WO1988006834A2 - Chalumeau hf a injection directe - Google Patents

Chalumeau hf a injection directe Download PDF

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Publication number
WO1988006834A2
WO1988006834A2 PCT/US1988/000741 US8800741W WO8806834A2 WO 1988006834 A2 WO1988006834 A2 WO 1988006834A2 US 8800741 W US8800741 W US 8800741W WO 8806834 A2 WO8806834 A2 WO 8806834A2
Authority
WO
WIPO (PCT)
Prior art keywords
torch
atomizer
analyte
plasma
sample
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1988/000741
Other languages
English (en)
Other versions
WO1988006834A3 (fr
Inventor
Michael David George Rogers
William Buford Henderson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Geochemical Services Inc
Original Assignee
Geochemical Services Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Geochemical Services Inc filed Critical Geochemical Services Inc
Publication of WO1988006834A2 publication Critical patent/WO1988006834A2/fr
Publication of WO1988006834A3 publication Critical patent/WO1988006834A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/26—Plasma torches
    • H05H1/30—Plasma torches using applied electromagnetic fields, e.g. high frequency or microwave energy

Definitions

  • This invention relates generally to a plasma generating apparatus for use in plasma spectroscopy, and more specifically to an improved apparatus having an inductively coupled plasma torch and electrothermal atomizer.
  • ICP inductively coupled plasma
  • prior art ICP spectroscopy systems have typically included an electrothermal atomizer 20 interconnected with a separate ICP torch 30 by means of a long pipe, conduit or similar device 35.
  • the atomizer 20 is composed of a large bell- shaped glass jar 22 which encases a carbon rod heater element 24 extending between two electrodes 26.
  • the glass jar 22 may be lifted, whereupon a sample of analyte may be placed in the heater element 24 and the jar 22 replaced.
  • the analyte is then heated to induce atomization of the analyte.
  • a supply of carrier gas 28 such as argon
  • the mixture flow within the bell jar 22 passes through the pipe or conduit 35 to the ICP torch 30.
  • a conventional ICP torch 30 is typically formed of quartz glass and includes intricate ducting.
  • a main duct 31 is provided into which the analyte mixture flow may pass.
  • An auxiliary duct 32 is also provided through which an auxiliary flow of argon or a similar gas may be introduced within a quartz glass containment wall 34.
  • a coolant duct 33 is provided into which a coolant gas may be introduced.
  • a conventional ICP torch also has a radio frequency (RF) induction coil 36 which is wrapped about the containment wall 34. When energized, the induction coil 36 generates plasma out of the gas introduced through the auxiliary duct 32.
  • RF radio frequency
  • the mixture Upon injection of the analyte mixture from the atomizer 20 into the of main duct, the mixture passes through the injector tip 37 of the torch 30 where it mixes with the plasma. The analyte mixture is thus heated up to the temperature of the plasma, wherein most of the molecules are ionized so that the mixture may be analyzed.
  • Another common prior art spectroscopy system provides for the interconnection of a spray chamber rather than an atomizer to an ICP torch by means of a pipe or conduit similar to the one described above.
  • a liquid analyte then may be placed within the spray chamber where it may be converted into a fine spray for introduction to the ICP torch 30.
  • Prior art conventional ICP spectroscopy systems such as those described above typically suffer from several disadvantages.
  • a myriad of locations exist within the system at which analyte may accumulate as condensation after completion of an analysis. This causes the system to have a "memory" that may cause contamination of subsequent analytes.
  • locations include, but are not limited to, (1) the walls of the atomizer 20; (2) the pipe or conduit 35 interconnecting the atomizer 20 or a spray chamber and the ICP torch 30; (3) the injector tip 37 of the ICP torch 30; and (4) the quartz glass containment wall 34 of the ICP torch 30.
  • a further disadvantage of the above-described systems is the severe signal loss which occurs between the atomizer 20 or spray chamber and the ICP torch 30 as a result of condensation.
  • a further disadvantage of the above-described prior art ICP spectroscopy systems is their inadaptability to robotic sample loading. Vaporization of the analyte typically occurs under sealed glassware. Robotic systems, however, are not typically suited to operate in environments where glassware is encountered.
  • the present invention relates to an ICP spectroscopy apparatus in which an electrothermal atomizer and an ICP torch are integrated as a single unit.
  • the apparatus is constructed using two adjacent annular electrodes through which an annular heater and a sample vessel may be removably inserted.
  • a sample of analyte may be placed in the sample vessel and heated by the electrodes to atomize the analyte.
  • the atomized analyte passes through a plasma nozzle into a plasma chamber portion of the ICP torch.
  • a nebulizer gas jet and a vapor pressure enhancer are passed through the ICP spectroscopy apparatus to increase atomization of the analyte and to ensure maximum transfer of the atomized material into the plasma chamber of the ICP torch.
  • a quartz glass plasma containment wall is provided about the plasma nozzle and is surrounded by a variable rate cooling manifold.
  • a conventional fadio frequency (RF) coil is wrapped about the containment wall and is inductively coupled to
  • An advantage of the present invention is the provision of an ICP torch/atomizer apparatus in which the amount of memory produced during analysis of a sample of analyte is mimimized, as are the number of locations at which memory condensate may accumulate.
  • a further advantage of the present invention is the provision of an ICP torch/atomizer apparatus in which the total volume of analyte passing to the ICP torch is increased, thereby increasing the sensitivity of the apparatus to a sample of analyte.
  • an ICP torch/atomizer apparatus is provided in which an increased number of types of sample materials may be analyzed. It is yet a further advantage of the present invention that an ICP torch/atomizer apparatus is provided which is adaptable to robotic sample loading.
  • an ICP torch/atomizer apparatus is provided to which a conventional spray chamber may be connected.
  • FIGURE 1 is a side plan view of a prior art atomizer/ICP torch configuration.
  • FIGURE 2 is a side cross-sectional plan view of the atomizer/ICP torch apparatus of the present invention.
