WO2001065244A9 - Microwave plasma monitoring system for real-time elemental analysis - Google Patents
Microwave plasma monitoring system for real-time elemental analysisInfo
- Publication number
- WO2001065244A9 WO2001065244A9 PCT/US2001/005092 US0105092W WO0165244A9 WO 2001065244 A9 WO2001065244 A9 WO 2001065244A9 US 0105092 W US0105092 W US 0105092W WO 0165244 A9 WO0165244 A9 WO 0165244A9
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- plasma
- gas
- sample gas
- recited
- conduit
- Prior art date
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Definitions
- This invention relates to a method and apparatus for elemental analysis.
- invention relates more particularly to a method and apparatus with microwave plasma
- transition metals rare earth elements, actinides, or alkali and alkaline earth elements.
- beryllium is extracted from beryl ore and converted to
- the filters can be taken off location for ranges of time from minutes to hours.
- Inductive plasma spectrometry has been used to analyze elements from a plasma
- Microwave plasmas have been used for trace element monitoring. Microwave
- inductively coupled plasma source atomic emission spectrometers for analysis.
- invention has a concentric arrangement of plasma gas and sample gas conduits so as to
- the multiple conduit apparatus of the invention comprises:
- the microwave plasma torch can either be contained within a sealed housing or
- the microwave plasma torch of this invention can be operated in ambient air at ambient pressures.
- the microwave plasma torch of this invention can be operated continuously for
- transition metals rare earth elements, actinides, and alkali and alkaline earth elements.
- the invention apparatus can also be used to monitor for the presence of halogens, sulfur
- the invention apparatuses and methods are more particularly useful for
- Figure 1 is a schematic of an example invention device wherein no additional
- carrier gas is needed for transport of the sample to the plasma region
- Figure 2 is a schematic of an example of an invention device having three
- Figure 3 is a flow chart showing process flow for use of the invention to monitor a
- transition metals rare earth elements, actinides, or alkali and alkaline earth elements
- sample gas generally ambient air
- microwave plasma torch can be operated in either an
- Figure 1 is a schematic drawing of an apparatus which can be used to analyze air
- sealed housing 2 is useful when the sample gas (the air or other gas containing the sample gas).
- analyte to be monitored is to be sucked or drawn through the microwave plasma torch K
- a pump _18 is
- a sealed housing Y2 can also be useful if the invention apparatus is to be used in a
- any combination thereof is positioned downstream or upstream of the plasma torch, any combination thereof.
- the sample gas to be tested is circulated through the sample gas conduit 20 into the plasma torch J_0.
- the sample gas conduit 20 has an open upper end 22 where, in the
- housing 2 causes the sample gas to circulate upward into the plasma region 16.
- the sample gas conduit 20 does not necessarily have to be made of an electrically
- Suitable materials include, but are not limited to, copper, brass, aluminum, alumina,
- the flow rate of the sample gas can be controlled by any suitable means such as a
- sample gas and the plasma gas can be introduced
- sample gas to be monitored or tested can be pretreated as needed.
- sample gas conduit 20 to dry the sample gas before introduction of the sample gas into
- sample gas conduit 20 so that the sample gas to be tested is circulated through the
- membraneous conduit 24 The membraneous conduit 24 is encased in a larger conduit 26
- dryers in series in the sample gas conduit can be employed as needed.
- Any suitable means for delivering the plasma gas into the plasma formation area is any suitable means for delivering the plasma gas into the plasma formation area
- Pressurized plasma gas can be released into the plasma gas conduit, or
- plasma gas can be pumped into the plasma gas conduit.
- the flow rate of the plasma gas can be controlled by any suitable means such as a
- a flowmeter in the conduit transporting the plasma gas into the plasma torch is used.
