Apparatus and method for inhibiting ionization source filament failure

Patent metadata

Field	Value
Publication number	US-9159542-B2
Application number	US-201213399791-A
Country	US
Kind code	B2
Filing date	Feb 17, 2012
Priority date	Dec 14, 2010
Publication date	Oct 13, 2015
Grant date	Oct 13, 2015

Abstract

An ion source apparatus for a mass spectrometer comprises a refractory metal filament operable to provide a flow of electrons by thermionic emission; an electrical current source electrically coupled to the filament for heating the filament; a vacuum chamber enclosing the filament; an ionization volume within the vacuum chamber capable of receiving the flow of electrons; a source of an oxygen-providing gas or gases; a restrictive fluidic coupling to the source of oxygen-providing gas or gases; and a gas conduit fluidically coupled to the restrictive fluidic coupling, the restrictive fluidic coupling and conduit operable to provide a flow of the oxygen-providing gas or gases into the vacuum chamber so as to maintain a partial pressure of said gas or gases within the vacuum chamber that is sufficiently high so as to inhibit the otherwise formation of a carbonaceous growth on the filament in the presence of a gaseous carbon-containing material.

First claim

What is claimed is:

1. A method of operating an ion source for a mass spectrometer comprising:
providing a refractory metal thermionic filament positioned within a vacuum chamber, wherein the filament is fabricated from rhenium or a rhenium alloy;
passing a current through the filament to generate a stream of electrons wherein the filament is operated at a temperature in excess of 1200 degrees Kelvin;
introducing a carbonaceous gas including one of a reagent gas or a sample gas into the vacuum chamber, wherein molecules in the gas interact with the stream of electrons or with ionized background gases to form ions, wherein a portion of the gas comes into contact with surfaces of the filament such that carbon from the carbonaceous gas is dissolved in the filament, resulting in the subsequent formation of at least one carbonaceous growth on the filament; and,
introducing an oxygen-containing gas devoid of fluorine gas or nitrogen trifluoride into the vacuum chamber, wherein the oxygen-containing gas removes all or part of the carbonaceous growth or inhibits its formation.

2. A method as claimed in claim 1 wherein the oxygen-containing gas comprises ambient air.

3. A method as claimed in claim 1 wherein one or more components of a sample provided to the mass spectrometer comprise the gaseous carbon-containing material.

4. A method as claimed in claim 1 wherein the pressure of the reagent gas is at least 1×10 −7 Torr in the vacuum chamber.

5. A method as claimed in claim 1 wherein a gas chromatograph is coupled to the ion source providing sample gas molecules as the carbonaceous gas.

6. A method as claimed in claim 1 wherein the partial pressure of the oxygen-providing gas or gases maintained within the vacuum chamber is at least 1×10 −6 Torr.

7. A method as claimed in claim 1 wherein the partial pressure of the oxygen-providing gas or gases within the vacuum chamber is insufficient to promote significant evaporation of the rhenium from the filament.

8. A method as claimed in claim 1 wherein the reagent gas comprises a polycyclic aromatic hydrocarbon.

9. A method as claimed in claim 1 wherein the reagent gas comprises at least one compound selected from the group consisting of naphthalene, fluorine, phenanthrene, pyrene, fluoranthene, chrysene, triphenylene, perylene, acridine, 2,2′ dipyridyl, 2,2′ biquinoline, 9-anthracenecarbonitrile, dibenzothiophene, 1,10′-phenanthroline, 9′ anthracenecarbonitrile, and anthraquinone.

10. A method as claimed in claim 1 wherein the reagent gas comprises at least one compound chosen from the group consisting of azulene, homoazulene, acenaphthylene, homodimers of azulene, homodimers of homoazulene, and homodimers of acenaphthylene.

11. A method as claimed in claim 1 wherein the reagent gas comprises at least one compound chosen from the group consisting of a heterodimer comprising one azulene unit and one homoazulene unit, a heterodimer comprising one azulene unit and one acenaphthylene unit and a heterodimer comprising one homoazulene unit and one acenaphthylene unit.

