1/4,3/4,5/4,7/4 λ.Wherein 1/4 λ is conducive to the miniaturization of instrument most.Microwave antenna is the antenna that can coincide with middle pipe outer tube wall, and as the ring body antenna, ring body can be loopful, semi-ring, ring piece etc.The preferential loopful body antenna that fits like a glove with middle pipe outer tube wall that adopts.Antenna and middle pipe upper port should approach as far as possible, transfer to the plasma torch district efficiently with the assurance microwave energy, and avoid microwave vertically to transmit the interference that brings in the plasma torch pipe.
Under the special requirement situation, can electronic semi-conductor's cooling piece be set at the outer pipe shell housing wall of plasma torch pipe, cool off with article on plasma body torch pipe outer pipe shell.It can certainly be other the type of cooling.
At least one plasma that is evenly equipped with some through holes is set in the perimetrical lumen between middle pipe and interior pipe keeps the gas distributor, the through hole that through hole on the distributor preferably tilts towards direction makes plasma keep gas and is the eddy flow shape and flows out from the plasma torch pipe.
Design has at least one to be used for the equalizing port of the inside and outside gaseous tension of balance pipe on the tube wall of middle pipe.
The over top design of torch equalization chamber has the toxic emission chamber, and torch equalization chamber is communicated with the toxic emission chamber by the through hole that is positioned at the center of top place, and outlet port designs on the sidewall of drain chamber.
Face the scope of plasma torch at torch equalization chamber sidewall for the window design that spectral measurement disposal system light collecting device is set.
The length of plasma torch pipe is preferably designed as the odd-multiple of microwave 1/4 wavelength, and is not more than 200cm.Concrete length depends on the requirement of instrument portability.Generally, the length of plasma torch pipe is 1/4 or 3/4 wavelength, is approximately 5 cm to 15 cm.
The middle pipe of plasma torch pipe is simultaneously as the conduit of microwave energy, so its material is necessary for the material that can electricity lead, with compatible microwave energy transfer.Its optional material has copper, brass, aluminium, stainless steel, silver, gold and alloy thereof.Inner tube material can be conductor or insulator, comprises copper, brass, aluminium, stainless steel, silver, gold and alloy thereof, and is quartzy, ceramic.Wherein stainless steel and pottery have best corrosion resistance and plasma stability.
Anyly can be excited the gas that forms plasma all to can be used as plasma by microwave energy to keep gas.Adoptable gas has argon gas, helium, nitrogen, air etc.The concrete selection determined by the kind that detects required sensitivity and analyte.
Microwave frequency all can be used for exciting and stable plasma between 1000 MHz to 10000 MHz.Usual range is 2000-3000 MHz, and wherein optimum frequency is 2450 MHz.Plasma torch is stablized power demand and is generally 50-200W or higher.Any microwave source device that proper frequency scope microwave energy is provided all can be used as the microwave source of microwave energy bringing device of the present invention.Usually the microwave source that adopts has microwave oscillator, magnetron and klystron generator motor.Wherein magnetron becomes the optimal selection of microwave source with its wideer power bracket.The microwave transmission lead pass plasma torch pipe outer pipe shell with microwave energy from microwave source transfer to be arranged on antenna on the pipe.The microwave call wire can be concentric cable, waveguide or other suitable device.
The initiation of realization plasma can be kept gas by the plasma of article on plasma tagma scope and apply enough energy to produce kind of an electronics.But the using plasma initiating device reaches plasma slab by conductor with the excitation energy of its generation, keeps exciting of gas to realize the article on plasma body.
The plasma slab flame shape can be flamboyancy or ring-type, all can be used for the measurement to testing sample.The shape of torch depends on the shape of the plasma torch pipe mouth of pipe.
Plasma torch equalization chamber prevents that for the protection of the plasma torch district air-flow or extraneous gas from entering and keeping the stable of plasma torch.The material of any anti-plasma high temperature all can be used for plasma torch equalization chamber.
Light collecting device in the spectral measurement disposal system has multiple choices, depends on the setting of system, the type of signal projector, the type of analytical instrument etc.Comprising various optical focus eyeglasses, optical filter, waveguide and optical fiber.Collimation lens can be collected the light that plasma sends from the side, and will import in the optical fiber after the light gathering.Yet the light collection efficiency of collimation lens commonly used is lower ,≤5 %.Adopt double lens to collect solid angle to improve ray-collecting efficient by expanded light beam.
