Patent US4977320A successfully refreshed from Google Patents.
US4977320A
Expired / Lapsed
US
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Electrospray ionization mass spectrometer with new features
Assignee: Rockefeller University
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Filing: 1990-01-22
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Granted: 1990-12-11
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Expires: 2010-01-22
Abstract
Abstract An electrospray ion source is designed for ready and simple plugging into commercial mass analyzers for mass spectrometric analysis of organic molecules. The electrospray is carried out is the ambient air and the ions and other charged species enter the mass analyuzer through a long metal capillary tube and three stages of differential pumping. The use of the long tube allows (a) convenient injection of the ions into the mass analyzer (b) optimization of the spray by direct visualization in the air (c) efficient and controlled heat transfer to the droplets and (d) efficient pumping of the region between the capillary exit and the skinner. Desolvation of the solvated ions is carried out using a combination of controlled heat transfer to the charged droplets during the transit through the tube and collisional activation in a region of reduced pressure. Desolvation with this system does not involve use of a strong countercurrent flow of heated gas. The system also may be used to obtain the collisional activated fragmentation spectra of molecule ions. The use of a metal capillary tube avoids complications from charging that arise from the use of dielectric capilliary tubes.
Inventors
- 👤 Swapan K. Chowdhury
- 👤 Viswanatham Katta
- 👤 Brian T. Chait
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 04:01
CPC Classifications
H; H01; H01J; H01J49/00; H01J49/02; H01J49/04; H01J49/0404; H01J49/0431; H01J49/044; H01J49/0468; H01J49/10; H01J49/16; H01J49/165
Claims Analysis
Total Claims: 28
Claim 1
Independent Claim
221 words
A system for the analysis of the mass spectra of ions comprising; (a) a mass analyzer having an inlet orifice means to receive ions to be analyzed (b) an electrospray ion source connected to said mass analyzer and including; (i) electrospray means to transport a dilute solution of the molecules of interest and to spray charged micron size droplets of the solution; (ii) means to impose a voltage of about 1-10 KV on said electrospray means; (iii) a capillary tube having an entrance orifice positioned across a gap from said electrospray means to receive said charged droplets, said capillary tube having an exit orifice; and said gap being without a counterflow of gas therein; (iv) means to impose a voltage on said capillary tube; (v) means to heat said capillary tube; (vi) a skimmer means to focus the ions and having an inlet and an outlet side and an orifice electrically isolated from the capillary tube, said skimmer means orifice being positioned at a distance from the capillary tube exit orifice; (vii) a first vacuum chamber enclosing the capillary tube exit orifice and the skimmer orifice and first means to create a vacuum therein; (viii) a second vacuum chamber enclosing the outlet side of the skimmer and the inlet orifice of the spectrometer and second means to create a vacuum therein,
Claim 2
Independent Claim
221 words
A system for the analysis of the mass spectra of ions comprising; (a) a mass analyzer having an inlet orifice means to receive ions to be analyzed (b) an electrospray ion source connected to said mass analyzer and including; (i) electrospray means to transport a dilute solution of the molecules of interest and to spray charged micron size droplets of the solution; (ii) means to impose a voltage of about 1-10 KV on said electrospray means; (iii) a capillary tube having an entrance orifice positioned across a gap from said electrospray means to receive said charged droplets, said capillary tube having an exit orifice; and said gap being without a counterflow of gas therein; (iv) means to impose a voltage on said capillary tube; (v) means to heat said capillary tube; (vi) a skimmer means to focus the ions and having an inlet and an outlet side and an orifice electrically isolated from the capillary tube, said skimmer means orifice being positioned at a distance from the capillary tube exit orifice; (vii) a first vacuum chamber enclosing the capillary tube exit orifice and the skimmer orifice and first means to create a vacuum therein; (viii) a second vacuum chamber enclosing the outlet side of the skimmer and the inlet orifice of the spectrometer and second means to create a vacuum therein,
Claim 3
Dependent Claim
15 words
A system as in claim 1 wherein said mass analyzer is a quadrupole mass analyzer.
Claim 4
Dependent Claim
21 words
A system as in claim 1 wherein said electrospray means includes a syringe needle tube through which the solution is pumped.
Claim 5
Dependent Claim
21 words
A system as in claim 1 wherein voltage imposed on the electrospray means is in the range of about 1-10 KV.
Claim 6
Dependent Claim
34 words
A system as in claim 3 wherein the syringe needle has an exit orifice which is positioned in the range of about 0.5 to 4 cm. from the entrance orifice of the capillary tube.
Claim 7
Dependent Claim
14 words
A system as in claim 1 wherein said capillary tube is a metal tube.
Claim 8
Dependent Claim
23 words
A system as in claim 1 wherein said capillary tube is in the range of about 1 cm to 300 cm in length.
Claim 9
Dependent Claim
19 words
A system as in claim 7 wherein said capillary tube is in the range of 1-300 mm in length.
Claim 10
Dependent Claim
24 words
A system as in claim 1 wherein said means to impose a voltage on the capillary tube imposes a voltage of about 0-1000 V.
Claim 11
Dependent Claim
24 words
A system as in claim 9 wherein said means to impose a voltage on the capillary tube imposes a voltage of about 100-300 V.
Claim 12
Dependent Claim
24 words
A system as in claim 1 wherein said means to heat the capillary tube is an electrical resistance wire wound around said capillary tube.
