US4982097A
Expired / Lapsed
US
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Vaporization device for continuous introduction of liquids into a mass spectrometer
Assignee: Battelle Memorial Institute Inc
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Filing: 1989-05-19
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Granted: 1991-01-01
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Expires: 2009-05-19
Abstract
Abstract This invention is designed to serve as an interface between a liquid chromatograph and a conventional or tandem mass spectrometer (LC/MS, LC/MS/MS). It may also be used for liquid sampling without prior separation of analytes by a liquid chromatograph. This invention differs from prior art in that vaporization of the analytical sample (LC eluent) occurs through the action of condensing pressurized steam on the exterior of a low thermal mass metal capillary, while the aqueous LC eluent is flowing through the metal capillary. The steam is obtained by heating a small volume of water sealed within the device. LC eluent entering the capillary results in localized cooling and subsequent condensation of the pressurized steam on the outer surface of the capillary. The process of condensation deposits energy to the capillary equivalent to the latent heat of vaporization of water. This energy results in flash vaporization of the LC eluent within the capillary. Condensed water flows along the outer wall of the metal capillary where it is returned to the trapped liquid reservoir for re-vaporization. Energy coupling to the LC eluent is substantially more efficient than methods used in prior art interface devices. This invention minimizes overheating of temperature sensitive analytes separated by the LC and rapidly self compensates for changes in eluent flow or eluent composition without the need for adjustment in operating temperature. This invention eliminates the need for aerosol desolvation prior to ionization.
Inventors
- 👤 Laurence E. Slivon
- 👤 Donald V. Kenny
- 👤 Richard A. Severance
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 13:41
CPC Classifications
H; H01; H01J; H01J49/00; H01J49/02; H01J49/04; H01J49/0431; H01J49/0404; H01J49/0468; H01J49/049; G; G01; G01N; G01N1/00; G01N1/02; G01N1/22; G01N30/00; G01N30/02; G01N30/26; G01N30/28; G01N30/30; G01N2030/3038; G01N30/62; G01N30/72; G01N30/7233; G01N30/724; G01N30/7253
Claims Analysis
Total Claims: 32
Claim 1
Independent Claim
89 words
An apparatus for use in a mass spectrometry system which vaporizes an eluent passing therethrough comprising: a. first heating means; b. fluid heat transfer means for transferring heat from the heating means to the eluent; c. means for transferring the eluent into and vapor out of the heat transfer means; and wherein a working fluid in the heat transfer means is converted from a liquid to a gas by the heating means and transfers energy to the eluent as the working fluid changes from a gas to a liquid.
Claim 2
Independent Claim
89 words
An apparatus for use in a mass spectrometry system which vaporizes an eluent passing therethrough comprising: a. first heating means; b. fluid heat transfer means for transferring heat from the heating means to the eluent; c. means for transferring the eluent into and vapor out of the heat transfer means; and wherein a working fluid in the heat transfer means is converted from a liquid to a gas by the heating means and transfers energy to the eluent as the working fluid changes from a gas to a liquid.
Claim 3
Dependent Claim
17 words
The apparatus of claim 1 further comprising control means for controlling the temperature of the heating means.
Claim 4
Dependent Claim
17 words
The apparatus of claim 1 wherein the working fluid has a heat of vaporization above 200 calories/gram.
Claim 5
Dependent Claim
11 words
The apparatus of claim 1 wherein the working fluid is water.
Claim 6
Dependent Claim
17 words
The apparatus of claim 1 wherein the working fluid is a mixture of water and a surfactant.
Claim 7
Dependent Claim
23 words
The apparatus of claim 1 wherein the fluid heat transfer means comprises a chamber partially filled with working fluid in the liquid phase.
Claim 8
Dependent Claim
15 words
The apparatus of claim 1 wherein the means for transferring the eluent comprises a capillary.
Claim 9
Independent Claim
13 words
The apparatus of claim wherein the first heating means comprises a resistance wire.
Claim 10
Dependent Claim
28 words
The apparatus of claim 2 wherein the control means comprises a temperature controller attached to the thermocouple that controls a relay that controls power to the heating means.
Claim 11
Dependent Claim
10 words
The apparatus of claim 1 further comprising temperature sensing means.
Claim 12
Independent Claim
100 words
An apparatus for vaporizing and introducing a vaporized eluent into a spectrometer comprising: a. a capillary tube having a first end and a second end; b. a working fluid surrounding the capillary tube between the first and second ends; c. means for permanently containing the working fluid around the capillary tube, wherein the means for containing the working fluid around the capillary tube comprises a wall in sealed relationship with the outer surface of the first and second ends of the capillary that defines a chamber containing the working fluid; and d. means for providing heat to the working fluid.