The light signal that plasma torch produces can be by one or more Optical Fiber Transmission to one or more detecting device.Detecting device commonly used is the linear CCD detecting device with element pixel.Any suitable computer control system all can be used for the processing of the control data of flow velocity.Can adopt commercial software, as 32 OOIBAS software.
The portable element spectrometer of online detection provided by the invention is that first realization is carried out the on-the-spot portable spectrometer of plasma source that real-time online detects to liquid/gas phase sample.This instrument adopts multinomial sophisticated technology under atmospheric pressure to obtain stable microwave induced plasma, and successfully is used for the express-analysis of sample.The collection of atomic emission spectrum and processing are carried out the qualitative and quantitative analysis of element to be measured by a small light spectrometer and computer data processing system by peak position and peak area.
Advantages such as that the portable element spectrometer of online detection provided by the invention has is powerful, easy to carry, compact conformation, flexible operation, support on-the-spotly detect, low manufacturing cost and running cost, can be applied to the on-line analysis of industry very ideally, teaching and scientific research work in the university, and Government Laboratory.Simultaneously, because this element spectrometer can combine with sampling device, touch screen operation effectively, possesses low keep gas and microwave energy consumption.
The portable element spectrometer of online detection provided by the invention is applicable to that all need carry out occasion on-the-spot or that online liquid and gas sample is measured fast, all has greatly market development potential in a plurality of fields.At first, its exclusive advantage and portability will provide great facility for the Government Laboratory that relates to manufacturing, offal treatment, nuclear fuel material recycling.Secondly, this instrument also will be conducive to relevant teaching and the research work of institution of higher learning.
The industry and the field that the portable element spectrometer of online detection provided by the invention are had big demand:
Semiconductor manufacturing industry
Environmental monitoring
Food ﹠ Drink processing
The energy and material science
Petrochemicals is analyzed
Geologic prospecting and exploitation
Nuclear material processing, national security and national defence
Electronics and space industry
Institution of higher learning's teaching and scientific research
The portable element spectrometer of online detection provided by the invention characteristics:
The sensitivity of ppb level is arranged.
Possess integration capability and can carry out online real-time analysis.
Simple to operation, can adopt the computer-controlled operation process.
Selectable integrated sampling system comprises ultrasonic atomizer and peristaltic pump.
Liquid, gaseous sample all can be handled.
Multiple gases can be used as plasma and keeps gas, comprises argon, helium and mixed gas thereof.
Steady operation under atmospheric pressure.
Plasma is introduced sample has good tolerability.
Plasma torch is formed in the plasma chamber, can guarantee its stability and operating personnel's safety.
The sealing exhaust does not need special ventilating system.
Plasma power is low to moderate 50-200W.
Plasma flow speed is lower than 1 L/min.
Can be designed to on-the-spot portable, desk-top or rack.
The portable element spectrometer of online detection provided by the invention advantage part:
Power is low, not equipment which requires cooling.Be 1500-2800 W with traditional ICP-AES(power) to compare, the power that possesses the portable element spectrometer of the online detection of advanced technology significantly descends, and only is 50-200 W.ICP-AES independently water storage device is used for forcing cooling with relevant refrigeration piping, and small-sized element spectrometer is without any need for external refrigeration equipment.
Gas consumption is low.Common competitive instrument has bigger gas consumption, is about 15-50 L/min, is used to form plasma, plasma protection gas and transmission sample.The gas consumption of the portable element spectrometer of online detection is lower than 1.0 L/min.Because do not need plasma protection gas, small-sized element spectrometer reaches same precision and detection level power demand and descends greatly.
Institute takes up space little.Conventional instrument requisite space is all above 1 m
3(not comprising atomizing and cooling device).And the portable element spectrometer of small-sized online detection in conjunction with atomization plant after 0.06 m only
3(not needing cooling device), its volume ratio General Instrument has dwindled more than 16 times.
Weight is little.At present available product weight surpasses 180 kg(mostly and does not comprise atomizer and water cooling equipment).The weight of the portable element spectrometer of online detection is only about 30 kg, than the light 6-12 of similar other instruments doubly.
Cost is low.