- a flow rate in the range from about 0.1 liter per minute to about 10 liters per minute can be used,
- plasma gas flow rate in the range from about 0.05 liter per minute to about 4.0 liters per
- sample gas and the plasma gas can be
- the plasma gas is
- sample gas and plasma gas conduits can be any convenient length from only
- plasma gas has a smaller diameter than the sample gas conduit and coaxially positioned
- the outermost conduit (which is the plasma gas conduit 30 in Figure 1 or the
- the one with the smaller diameter must be made of an electrically conductive material
- Suitable materials include, but
- the innermost conduit (the sample gas conduit 20 in Figure 1 or the plasma gas
- conduit can be made of any suitable conducting or nonconducting material, including,
- Ceramic materials are useful as acous mixtures or alloys thereof, or quartz or ceramic materials. Ceramic materials are useful as acous mixtures or alloys thereof, or quartz or ceramic materials. Ceramic materials are useful as acous mixtures or alloys thereof, or quartz or ceramic materials. Ceramic materials are useful as acous mixtures or alloys thereof, or quartz or ceramic materials. Ceramic materials are useful
- argon include, but are not limited to, argon, helium, nitrogen, or air, depending upon the sensitivity of monitoring needed and upon which analytes are being monitored in the
- argon is generally
- the plasma gas can be pumped through the plasma gas conduit inlet 36 into the
- the plasma 'gas is introduced into the plasma gas conduit 30 from a
- one hole (not shown) near the base of the sample gas conduit 20 can be used to allow a
- sample gas pressure if greater than the sample gas pressure, can be used to accomplish intermingling of the plasma gas with the sample gas. Otherwise, pressure of the sample
- conduit 20 by a Venturi effect.
- a collar 40 of electrically conductive material is positioned
- One or more refractory spacers are positioned between
- the collar 40 needs to be close enough to the
- reflector 42 is moveably, or more particularly, slidably, connected to the plasma gas
- the conductance tube between the collar 40 and the microwave reflector 42 can be any conductance tube between the collar 40 and the microwave reflector 42.
- the torch can be operated successfully with a conductance tube length equal to
- One-quarter wavelength conductance tube lengths are presently preferred for enabling smaller
- microwave reflector 42 Any suitable device or method can be used to move the microwave reflector 42
- a microwave transmitter 48 through which microwave energy can be transmitted
- the microwave transmitter 48 can be either a coaxial cable, waveguide, or other
- microwave' source which can provide microwave energy in the
- sources include, but are not limited to, microwave oscillators, magnetrons, or klystron
- microwave source Presently preferred as a microwave source is a magnetron because of the
- the invention apparatus can be operated using low levels of microwave energy
- source can be operated in pulsed or continuous wave mode. Energy levels in the range from about 20 to about 300 Watts can be used. Generally presently preferred are energy
- An electrical semiconductor cooling chip or other suitable cooling device can be any suitable cooling device.
- Microwaves in the range from about 1000 MHz to about 10,000 MHz can be used
- microwaves in the range from
- the plasma is initiated by contact of the plasma gas in the plasma region 16 with
- plasma can be accomplished by any suitable means such as contacting the plasma gas in
- the plasma region 16 with energy from a tesla coil, a laser, UV radiation, or an electrical
- the plasma initiator 54 has connected thereto an initiator energy
- conductor can be simply an electrically conductive wire, or any other suitable means of
- the plasma region j_6 is generally in a naturally occurring flame shape or toroidal
- microwave energy is highly focused there.
- a chimney 58 may be used to shield the plasma region _16 from air currents or
- the chimney 58 may be made of any material
- the chimney may be made of
- quartz, glass or gallium can be used to shield the metal screen
- the light in the plasma region J_6 is focused and collected by any suitable
- focusing lenses optical filters, waveguides, and/or optical fibers can be employed.
- optical filters optical filters, waveguides, and/or optical fibers
- a collimating lens can be used to direct light from a side-on view of the plasma region into an optical fiber.
- Any of several types of transmitter can be used to transmit signals from the
- analytical equipment are focusing lens and fiber optic lines.
- a light pipe Alternatively, a light pipe
- a single signal transmitting line is usually sufficient, particularly when sampling
- a plurality of transmission lines or other devices for transmission are provided.
- the light from the plasma region 16 is analyzed by any suitable means, depending on
- CCD CCD
- mass spectrometer Generally presently preferred when analyzing
- CCD detector or a monochronometer with a photomultiplier tube detector.
- element pixels is used for instantaneous measurements of analyte signals.
- resistance also could be used for signal analysis.
- instruments 60, 62, and 64 receive signals from the plasma region 16 through three fiber
- optic lines 66, 68, and 70 which each have one end proximate to the quartz glass chimney
- each of the signal transmitting lines are positioned proximate to
- Portable computing devices are
- sampling frequency DAQ-700 card can be used to show a real time spectrum on its screen
- a CBL-2-NI interface cable can be used to make a connection between
- the invention device can be operated continuously for as long a period of time as
- Any suitable carrier gas which is stable in monoatomic form and has potential for the plasma is any suitable carrier gas which is stable in monoatomic form and has potential for the plasma.
