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US4281246A Expired / Lapsed US ⏱️ 0.0 years remaining

Continuous-flow solution concentrator and liquid chromatograph/mass spectrometer interface and methods for using both

Assignee: Environmental Protection Agency
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Filing: 1979-10-12
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Granted: 1981-07-28
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Expires: 1999-10-12
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Abstract

Abstract An interface between a liquid chromatograph and a mass spectrometer is provided for conducting a liquid stream from the chromatograph to the spectrometer. The stream passes from the chromatograph continuously along a tapered concentrator wire toward the narrow end of the wire. The stream is heated in order to evaporate solvent therefrom and to increase the concentration of the solute therein. When the stream reaches the narrow end of the wire, the vacuum created by the mass spectrometer draws the stream through an elongated capillary tube which has a pointed carrier wire positioned therein. A gap is provided in the tube where the tube and the carrier wire intersect the concentrator wire. The capillary tube is either formed with a reduced diameter at one end adjacent the spectrometer or the carrier wire has a ball of solder at that end in order to partially restrict the flow through the tube. The carrier wire is longitudinally moveable within the tube in order to control the flow of material into the spectrometer. Other uses for the tapered and heated wires are contemplated for removing solvent from a liquid stream in order to diminish the stream's flow rate or to increase the concentration of the solute of such a stream. Methods for conducting liquid from a liquid chromatograph to a mass spectrometer and for removing solvent from a liquid stream are also disclosed.

Inventors

  • 👤 V Edward White
  • 👤 Harry S. Hertz
  • 👤 Richard G. Christensen

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-24 23:01
CPC Classifications
H; H01; H01J; H01J49/00; H01J49/02; H01J49/04; H01J49/0431; G; G01; G01N; G01N30/00; G01N30/02; G01N30/62; G01N30/72; G01N30/7233; H01J49/0468; H01J49/049