Be conducive to keep the cleaning of indoor environment.Existing ICP-AES all is equipped with not contact above its plasma chamber ventilating duct (diameter is 15 cm) is used for plasma gas is discharged to outdoor.Yet the gas of emptying will not influence the cleaning of indoor environment.The portable element spectrometer of online detection is because its low-power and low-flow amount only need a filtrator and a simply pipeline.
But nearly all element in the sense cycle table.
Description of drawings
Fig. 1 is structural representation of the present invention.
Fig. 2 is a kind of structural representation of drawing-in system of the present invention, is used for the detection of gaseous sample.
In above-mentioned each accompanying drawing, each shown by reference numeral sign object is respectively: manage among the 1-; Pipe in the 2-; The 3-shaft collar; The 4-outer pipe shell; 5-microwave reflection mirror; 6-electronic semi-conductor cooling piece; The 7-tours antenna; 8-spectral measurement treating apparatus; The 9-convex lens; Toxic emission chambers 10; The 11-plasma torch; The 12-plasma torch; The 13-microwave source; The 14-plasma is kept the gas distributor; The 15-equalizing port; The 16-gasometer; The 17-gasometer; The 18-discharge pump; The 19-atomizer; 20-removal of solvents device; The 21-exsiccator.
Embodiment
The present invention is described in further detail below in conjunction with embodiment; it is important to point out; following embodiment is only for the present invention is described further; can not be interpreted as limiting the scope of the invention; affiliated art skilled staff is according to the foregoing invention content; the present invention is made some nonessential improvement and adjustment is specifically implemented, should still belong to protection scope of the present invention.
Embodiment 1
Present embodiment is the portable element spectrometer for the online detection of fluid sample, mainly by sample drawing-in system, plasma atomization system and spectral measurement disposal system.Wherein plasma atomization system is made of equalization chamber and the toxic emission chamber 10 of plasma torch pipe, microwave energy bringing device, microwave reflection mirror 5, plasma initiating device 12, plasma torch.Described plasma torch pipe by manage 2 in the sample delivery, it is coaxial that to be nested with outside interior pipe material be that middle pipe 1 and the coaxial outer pipe shell 4 that is nested with outside middle pipe of conducting metal constitutes, perimetrical lumen between the interior Guan Yuzhong pipe is that plasma is kept the letter shoot road, its import and the plasma in the drawing-in system are kept the gas outlet and are connected, and the import of interior pipe exports with testing sample in the sample drawing-in system and is connected.The tours antenna 7 that described microwave energy bringing device matches by microwave source 13, with middle pipe 1 tube wall with pass the microwave transmission concentric cable that outer pipe shell 4 is connected with tours antenna 7 and constitute, tube wall was outward near the exit during tours antenna was arranged on and approaches.Annular space in described microwave reflection mirror 5 can be arranged on up or down by regulating device between pipe and the outer pipe shell, be positioned at microwave tours antenna below apart from the position of antenna 3/4 microwave wavelength, described regulating device is made of shaft collar 3 and the set screw on the pipe shell in being fixed on, and the two ends of screw act on microwave reflection mirror and shaft collar respectively.Described plasma initiating device 12 connects the plasma torch district by lead.Described torch equalization chamber is arranged on the plasma torch pipe port, the locular wall of torch equalization chamber is positioned at the trough place of microwave, the diameter of torch equalization chamber and axial height are a wavelength, design is useful on the window of the convex lens 9 that is provided as a spectral measurement disposal system part on the torch equalization chamber sidewall, the over top design has toxic emission chamber 10 in torch equalization chamber, torch equalization chamber is communicated with the toxic emission chamber by the through hole that is positioned at the center of top place, and outlet port designs on the sidewall of drain chamber.Fluid sample in the described drawing-in system is introduced subsystem, peristaltic pump 18, atomizer 19, removal of solvents device 20 and exsiccator 21 by the conveying fluid sample that connects successively by pipeline constitute, and the outlet of exsiccator is connected with the interior pipe import of plasma torch pipe; Plasma in the drawing-in system is kept gas introducing subsystem and is provided with two introducing branch roads, the meter 17 of leading up to is connected with the atomizer that liquid test sample product are introduced in the subsystem, fluid sample is atomized, another road is kept the conduit entrance of gas conveying annular by meter 16 and the plasma in the plasma torch pipe and is connected, and keeps gas for plasma provides.The spectral measurement disposal system with double lens 9 as the spectrum gathering-device, by luggable computer control spectral measurement treating apparatus 8, the spectral measurement treating apparatus is the linear CCD detecting device with element pixel, and the software that computing machine uses is 32 commercially available OOIBAS softwares.