  • FIG. 2 illustrates the preferred embodiment or the present invention.
  • An integral ICP torch/ electrothermal atomizer apparatus 40 is provided having a torch portion 42 and an electrothermal atomizer portion 44.
  • the electrothermal atomizer portion 44 is composed of a first annular electrode 46, a second annular electrode 48, and a plasma nozzle 49.
  • the first and second annular electrodes are interconnected to one another to form an electrode block 51 which may be removably attached to the plasma nozzle 49.
  • the electrode contains an aperture 53 formed therethrough in which are housed an annular heating element 54 and an annular analytic sample vessel tube 56.
  • the analytic sample vessel tube 56 extends through an aperture 58 in the plasma nozzle 49 and terminates to form an analyte injector tip 62 located immediately adjacent to a plasma chamber 64.
  • a breech block 59 having a sample holder or spoon 55 at one end is removably insertable within the aperture 53.
  • the breech block 59 may be maintained in sealing engagement with the electrode block 51 by means of an 0-ring 61.
  • a nebulizer jet represented schematically by numeral 63 having a vapor pressure enhancer (such as, for example, florine, chlorine, bromine, iodine, oxygen or sulphur) may be removably connected to the electrode block 51 at an aperture 57 formed through the breech block 59.
  • the torch portion 42 of the apparatus 40 contains a cylindrical quartz glass plasma containment wall 70, the interior of which defines the boundary of the plasma chamber 64.
  • the plasma containment wall 70 surrounds a portion 72 of the plazma nozzle 49 such that the analyte injector tip 62 is located immediately adjacent to or within the plasma chamber 64.
  • a cooling manifold 76 is provided through which a coolant gas (such as argon) may be continuously passed in order to prevent melting of the containment wall 70.
  • a radio frequency (RF) coil 71 is provided which surrounds the containment wall 70 in order to allow inductive coupling to the gas passing through the plasma chamber 64.
  • a variable rate cooling manifold 73 having an inlet duct 74 and an outlet duct 78 also surrounds the plasma containment wall 70. By passing a fluid of a preselected temperature through the inlet duct 74, selective heating or cooling of the the exterior of the plasma containment wall 70 may be obtained.
  • integral ICP apparatus 40 Operation of the above described integral ICP apparatus 40 occurs in the following manner.
  • the integral breech block. 59 and sample holder 55 are withdrawn from the atomizer portion 44 by robotic or other means (not shown).
  • An analyte sample is placed within the sample holder 55 and the breech block 59 is replaced within the atomizer portion 44 with the sample holder 55 extending within the sample vessel tube 56.
  • the electrode block 51 is then activated, raising the temperature of the sample vessel tube 56 and sample holder 55 to a point where atomization of the analyte commences.
  • the nebulizer jet 63 (argon in the present example) containing a vapor pressure enhancer is introduced through the aperture 57 of the electrode block 51.
  • the argon gas and the vapor pressure enhancer pass over the heated analyte to ensure that maximum transfer of the atomized analyte occurs from the sample holder 55 through the sample vessel tube 56 into the plasma chamber 64.
  • the RF coil 71 creates a plasma out of the argon coolant gas/vapor pressure enhancer/analyte mixture traveling into the plasma chamber 64. Since the plasma chamber 64 is located immediately adjacent to the analyte injector tip 62 of the sample vessel tube 56, no lengthy surface exists along which analyte may condense.
  • the exterior of the containment wall 70 is heated and condensate is removed by passing a fluid or high temperature through the variable rate cooling manifold 73.
  • the coolant gas flowrate passing through the cooling manifold 76 may also be increased in order to quickly cool the interior of the containment glass wall 70.
  • the present invention is superior to prior art ICP torch/electrothermal atomizer configurations for a variety of reasons.
  • buildup of analyte memory is prevented at virtually all of the locations at which condensate accumulated in prior art systems.
  • the bellshaped atomizer glass 22 is eliminated, and the length of the path between the atomizer and the torch is reduced to a minimum by placing the analyte injector tip 62 of the sample vessel 56 immediately adjacent to the plasma chamber 64.
  • the selected heating and cooling of the containment wall through the use of coolant gas within the boundaries of the containment wall and the heating of the variable rate cooling manifold at the outer surface of the containment wall effectively reduces condensate accumulation at this location.
  • Tests performed with a prototype of this apparatus have in fact produced greater than six orders of magnitude decay in signal between samples when compared to conventional ICP torch/atomizer systems in which decay of approximately three orders of magnitude between samples is common.
  • sample concentrations may be analyzed sequentially without fear that analyte memory from prior analyses will influence the results of subsequent analyses. Less maintenance is therefore required for the system since cleaning of the various elements is not necessary as frequently.
  • additional operating time and better precision in results are obtained.
  • the nebulizer jet 63 and the vapor pressure enhancer dramatically increase the rate at which the atomization of solid analyte occurs. It is therefore possible to atomize and subsequently observe the spectra of analyte which is in solid form, as well as conventional liquids and gases.
  • a conventional spray chamber capable of creating a fine spray of liquid analyte may be used without activation of the electrothermal atomizer portion 44.
  • the conventional spray chamber may be connected to the aperture 57 of the electrode block 51.
  • liquid analyte may be vaporized by the spray chamber and may be passed directly to the torch portion 42 where its spectra may be observed.
  • the ICP torch/atomizer apparatus 40 may thus be adaptable to be used as an ICP torch alone in conjunction with conventional analyte spray chambers.
  • means other than an inductively coupled plasma torch may be used to produce an analyte-bearing plasma, such as a microwave induced or capacatively coupled torch or the like.
  • the plasma may be contained within a predetermined boundary by other than a quartz glass containment wall, such as by magnetic means.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Electromagnetism (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