- argon, helium, neon, xenon and krypton can be used.
- diatomic nitrogen can also be used as the carrier gas.
- a mixture of different carrier gases can also be used as the carrier gas.
- sample gas introduction of the sample gas into the sample gas conduit.
- carrier gas selected will depend upon the plasma gas used, analyte concentration, and the
- a centermost first conduit 100 transports plasma gas to the center 102 of a plasma
- sample gas conduit 106 positioned with respect to the centermost first conduit 100 so as to form an anulus 108 between the first conduit 100 and the second (sample gas) conduit 106.
- conduit 106 is generally longer than the centermost, first conduit HX), with the end of the
- carrying plasma gas can have a plurality of openings 109 arranged about the
- the second (sample gas) conduit 106 is in turn surrounded by a third (plasma)
- conduit 110 which is larger in diameter than the second conduit 106 and coaxially
- third conduit 110 is generally the same length as the second conduit 106 so that the upper
- a second portion of plasma gas is
- the triple-conduit plasma torch 1 18 of this embodiment of the invention can be
- inventions are set up and operated. Any suitable conventional microwave power
- a microwave source 120 is connected to a conductive collar 122 using a microwave transmitter 124 or
- the conductive collar 122 is positioned on the outer wall of
- the sample gas conduit 106 is not
- Microwaves from the microwave power source 120 are reflected by a
- microwave reflector 126 located near the lower end of the three conduits at a distance
- the microwave reflector 126 is
- Instrumentation L36 for analyzing signals from the plasma region JO4 is
- a sample portion of the liquid is nebulized and/or desolvated to
- the aerosol or gas sample is obtained.
- the aerosol or gas sample is obtained.
- FIG. 3 is a flow chart for one particular example of use of the invention to
- nebulizers or from streams are transported into a nebulizer using a peristaltic or other suitable pump
- the liquid sample is first nebulized in any convenient nebulizer
- the ultrasonic nebulizer can be any suitable ultrasonic nebulizer to produce an aerosol.
- the ultrasonic nebulizer can be
- the aerosol is desolvated in a two-step desolvation process with
- the sample is then transported to the plasma torch which is configured and
- the nebulized sample can be transported with a carrier gas directly to the
- plasma gas is combined with the nebulized sample as a carrier gas prior to further drying
- the invention device is portable and can be operated in a continuous operation
- Carrier gases although not necessary for air monitoring, can be used as needed
- samples which can be air or gas samples, including aerosols, and airborne
- Low power microwave plasmas can be used.
- the invention instrument is less complex than other presently used air monitoring
- metals rare earth elements, actinides, and alkali and alkaline earth elements.
Landscapes
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2001241527A AU2001241527A1 (en) | 2000-03-02 | 2001-02-15 | Microwave plasma monitoring system for real-time elemental analysis |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US18642800P | 2000-03-02 | 2000-03-02 | |
US60/186,428 | 2000-03-02 | ||
US09/580,100 US6429935B1 (en) | 2000-03-02 | 2000-05-26 | Microwave plasma monitoring system for real-time elemental analysis |
US09/580,100 | 2000-05-26 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2001065244A1 WO2001065244A1 (en) | 2001-09-07 |
WO2001065244A9 true WO2001065244A9 (en) | 2002-10-17 |
Family
ID=26882078
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2001/005092 WO2001065244A1 (en) | 2000-03-02 | 2001-02-15 | Microwave plasma monitoring system for real-time elemental analysis |
Country Status (2)
Country | Link |
---|---|
AU (1) | AU2001241527A1 (en) |
WO (1) | WO2001065244A1 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104792768B (en) * | 2015-04-25 | 2017-07-25 | 浙江大学 | Solid sample direct injected device for microwave plasma torch spectrometer |
CN116936329B (en) * | 2023-09-15 | 2023-12-15 | 武汉市飞瓴光电科技有限公司 | Normal pressure microwave plasma double waveguide coupling device |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5671045A (en) * | 1993-10-22 | 1997-09-23 | Masachusetts Institute Of Technology | Microwave plasma monitoring system for the elemental composition analysis of high temperature process streams |
-
2001
- 2001-02-15 WO PCT/US2001/005092 patent/WO2001065244A1/en active Application Filing
- 2001-02-15 AU AU2001241527A patent/AU2001241527A1/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
AU2001241527A1 (en) | 2001-09-12 |
WO2001065244A1 (en) | 2001-09-07 |
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