Embodiment 2
Present embodiment also is the portable element spectrometer for the online detection of fluid sample, its structure is substantially the same manner as Example 1, difference is that plasma atomization system is provided with electronic semi-conductor's cooling piece 6 at the outer pipe shell shell wall of plasma torch pipe, keeping the design of gas conveying annular pipeline at plasma has plasma to keep gas distributor 14, design has 8 uniform air holes on the distributor annular disk, in the design of plasma torch pipe inner tubal wall 3 equalizing ports 15 are arranged, with the inside and outside hydrodynamic pressure of pipe in the balance.
Embodiment 3
Present embodiment is the portable element spectrometer for the online detection of gaseous sample, and its structure and substantially the same manner as Example 1, difference are the sample drawing-in systems.The structure of drawing-in system as shown in Figure 2.Gaseous sample to be measured directly is sent to the interior pipe of plasma torch pipe by air pump, plasma is kept gas introducing subsystem and still is provided with two introducing branch roads, the meter 17 of leading up to is incorporated the gas testing sample into and is introduced subsystem, the deficiency of make-up gas sample size, another road is kept the conduit entrance of gas conveying annular by meter 16 and the plasma in the plasma torch pipe and is connected, and keeps gas for plasma provides.
Embodiment 4
Present embodiment also is the portable element spectrometer for the online detection of gaseous sample, and the structure of its plasma atomization system is substantially the same manner as Example 2, and the structure of its sample drawing-in system is substantially the same manner as Example 3.
Claims (11)
1. portable element spectrometer that is used for the online detection of liquid/gas phase sample, comprise the sample drawing-in system, plasma atomization system and spectral measurement disposal system, it is characterized in that described plasma atomization system comprises the plasma torch pipe, the microwave energy bringing device, plasma initiating device and plasma torch equalization chamber, described plasma torch pipe is by managing in the sample delivery, coaxially be nested with middle pipe and the coaxial outer pipe shell that is nested with outside middle pipe that outside interior pipe material is conducting metal and constitute, perimetrical lumen between the interior Guan Yuzhong pipe is that plasma is kept the letter shoot road, its import is kept the gas outlet with the plasma in the sample drawing-in system and is connected, testing sample outlet in the import of interior pipe and the sample drawing-in system is connected, described microwave energy bringing device is made of with the antenna that is connected with microwave source by the microwave transmission lead microwave source, tube wall was outward near the exit during antenna was arranged on, described plasma initiating device connects the plasma torch district by lead, described torch equalization chamber is arranged on the plasma torch pipe port, and locular wall is arranged on the trough place of microwave propagation direction, designs the window that outlet port is arranged and be used for being provided as the light collecting device of a spectral measurement disposal system part on the locular wall; When testing sample is liquid, fluid sample in the described sample drawing-in system is introduced Subsystem Design interconnective fluid sample discharge pump, atomizer, removal of solvents device and exsiccator, atomizer is connected with the air shooter of atomized liquid sample, the outlet of the import of exsiccator and removal of solvents device is connected, and the outlet of exsiccator is connected with interior pipe import in the plasma atomization system; When testing sample was gas, sample drawing-in system gaseous sample to be measured directly was sent to the interior pipe of plasma torch pipe by air pump.
2. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 1, it is characterized in that when testing sample is liquid, plasma in the described sample drawing-in system is kept gas introducing subsystem and is provided with two introducing branch roads, the meter of leading up to is connected with the atomizer that the testing liquid sample is introduced in the subsystem, and another road is kept the import of letter shoot road by meter with the plasma in the plasma atomization system and is connected.
3. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 1 and 2 is characterized in that the chamber radial dimension of torch equalization chamber and axial dimension all are not more than 5 wavelength.
4. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 3, it is characterized in that being provided with the microwave reflection mirror at the middle pipe of plasma torch pipe and the annular space between the outer pipe shell, the microwave reflection mirror is positioned at the microwave antenna below, and the distance of microwave antenna and microwave reflection mirror is the odd multiple of microwave 1/4 wavelength.
5. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 4 is characterized in that described microwave reflection mirror can move up and down the annular space that is arranged between middle pipe and the outer pipe shell with regulating.
6. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 3 is characterized in that the outer pipe shell housing wall of plasma torch pipe is provided with electronic semi-conductor's cooling piece.
7. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 3 is characterized in that being provided with at least one plasma that is evenly equipped with some through holes in the middle pipe of plasma torch pipe and the perimetrical lumen between the interior pipe keeps the gas distributor.
8. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 3 is characterized in that design has at least one to be used for the equalizing port of the inside and outside gaseous tension of balance pipe on the tube wall of plasma torch tube-in-tube.
9. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 3, it is characterized in that in the over top design of torch equalization chamber the toxic emission chamber being arranged, torch equalization chamber is communicated with the toxic emission chamber by the through hole that is positioned at the center of top place, and outlet port designs on the sidewall of drain chamber.
10. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 3 is characterized in that facing at torch equalization chamber sidewall be used to the window design that spectral measurement disposal system light collecting device is set the scope of plasma torch.
11. the portable element spectrometer for the online detection of liquid/gas phase sample according to claim 3 is characterized in that the length of plasma torch pipe is the odd-multiple of microwave 1/4 wavelength, and is not more than 200cm.
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CN102914522B (en) * | 2012-11-13 | 2014-07-30 | 西北师范大学 | Gas-liquid combined laser induced breakdown spectroscopy detection device and method |
CN103983620A (en) * | 2013-02-07 | 2014-08-13 | 北京瑞利分析仪器有限公司 | Closed type atomization system |
CN103196894B (en) * | 2013-03-13 | 2015-07-15 | 天津师范大学 | Plasma atomic emission spectroscopy analysis method and plasma atomic emission spectroscopy analysis apparatus using gaseous sample injection |
US9427821B2 (en) * | 2013-03-15 | 2016-08-30 | Agilent Technologies, Inc. | Integrated magnetron plasma torch, and related methods |
CN104749139B (en) * | 2015-03-26 | 2018-08-03 | 四川大学 | Plasma surface sample introduction excitation spectrum detecting system under matrix auxiliary |
GB2582948B (en) * | 2019-04-10 | 2021-12-08 | Thermo Fisher Scient Bremen Gmbh | Plasma source chamber for a spectrometer |
CN110487775A (en) * | 2019-07-25 | 2019-11-22 | 电子科技大学 | A kind of portable spectral analysis device based on plasma |
CN112255149B (en) * | 2020-10-10 | 2022-07-05 | 中国科学院近代物理研究所 | Method and system for detecting particle size of loose particle accumulation and storage medium |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1174991A (en) * | 1997-07-08 | 1998-03-04 | 吉林大学 | Microwave plasma torch atomic emission spectrometer |
CN2641645Y (en) * | 2003-08-08 | 2004-09-15 | 吉林大学 | Microwave plasma torch full spectrometer |
CN201107273Y (en) * | 2007-11-28 | 2008-08-27 | 成都理工大学 | Atomic fluorescent spectrometer |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AUPS245402A0 (en) * | 2002-05-21 | 2002-06-13 | Varian Australia Pty Ltd | Plasma torch for microwave induced plasmas |
-
2011
- 2011-07-13 CN CN 201110195562 patent/CN102269707B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1174991A (en) * | 1997-07-08 | 1998-03-04 | 吉林大学 | Microwave plasma torch atomic emission spectrometer |
CN2641645Y (en) * | 2003-08-08 | 2004-09-15 | 吉林大学 | Microwave plasma torch full spectrometer |
CN201107273Y (en) * | 2007-11-28 | 2008-08-27 | 成都理工大学 | Atomic fluorescent spectrometer |
Non-Patent Citations (5)
Title |
---|
冯国栋.小型微波等离子体炬全谱仪的研制及其应用基础研究.《中国优秀博硕士学位论文全文数据库(博士) 工程科技II辑》.2005,2-4页. * |
刘军等.微波等离子体炬结构的改进.《分析仪器》.1993,(第2期),第22-24页. |
张晓惠等.微波诱导等离子体原子发射光谱法测定被铬相钒错锗的研究.《岩矿测试》.1992,第11卷(第3期),第221-224页. |
微波等离子体炬结构的改进;刘军等;《分析仪器》;19930430(第2期);第22-24页 * |
微波诱导等离子体原子发射光谱法测定被铬相钒错锗的研究;张晓惠等;《岩矿测试》;19920930;第11卷(第3期);第221-224页 * |
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