Dans un appareil de spectroscopie (40) à plasma inductivement couplé, un chalumeau (42) de plasma inductivement couplé et un atomiseur (44) d'échantillons d'analytes forment intégralement une seule unité. La partie d'atomisation de l'appareil comprend deux électrodes (46, 48) et un ajutage (49) de plasma dans lequel est agencé un élément de chauffage (54). Des échantillons d'analyse peuvent être placés dans un récipient (55) d'échantillons situé à l'intérieur de l'élément de chauffage. La partie à chalumeau comprend une paroi (70) de confinement en verre qui entoure au moins une partie de l'ajutage de plasma, définissant une chambre (64) de plasma immédiatement adjacente au récipient d'échantillons. La paroi de confinement en verre contient une bobine (71) de haute-fréquence (HF) enroulée autour de sa périphérie et couplée inductivement à une alimention en gaz. Un distibuteur (74, 76) de refroidissement à vitesse variable est également agencé autour de la périphérie de la paroi de confinement. Cette conception en une seule pièce réduit efficacement l'accumulation de condensés résiduels dans l'appareil, réduisant les risques de contamination et augmentant l'exactitude des résultats obtenus.
PCT/US1988/000741 1987-03-06 1988-03-07 Chalumeau hf a injection directe Ceased WO1988006834A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US2306987A 1987-03-06 1987-03-06
US023,069 1987-03-06