Claim 13
Dependent Claim
31 words
A system as in claim 1 wherein said capillary tube is a metal tube and the means to heat said tube utilizes the resistance of said tube as the heating element.
Claim 14
Dependent Claim
22 words
A system as in claim 1 wherein said first vacuum means creates vacuum in the range of about 0.1 to 50 torr.
Claim 15
Dependent Claim
25 words
A system as in claim 1 wherein said second vacuum means creates a vacuum in the range of about 1×10 -3 to 1×10 -6 torr.
Claim 16
Dependent Claim
24 words
A system as in claim 1 wherein the means to heat the capillary tube heats said tube in the range of about 25°-200° C.
Claim 17
Dependent Claim
24 words
A system as in claim 15 wherein the means to heat the capillary tube heats said tube in the range of about 80°-90° C.
Claim 18
Dependent Claim
26 words
A system as in claim 1 wherein the capillary tube exit orifice is positioned in the range of about 1-10 mm from the skimmer means orifice.
Claim 19
Dependent Claim
16 words
A system as in claim 1 wherein said gap is in the range of about 0.5-5cm.
Claim 20
Dependent Claim
23 words
A system as in claim 1 wherein said gap is in the laboratory atmosphere so that the spray may be viewed and adjusted.
Claim 21
Dependent Claim
15 words
A system as in claim 1 wherein said gap is in a gas controlled atmosphere.
Claim 22
Independent Claim
272 words
A system for the analysis of the mass spectra of ions comprising an electrospray ion source adapted to be connected to a mass analyzer and including; (i) electrospray means including a syringe needle to transport a dilute solution of the molecules of interest and to spray charged micron size droplets of the solution; means to pump said solution through said syringe needle; (ii) means to impose a voltage of about 1-10 KV on said electrospray syringe needle; (iii) an elongated metal capillary tube and having an entrance orifice positioned across a gap from said electrospray means to receive said charged droplets, said capillary tube having an exit orifice; said gap being in the atmosphere and being about 0.5-4cm in width; said gap being without a counterflow of gas therein; (iv) means to impose a voltage of 100-300 V on said capillary tube and means operable by the user to vary said voltage within said range; (v) means to heat said capillary tube in the range of about 80°-90° C.; (vi) a skimmer means to focus the ions and having an inlet and an outlet side and an orifice electrically isolated from the capillary tube, said skimmer means orifice being positioned at a distance from the capillary tube exit orifice; (vii) a first vacuum chamber enclosing the capillary tube exit orifice and the skimmer orifice and first means to create a vacuum therein. (viii) a second vacuum chamber enclosing the outlet side of the skimmer and the inlet orifice of the spectrometer and second means to create a vacuum therein which is a greater vacuum then the vacuum of said first vacuum chamber.
Claim 23
Independent Claim
272 words
A system for the analysis of the mass spectra of ions comprising an electrospray ion source adapted to be connected to a mass analyzer and including; (i) electrospray means including a syringe needle to transport a dilute solution of the molecules of interest and to spray charged micron size droplets of the solution; means to pump said solution through said syringe needle; (ii) means to impose a voltage of about 1-10 KV on said electrospray syringe needle; (iii) an elongated metal capillary tube and having an entrance orifice positioned across a gap from said electrospray means to receive said charged droplets, said capillary tube having an exit orifice; said gap being in the atmosphere and being about 0.5-4cm in width; said gap being without a counterflow of gas therein; (iv) means to impose a voltage of 100-300 V on said capillary tube and means operable by the user to vary said voltage within said range; (v) means to heat said capillary tube in the range of about 80°-90° C.; (vi) a skimmer means to focus the ions and having an inlet and an outlet side and an orifice electrically isolated from the capillary tube, said skimmer means orifice being positioned at a distance from the capillary tube exit orifice; (vii) a first vacuum chamber enclosing the capillary tube exit orifice and the skimmer orifice and first means to create a vacuum therein. (viii) a second vacuum chamber enclosing the outlet side of the skimmer and the inlet orifice of the spectrometer and second means to create a vacuum therein which is a greater vacuum then the vacuum of said first vacuum chamber.
Claim 24
Dependent Claim
37 words
A system as in claim 21 wherein said means to heat the capillary tube is selected from the group consisting of an electrical resistance wire wound around said capillary tube and the electrical resistance of the tube.
Claim 25
Dependent Claim
23 words
A system as in claim 21 wherein said first vacuum means creates a vacuum in the range of about 0.1 to 50 torr.
Claim 26
Dependent Claim
25 words
A system as in claim 21 wherein said second vacuum means creates a vacuum in the range of about 1×10 -3 to 1×10 -6 torr.
Claim 27
Dependent Claim
25 words
A system as in claim 21 wherein the capillary tube exit orifice is positioned in the range of about 1-10mm from the skimmer means orifice.
Claim 28
Dependent Claim
16 words
A system as in claim 21 wherein said gap is in the range of about 0.5-4cm.
References Cited (Backward Citations)
US4209696A
Cited
US4542293A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1993-12-10 | 1994-06-11 | 1994-12-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-12-10 | 1998-06-11 | 1998-12-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-12-10 | 2002-06-11 | 2002-12-11 | $7700.00 | Window Closed / Lapsed |