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US4861988A Expired / Lapsed US ⏱️ 0.0 years remaining

Ion spray apparatus and method

Assignee: Cornell Research Foundation Inc
•
Filing: 1987-09-30
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Granted: 1989-08-29
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Expires: 2007-09-30
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Abstract

Abstract A device for interfacing between a microbore liquid chromatograph and a mass analyser. In such a device, liquid from the liquid chromatograph is sprayed through a stainless steel capillary tube into the atmospheric pressure ionization chamber of a mass spectrometer. A voltage of e.g., plus or minus 3 KV is applied to the stainless steel tube, and a nebulizing gas, e.g. nitrogen, is directed at high velocity past the tube tip through another tube encircling the stainless steel tube. The combination of the nebulizing gas and the electric potential disperses the liquid at room temperature into a fine mist providing an increased and more stable ion signal without thermal decomposition of the compounds being analysed.

Inventors

  • 👤 John D. Henion
  • 👤 Thomas R. Covey
  • 👤 Andries P. Bruins

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 19:47
CPC Classifications
H; H01; H01J; H01J49/00; H01J49/02; H01J49/10; H01J49/16; H01J49/165; H01J49/167; G; G01; G01N; G01N30/00; G01N30/02; G01N30/62; G01N30/72; G01N30/7233; G01N30/724; G01N30/7246; G01N30/7266; H01J49/04; H01J49/0431; H01J49/0445; G01N30/7293