Claims Analysis

Total Claims: 40
Claim 1
Independent Claim 101 words
An interface between a liquid chromatograph and a mass spectrometer for introducing a liquid stream from the chromatograph into the spectrometer, wherein said interface comprises: (a) a tapered wire having a first end and a second end, the tapered wire adapted to carry said stream from said chromatograph; (b) means for providing heat to the stream in order to cause part of the liquid stream to turn into vapor; (c) means for drawing said stream from adjacent said second wire end towards said spectrometer; and (d) means for conducting said stream from adjacent said second wire end into said mass spectrometer.
Claim 2
Dependent Claim 101 words
An interface between a liquid chromatograph and a mass spectrometer for introducing a liquid stream from the chromatograph into the spectrometer, wherein said interface comprises: (a) a tapered wire having a first end and a second end, the tapered wire adapted to carry said stream from said chromatograph; (b) means for providing heat to the stream in order to cause part of the liquid stream to turn into vapor; (c) means for drawing said stream from adjacent said second wire end towards said spectrometer; and (d) means for conducting said stream from adjacent said second wire end into said mass spectrometer.
Claim 3
Dependent Claim 38 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 1 wherein said tapered wire decreases from a relatively wide diameter at said first end to a relatively narrow diameter at said second end.
Claim 4
Dependent Claim 39 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 2 wherein said heating means provides more heat at a relatively wide part of the wire than at a relatively narrow part of the wire.
Claim 5
Dependent Claim 33 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 1 wherein said means for providing heat to said stream comprises means for passing electric current through said wire.
Claim 6
Dependent Claim 29 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 1 wherein said tapered wire comprises a plurality of materials each having a different diameter.
Claim 7
Dependent Claim 24 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 5 wherein said materials comprise stainless steel, constantan and copper.
Claim 8
Dependent Claim 39 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 1 wherein said tapered wire is surrounded by a glass container and a flow of gas is provided for purging said vapor from said container.
Claim 9
Dependent Claim 23 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 1 wherein said conducting means comprises a capillary tube.
Claim 10
Dependent Claim 32 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 8 wherein said capillary tube has a gap at the point at which it crosses said tapered wire.
Claim 11
Dependent Claim 35 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 9 wherein said capillary tube has a reduced diameter at one end thereof, said end being adjacent to said mass spectrometer.
Claim 12
Dependent Claim 35 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 8 wherein a flow control carrier wire is situated within the tube and partially occludes the tube at one end thereof.
Claim 13
Dependent Claim 28 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 11 further including means for moving said flow control wire longitudinally within said tube.
Claim 14
Dependent Claim 43 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 11 wherein said carrier wire has a ball of solder on one end thereof adjacent to said one tube end, said ball serving to partially constrict said tube end.
Claim 15
Dependent Claim 31 words
An interface between a liquid chromatograph and a mass spectrometer in accordance with claim 1 further including means for sensing the flow rate of said stream adjacent said second wire end.
Claim 16
Independent Claim 84 words
A method of conducting a liquid stream from a liquid chromatograph and introducing the stream into a mass spectrometer, said method comprising: (a) transporting a liquid stream from one end of a tapered wire to the other end of said wire; (b) heating said stream so as to evaporate a portion of said solvent from said liquid stream; and (c) drawing and conducting said liquid stream from adjacent said second end of said wire along the inside of a tube towards said mass spectrometer.
Claim 17
Independent Claim 84 words
A method of conducting a liquid stream from a liquid chromatograph and introducing the stream into a mass spectrometer, said method comprising: (a) transporting a liquid stream from one end of a tapered wire to the other end of said wire; (b) heating said stream so as to evaporate a portion of said solvent from said liquid stream; and (c) drawing and conducting said liquid stream from adjacent said second end of said wire along the inside of a tube towards said mass spectrometer.
Claim 18
Dependent Claim 32 words
A method of conducting a liquid stream in accordance with claim 15 wherein said first wire end has a relatively wide diameter and said second wire end has a relatively narrow diameter.
Claim 19
Dependent Claim 36 words
A method of conducting a liquid stream in accordance with claim 15 wherein said solvent portion is converted into a vapor which is purged from a container surrounding said wire by a flow of purging gas.
Claim 20
Dependent Claim 31 words
A method of conducting a liquid stream in accordance with claim 15 which comprises conducting and drawing said liquid through said tube by a high vacuum created by said mass spectrometer.
Claim 21
Dependent Claim 31 words
A method of conducting a liquid stream in accordance with claim 18 further comprising controlling the flow of said liquid being drawn by a longitudinally moving pointed wire within said tube.
Claim 22
Dependent Claim 31 words
A method of conducting a liquid stream in accordance with claim 15 wherein said tube has a ball of solder on one end thereof adjacent to one end of said tube.
Claim 23
Dependent Claim 31 words
A method of conducting a liquid stream in accordance with claim 15 wherein said liquid stream is drawn from said tapered wire where said wire intersects a gap in said tube.
Claim 24
Dependent Claim 45 words
A method for conducting a liquid stream in accordance with claim 15 which comprises heating said wire proportionally to its diameter whereby more heat is provided to a relatively wide portion of the wire and less heat is provided to a relatively narrow portion thereof.
Claim 25
Dependent Claim 21 words
A method for conducting a liquid stream in accordance with claim 15 comprising heating said wire by passing electric current therethrough.
Claim 26
Dependent Claim 25 words
A method for conducting a liquid stream in accordance with claim 15 further comprising maintaining said liquid stream in a continuous condition about said wire.
Claim 27
Dependent Claim 103 words
A continuous-flow solution concentrator for removing solvent from a liquid stream which comprises: (a) a tapered wire for transporting said liquid stream, said wire decreasing from a first end having a relatively wide diameter to a second end having a relatively narrower diameter; (b) means for providing heat to the stream such that more heat is provided to a portion of the stream at a relatively wide part of the wire than to a portion of the stream at a relatively narrow part of the wire, said heating means vaporizing a portion of the liquid stream; and (c) a container surrounding said wire.
Claim 28
Dependent Claim 103 words
A continuous-flow solution concentrator for removing solvent from a liquid stream which comprises: (a) a tapered wire for transporting said liquid stream, said wire decreasing from a first end having a relatively wide diameter to a second end having a relatively narrower diameter; (b) means for providing heat to the stream such that more heat is provided to a portion of the stream at a relatively wide part of the wire than to a portion of the stream at a relatively narrow part of the wire, said heating means vaporizing a portion of the liquid stream; and (c) a container surrounding said wire.
Claim 29
Dependent Claim 19 words
A continuous-flow solution concentrator in accordance with claim 25 further comprising means for purging the vapor from said container.
Claim 30
Dependent Claim 26 words
A continuous-flow solution concentrator in accordance with claim 25 wherein said tapered wire is comprised of a plurality of different materials each having a different diameter.
Claim 31
Dependent Claim 18 words
A continuous-flow solution concentrator in accordance with claim 25 wherein said materials comprise stainless steel, constantan and copper.
Claim 32
Dependent Claim 25 words
A continuous-flow solution concentrator in accordance with claim 25 wherein said container is a glass envelope and said sweeping means comprises a flow of gas.
Claim 33
Dependent Claim 22 words
A continuous-flow solution concentrator in accordance with 25 wherein said heating means comprises means for passing an electric current through said wire.
Claim 34
Dependent Claim 22 words
A continuous-flow solution concentrator in accordance with 25 wherein said heating means comprises means for passing an electric current through said wire.
Claim 35
Independent Claim 108 words
A method for removing solvent from a continuously flowing liquid stream which comprises: (a) conducting said liquid stream along a tapered wire which decreases in diameter from a relatively wide diameter at one end to a relatively narrow diameter at its second end; (b) providing heat to said stream in order to heat said stream and convert a portion of said stream into vapor, whereby more heat is provided to a portion of the stream at a relatively wide portion of the wire than to a portion of the stream at a relatively narrow portion thereof; and (c) sweeping the vapors from a container positioned around said wire.
Claim 36
Independent Claim 108 words
A method for removing solvent from a continuously flowing liquid stream which comprises: (a) conducting said liquid stream along a tapered wire which decreases in diameter from a relatively wide diameter at one end to a relatively narrow diameter at its second end; (b) providing heat to said stream in order to heat said stream and convert a portion of said stream into vapor, whereby more heat is provided to a portion of the stream at a relatively wide portion of the wire than to a portion of the stream at a relatively narrow portion thereof; and (c) sweeping the vapors from a container positioned around said wire.
Claim 37
Dependent Claim 26 words
A method for removing solvent from a liquid stream in accordance with claim 31 comprising sweeping said vapors from said container by flowing purge gas therethrough.
Claim 38
Dependent Claim 20 words
A method for removing solvent from a liquid stream in accordance with claim 31 wherein said purge gas is nitrogen.
Claim 39
Dependent Claim 24 words
A method for removing solvent from a liquid stream in accordance with claim 31 comprising heating said wire by passing an electric current therethrough.
Claim 40
Dependent Claim 27 words
A method for removing solvent from a liquid stream in accordance with claim 31 further comprising maintaining said liquid stream in a continuous condition about said wire.

References Cited (Backward Citations)

US2601097A Cited
US3080746A Cited
US3929004A Cited
US3896661A Cited
US3997298A Cited
US4055987A Cited
US4112297A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-07-27 1985-01-26 1985-07-28 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-07-27 1989-01-26 1989-07-28 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-07-27 1993-01-26 1993-07-28 $7700.00 Window Closed / Lapsed

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