Claim 13
Independent Claim
100 words
An apparatus for vaporizing and introducing a vaporized eluent into a spectrometer comprising: a. a capillary tube having a first end and a second end; b. a working fluid surrounding the capillary tube between the first and second ends; c. means for permanently containing the working fluid around the capillary tube, wherein the means for containing the working fluid around the capillary tube comprises a wall in sealed relationship with the outer surface of the first and second ends of the capillary that defines a chamber containing the working fluid; and d. means for providing heat to the working fluid.
Claim 14
Dependent Claim
17 words
The apparatus of claim 11 further providing control means for controlling the temperature of the working fluid.
Claim 15
Dependent Claim
17 words
The apparatus of claim 11 wherein the working fluid has a heat of vaporization above 200 calories/gram.
Claim 16
Dependent Claim
11 words
The apparatus of claim 11 wherein the working fluid is water.
Claim 17
Dependent Claim
17 words
The apparatus of claim 11 wherein the working fluid is a mixture of water and a surfactant.
Claim 18
Dependent Claim
13 words
The apparatus of claim 11 wherein the capillary and wall are of nickel.
Claim 19
Dependent Claim
12 words
The apparatus of claim 11 wherein the wall has an outer sheath.
Claim 20
Dependent Claim
10 words
The apparatus of claim 17 wherein the sheath is copper.
Claim 21
Dependent Claim
10 words
The apparatus of claim 11 further comprising temperature sensing means.
Claim 22
Dependent Claim
139 words
Apparatus for vaporizing an eluent to be introduced into a mass spectrometer comprising: a. a capillary tube having inlet and outlet ends through which the eluent may flow, the capillary tube passing through a chamber having a metal wall disposed coaxially about the capillary and sealing means at the input and output ends sealingly disposed between the metal wall and an outer wall of the capillary tube to form a sealed coaxial chamber about the capillary; b. a working fluid within the chamber that is in both the liquid and gas phases and the liquid phase fills only a portion of the chamber; c. heating means disposed to heat the fluid within the chamber; and d. an orifice in axial alignment with the outlet end of the capillary tube whereby a flow of vapor from the capillary is maintained.
Claim 23
Dependent Claim
139 words
Apparatus for vaporizing an eluent to be introduced into a mass spectrometer comprising: a. a capillary tube having inlet and outlet ends through which the eluent may flow, the capillary tube passing through a chamber having a metal wall disposed coaxially about the capillary and sealing means at the input and output ends sealingly disposed between the metal wall and an outer wall of the capillary tube to form a sealed coaxial chamber about the capillary; b. a working fluid within the chamber that is in both the liquid and gas phases and the liquid phase fills only a portion of the chamber; c. heating means disposed to heat the fluid within the chamber; and d. an orifice in axial alignment with the outlet end of the capillary tube whereby a flow of vapor from the capillary is maintained.
Claim 24
Dependent Claim
17 words
The apparatus of claim 20 further comprising control means for controlling the temperature of the heating means.
Claim 25
Dependent Claim
17 words
The apparatus of claim 20 wherein the working fluid has a heat of vaporization above 200 calories/gram.
Claim 26
Dependent Claim
11 words
The apparatus of claim 20 wherein the working fluid is water.
Claim 27
Dependent Claim
17 words
The apparatus of claim 20 wherein the working fluid is a mixture of water and a surfactant.
Claim 28
Dependent Claim
17 words
The apparatus of claim 20 further comprising a sheath of metal axially disposed about the metal wall.
Claim 29
Dependent Claim
30 words
The apparatus of claim 25 wherein the capillary consists of nickel, stainless steel, or gold; the metal wall consists of nickel or stainless steel; and the sheath consists of copper.
Claim 30
Dependent Claim
10 words
The apparatus of claim 21 further comprising temperature sensing means.
Claim 31
Dependent Claim
67 words
A process for vaporizing an eluent for introduction into a mass spectrometer comprising: a. heating a working fluid in a sealed chamber so as to vaporize at least a portion of the fluid; and b. transferring energy to the eluent in a manner adapted to vaporize the eluent by heat transfer from the vaporized working fluid as the working fluid changes from a gas to a liquid.
Claim 32
Dependent Claim
67 words
A process for vaporizing an eluent for introduction into a mass spectrometer comprising: a. heating a working fluid in a sealed chamber so as to vaporize at least a portion of the fluid; and b. transferring energy to the eluent in a manner adapted to vaporize the eluent by heat transfer from the vaporized working fluid as the working fluid changes from a gas to a liquid.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1993-12-31 | 1994-07-02 | 1995-01-01 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-12-31 | 1998-07-02 | 1999-01-01 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-12-31 | 2002-07-02 | 2003-01-01 | $7700.00 | Window Closed / Lapsed |