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 269 words
Apparatus for analyzing ions from trace sample molecules in a liquid comprising: (a) a chamber, (b) an inner capillary tube to receive said liquid and having a first free end in said chamber for discharging said liquid into said chamber, (c) an outer tube encircling said inner capillary tube and defining therewith an annular space therebetween, said outer tube having a second free end located substantially at said first free end, said second free end therefore also being in said chamber, (d) means for directing a flow of gas through said annular space for said gas to flow over said first free and into said chamber at a velocity of substantially at least 50 meters per second, (e) an orifice plate having an orifice therein, said tubes being located on one side of said orifice plate with said free ends spaced therefrom, said orifice defining an outlet from said chamber, (f) a mass analyser on the other side of said orifice plate, outside said chamber, for receiving ions passing through said orifice plate, (g) means for providing the pressure in said chamber to be substantially atmospheric pressure, and the temperature in said inner tube and in said chamber being sufficiently low to avoid thermal decomposition of said trace sample molecules, (h) means for creating an electric field between said first free end and said orifice plate, wherein the combination of said electric field and said gas flow past said free end of said inner capillary tube produces a mist of fine charged droplets of said liquid, and wherein said charged droplets evaporate in said chamber and release ions therefrom.
Claim 2
Dependent Claim 269 words
Apparatus for analyzing ions from trace sample molecules in a liquid comprising: (a) a chamber, (b) an inner capillary tube to receive said liquid and having a first free end in said chamber for discharging said liquid into said chamber, (c) an outer tube encircling said inner capillary tube and defining therewith an annular space therebetween, said outer tube having a second free end located substantially at said first free end, said second free end therefore also being in said chamber, (d) means for directing a flow of gas through said annular space for said gas to flow over said first free and into said chamber at a velocity of substantially at least 50 meters per second, (e) an orifice plate having an orifice therein, said tubes being located on one side of said orifice plate with said free ends spaced therefrom, said orifice defining an outlet from said chamber, (f) a mass analyser on the other side of said orifice plate, outside said chamber, for receiving ions passing through said orifice plate, (g) means for providing the pressure in said chamber to be substantially atmospheric pressure, and the temperature in said inner tube and in said chamber being sufficiently low to avoid thermal decomposition of said trace sample molecules, (h) means for creating an electric field between said first free end and said orifice plate, wherein the combination of said electric field and said gas flow past said free end of said inner capillary tube produces a mist of fine charged droplets of said liquid, and wherein said charged droplets evaporate in said chamber and release ions therefrom.
Claim 3
Dependent Claim 16 words
Apparatus according to claim 1 wherein said inner tube is formed from an electrically conductive material.
Claim 4
Dependent Claim 33 words
Apparatus according to claim 2 wherein said inner tube is a stainless steel tube and said means for generating said electrical field includes means for applying a potential to said stainless steel tube.
Claim 5
Dependent Claim 23 words
Apparatus according to claim 2 wherein the inner diameter of said inner tube is of the order of between 0.05 and 0.15 millimeters.
Claim 6
Dependent Claim 20 words
Apparatus according to claim 4 wherein the inner diameter of said inner tube is of the order of 0.1 millimeters.
Claim 7
Dependent Claim 19 words
Apparatus according to claim 2 wherein the thickness of said annular space is of the order of 0.075 millimeters.
Claim 8
Dependent Claim 31 words
Apparatus according to claim 2 wherein said means for directing said flow of gas includes a source of pressurized gas, the pressure of said gas being between 2 and 3 bar.
Claim 9
Dependent Claim 54 words
Apparatus according to claim 2 and including a liquid chromatograph for supplying said liquid, said liquid chromatograph having an outlet tube for said liquid flowing therefrom, said outlet tube being of an insulating material and being connected to said inner tube for said inner tube to receive the entire flow from said liquid chromatograph.
Claim 10
Dependent Claim 10 words
Apparatus according to claim 8 wherein said gas is nitrogen.
Claim 11
Dependent Claim 17 words
Apparatus according to claim 2 wherein said first free end extends slightly beyond said second free end.
Claim 12
Dependent Claim 29 words
Apparatus according to claim 2 wherein said means (d) includes means for producing a gas velocity of between about 78 and 250 meters per second through said annular space.
Claim 13
Dependent Claim 29 words
Apparatus according to claim 2 wherein said means (d) includes means for producing a gas velocity of between about 140 and 250 meters per second through said annular space.
Claim 14
Independent Claim 166 words
A method of analyzing ions from trace sample molecules in a liquid, comprising: (a) directing said liquid through a conductive capillary tube having a free end in a chamber, (b) directing an annular jet of gas having a velocity of at least 50 meters per second past said free end in the direction of flow of said liquid, (c) maintaining the pressure in said chamber at substantially atmospheric pressure and maintaining the temperature in said tube and in said chamber sufficiently low to avoid thermal decomposition of said trace sample molecules, (d) generating an electric field in said chamber between said free end and an orifice plate for said ions, the combination of said jet of gas and said electric field acting to produce a mist of charged droplets and to produce ions in said chamber from said droplets, (e) and guiding ions out of said chamber through an orifice in said orifice plate, into a mass analyzer located outside said chamber beyond said orifice plate.
Claim 15
Independent Claim 166 words
A method of analyzing ions from trace sample molecules in a liquid, comprising: (a) directing said liquid through a conductive capillary tube having a free end in a chamber, (b) directing an annular jet of gas having a velocity of at least 50 meters per second past said free end in the direction of flow of said liquid, (c) maintaining the pressure in said chamber at substantially atmospheric pressure and maintaining the temperature in said tube and in said chamber sufficiently low to avoid thermal decomposition of said trace sample molecules, (d) generating an electric field in said chamber between said free end and an orifice plate for said ions, the combination of said jet of gas and said electric field acting to produce a mist of charged droplets and to produce ions in said chamber from said droplets, (e) and guiding ions out of said chamber through an orifice in said orifice plate, into a mass analyzer located outside said chamber beyond said orifice plate.
Claim 16
Dependent Claim 26 words
The method according to claim 13 wherein the velocity of said jet of gas is in the range between about 78 and 250 meters per second.
Claim 17
Dependent Claim 26 words
The method according to claim 13 wherein the velocity of said jet of gas is in the range between about 140 and 250 meters per second.
Claim 18
Dependent Claim 11 words
The method according to claim 13 wherein said gas is nitrogen.
Claim 19
Dependent Claim 29 words
The method according to claim 13 and including the step of pre-separating components of said liquid in a liquid chromatograph prior to directing said liquid through said capillary tube.

References Cited (Backward Citations)

US4160161A Cited
US4298795A Cited
US4531056A Cited
US4730111A Cited
US4607163A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-08-28 1993-02-27 1993-08-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-08-28 1997-02-27 1997-08-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-08-28 2001-02-27 2001-08-29 $7700.00 Window Closed / Lapsed

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