Synchronization of ion generation with cycling of a discontinuous atmospheric interface

Patent metadata

Field	Value
Publication number	US-10755910-B2
Application number	US-201916260924-A
Country	US
Kind code	B2
Filing date	Jan 29, 2019
Priority date	Jan 20, 2011
Publication date	Aug 25, 2020
Grant date	Aug 25, 2020

Abstract

The invention generally relates to methods and devices for synchronization of ion generation with cycling of a discontinuous atmospheric interface. In certain embodiments, the invention provides a system for analyzing a sample that includes a mass spectrometry probe that generates sample ions, a discontinuous atmospheric interface, and a mass analyzer, in which the system is configured such that ion formation is synchronized with cycling of the discontinuous atmospheric interface.

First claim

What is claimed is:

1. A method for monitoring a reaction in real-time, the method comprising:
conducting a reaction in a solvent in a vessel;
flowing a portion of the solvent from the vessel through a channel, wherein an electrode is operably associated with a distal end of the channel and the electrode is external to the channel and does not physically contact the channel or a liquid or vapor within the channel;
generating ions of one or more analytes in the solvent via application of an inductive charge to a distal portion of the channel; and
analyzing the ions, thereby monitoring the reaction in real-time.

2. The method according to claim 1 , wherein the flowing step and the generating step are continuous.

3. The method according to claim 2 , wherein the inductive charge is a pulsed DC charge.

4. The method according to claim 1 , further comprising pulsing nebulizing gas through the channel to interact with the flowing solvent.

5. The method according to claim 1 , wherein analyzing comprises providing a mass analyzer to generate a mass spectrum of analytes in the sample.

6. The method according to claim 1 , wherein both positive and negative ions are produced.

7. The method according to claim 6 , further comprising recording mass spectra of the positive and negative ions.

8. The method according to claim 7 , wherein recording comprises switching polarity of a mass spectrometer while the mass spectrometer is receiving the sample.

9. The method according to claim 1 , further comprising splitting the flowing solvent prior to a distal portion of the channel such that only a portion of the solvent flowing from the vessel flows to the distal portion of the channel.

10. A method for monitoring a reaction in real-time, the method comprising:
conducting a reaction in a solvent in a vessel, wherein the solvent is compatible as an ionization solvent;
flowing a portion of the solvent from the vessel through a channel, wherein an electrode is operably associated with a distal end of the channel and the electrode is external to the channel and does not physically contact the channel or a liquid or vapor within the channel;
generating ions of one or more analytes in the solvent via application of an inductive charge to a distal portion of the channel; and
analyzing the ions, thereby monitoring the reaction in real-time.

11. The method according to claim 10 , wherein the flowing step and the generating step are continuous.

12. The method according to claim 10 , wherein the inductive charge is a pulsed DC charge.

13. The method according to claim 10 , further comprising pulsing nebulizing gas through the channel to interact with the flowing solvent.

14. The method according to claim 10 , wherein analyzing comprises providing a mass analyzer to generate a mass spectrum of analytes in the sample.

15. The method according to claim 10 , wherein both positive and negative ions are produced.

16. The method according to claim 15 , further comprising recording mass spectra of the positive and negative ions.

17. The method according to claim 16 , wherein recording comprises switching polarity of a mass spectrometer while the mass spectrometer is receiving the sample.

18. The method according to claim 10 , further comprising splitting the flowing solvent prior to a distal portion of the channel such that only a portion of the solvent flowing from the vessel flows to the distal portion of the channel.

19. A method for monitoring a reaction in real-time, the method comprising:
providing a system comprising a reaction vessel comprising an outlet port; a channel that extends from within the outlet port; an electrode operably associated with a distal end of the channel, wherein the electrode is external to the channel and does not physically contact the channel or a liquid or vapor within the channel; and a mass spectrometer;
conducting an reaction in the system and analyzing a reaction product in the mass spectrometer of the system, thereby monitoring the reaction in real-time.

20. The method of claim 19 , wherein the electrode is positioned to inductively interact with a distal end of the channel.

Assignees

• Purdue Research Foundation

Inventors

• Cooks Robert Graham
• Li Guangtao
• Huang Guangming
• Duncan Jason
• Li Xin
• Sokol Ewa
• Yan Xin

Classifications

• G01N27/62 Primary

  by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode · CPC title

• H01J49/045 Primary

  with means for using a nebulising gas, i.e. pneumatically assisted · CPC title

• H01J49/0018

  Microminiaturised spectrometers, e.g. chip-integrated devices, Micro-Electro-Mechanical Systems [MEMS] · CPC title

• Y10T436/24

  Nuclear magnetic resonance, electron spin resonance or other spin effects or mass spectrometry · CPC title

• H01J49/0445

  with means for introducing as a spray, a jet or an aerosol (electrospray ion sources H01J49/165) · CPC title