Publications (2)

Publication Number Publication Date
WO1988006834A2 true WO1988006834A2 (fr) 1988-09-07
WO1988006834A3 WO1988006834A3 (fr) 1988-09-22

Family

ID=21812952

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US1988/000741 Ceased WO1988006834A2 (fr) 1987-03-06 1988-03-07 Chalumeau hf a injection directe

Country Status (2)

Country Link
AU (1) AU1708188A (fr)
WO (1) WO1988006834A2 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2652702A1 (fr) * 1989-02-27 1991-04-05 Durr Henri Bruleur a plasma inductif haute frequence, destine au traitement des effluents toxiques ou non.
GB2410830A (en) * 2004-02-06 2005-08-10 Micromass Ltd Ion source for a mass spectrometer
US7265362B2 (en) 2004-02-06 2007-09-04 Micromass Uk Limited Mass spectrometer
US7294841B2 (en) 2004-02-06 2007-11-13 Micromass Uk Limited Mass spectrometer
US8622735B2 (en) * 2005-06-17 2014-01-07 Perkinelmer Health Sciences, Inc. Boost devices and methods of using them
US9686849B2 (en) 2012-07-13 2017-06-20 Perkinelmer Health Sciences, Inc. Torches and methods of using them
US9847217B2 (en) 2005-06-17 2017-12-19 Perkinelmer Health Sciences, Inc. Devices and systems including a boost device

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7511246B2 (en) 2002-12-12 2009-03-31 Perkinelmer Las Inc. Induction device for generating a plasma

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3310742A1 (de) * 1983-03-24 1984-09-27 Siemens AG, 1000 Berlin und 8000 München Plasmabrenner fuer die icp-emissionsspektrometrie

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2652702A1 (fr) * 1989-02-27 1991-04-05 Durr Henri Bruleur a plasma inductif haute frequence, destine au traitement des effluents toxiques ou non.
WO1991016804A1 (fr) * 1989-02-27 1991-10-31 S.A.R.L. Plasma Depollution Bruleur a plasma inductif haute frequence destine au traitement des effluents toxiques ou non au gaz des moteurs a explosion au sechage du papier ou du bois
GB2410830A (en) * 2004-02-06 2005-08-10 Micromass Ltd Ion source for a mass spectrometer
US7265362B2 (en) 2004-02-06 2007-09-04 Micromass Uk Limited Mass spectrometer
US7294841B2 (en) 2004-02-06 2007-11-13 Micromass Uk Limited Mass spectrometer
GB2410830B (en) * 2004-02-06 2008-06-04 Micromass Ltd Mass spectrometer
US8622735B2 (en) * 2005-06-17 2014-01-07 Perkinelmer Health Sciences, Inc. Boost devices and methods of using them
US9847217B2 (en) 2005-06-17 2017-12-19 Perkinelmer Health Sciences, Inc. Devices and systems including a boost device
US9686849B2 (en) 2012-07-13 2017-06-20 Perkinelmer Health Sciences, Inc. Torches and methods of using them

Also Published As

Publication number Publication date
AU1708188A (en) 1988-09-26
WO1988006834A3 (fr) 1988-09-22

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