12. A method as claimed in claim 1 wherein the reagent gas comprises an aliphatic compound with an electron affinity between 0.3 and 0.8 electron-volts.

13. A method as claimed in claim 12 wherein the aliphatic compound is 1-3-5-7-cyclooctatetraene.

14. A method as claimed in claim 1 wherein the reagent gas comprises at least one compound chosen from the group consisting of benzoic acid, perfluoro-1,3-dimethylcyclohexane, and perfluorotributylamine.

15. A method as claimed in claim 1 wherein the reagent gas comprises an unsaturated organic compound having a Franck-Condon factor between 0.1 and 1.0 and a positive electron affinity value between 0.1 and 200 kJ/mol.

16. A method as claimed in claim 1 wherein the reagent gas comprises at least one compound chosen from the group consisting of nitrosobenzene; nitrobenzene; 1,4 dicyanobenzene; 1,3 dicyanobenzene; 5-cyano 1,2,4-triazole; amitrole 2-aminopyridine; 2-pyridine carbonitrile; 3-pyridine carbonitrile; 3-chlorobenzonitrile; 4-chlorobenzonitrile; 3-pyridinecarbonitrile; 4-pyridinecarbonitrile; 1,2-dicyanoethylene and 1,2-dicyanoacetylene.

17. A method as claimed in claim 1 wherein the oxygen-containing gas or gases comprises a pressurized gas mixture of x percent oxygen (O 2 ) and (100−x) percent of another gas or of a mixture of gases, wherein 0.1≦x≦25.

18. A method as claimed in claim 1 wherein the oxygen-providing gas or gases comprises zero-grade air.

19. A method as claimed in claim 1 wherein the oxygen-providing gas or gases comprises nitrous oxide (N 2 O).

20. A method as claimed in claim 1 wherein the oxygen-providing gas or gases comprises water vapor (H 2 O).

21. A method as claimed in claim 1 wherein the electrical current source is an alternating current (AC) current source.

22. A method as claimed in claim 1 wherein the electrical current source is a direct current (DC) current source.

23. A method as recited in claim 1 , wherein the ion source comprises an electron ionization (EI) source and wherein a sample provided to the mass spectrometer comprises the gaseous carbon-containing material.

24. A method as recited in claim 1 , further comprising:
providing an ionization volume fluidically coupled to the vacuum chamber; and
providing a conduit operable to provide a reagent gas into the ionization volume so as to maintain a partial pressure of the reagent gas within the ionization volume of at least 1×10 −7 Torr, wherein the ion source comprises a chemical ionization (CI) source and wherein the reagent gas comprises the gaseous carbon-containing material.

25. A method as recited in claim 1 , wherein the controlled flow of the gas or gases from the source of oxygen-providing gas or gases is provided into the vacuum chamber so as to maintain the partial pressure of the oxygen-providing gas or gases within the vacuum chamber at a level that is insufficient to promote significant evaporation of the rhenium from the filament.

26. A method as recited in claim 1 , further comprising:
providing an ionization volume fluidically coupled to the vacuum chamber; and,
providing a conduit operable to provide a reagent gas into the ionization volume so as to maintain a partial pressure of the reagent gas within the ionization volume of at least 1×10 −7 Torr, wherein the ion source comprises a chemical ionization (Cl) source and wherein the reagent gas comprises the gaseous carbon-containing material.

Assignees

• Mullen Christopher
• Syka John E P
• Quarmby Scott T
• Thermo Finnigan Llc

Inventors

• Mullen Christopher
• Syka John E P
• Quarmby Scott T

Classifications

• H01J49/147 Primary

  with electrons, e.g. electron impact ionisation, electron attachment (H01J49/145 takes precedence) · CPC title

• H01J2237/06308

  Thermionic sources · CPC title

• H01J49/16

  using surface ionisation, e.g. field-, thermionic- or photo-emission · CPC title

• H01J27/26

  using surface ionisation, e.g. field effect ion sources, thermionic ion sources (H01J27/20, H01J27/24 take precedence) · CPC title

• H01J49/0027

  Methods for using particle spectrometers · CPC title