Integrated monolithic microfabricated electrospray and liquid chromatography system and method

• US 6,461,516 B2
• Filed: 12/21/2000
• Issued: 10/08/2002
• Est. Priority Date: 09/17/1998
• Status: Expired due to Term

• Current Assignee: Rheonix, Inc.
• Original Assignee: Kionix Incorporated (ROHM Co., Ltd.)
• Inventors: Davis, Timothy J., Moon, James E., Galvin, Gregory J.
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US09/746,866
• Publication Number:
  US 20010001474A1
• Time in Patent Office: 656 Days
• Field of Search: 250/288, 250/288.A, 210/656, 210/748, 210/198.2, 210/243, 204/450, 204/600, 422/70, 436/161
• US Class Current: 210/656
• CPC Class Codes: G01N 30/6095 Micromachined or nanomachined, e.g. micro- or nanosize
• CPC Class Codes: G01N 30/7266 by electric field, e.g. electrospray
• CPC Class Codes: H01J 49/0018 Microminiaturised spectrometers, e.g. chip-integrated devices, Micro-Electro-Mechanical Systems [MEMS]
• CPC Class Codes: H01J 49/167 Capillaries and nozzles specially adapted therefor; electrostatic spraying per se B05B5/00
• CPC Class Codes: Y10T 29/49002 Electrical device making
• CPC Class Codes: Y10T 436/25375 Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.]
• CPC Class Codes: Y10T 436/255 including use of a solid sorbent, semipermeable membrane, or liquid extraction

Abstract

An electrospray device, a liquid chromatography device and an electrosprayliquid chromatography system are disclosed. The electrospray device comprises a substrate defining a channel between an entrance orifice on an injection surface and an exit orifice on an ejection surface, a nozzle defined by a portion recessed from the ejection surface surrounding the exit orifice, and an electrode for application of an electric potential to the substrate to optimize and generate an electrospray; and, optionally, additional electrode(s) to further modify the electrospray. The liquid chromatography device comprises a separation substrate defining an introduction channel between an entrance orifice and a reservoir and a separation channel between the reservoir and an exit orifice, the separation channel being populated with separation posts perpendicular to the fluid flow; a cover substrate bonded to the separation substrate to enclose the reservoir and the separation channel adjacent the cover substrate; and, optionally, electrode(s) for application of a electric potential to the fluid. The exit orifice of the liquid chromatography device may be homogeneously interfaced with the entrance orifice of the electrospray device to form an integrated single system. An array of multiple systems may-be fabricated in a single monolithic chip for rapid sequential fluid processing and generation of electrospray for subsequent analysis, such as by positioning the exit orifices of the electrospray devices near the sampling orifice of a mass spectrometer.

Claims

1. A method for generating an electrospray of a fluid, comprising:

providing a channel extending between an entrance orifice defined on an injection surface of a substrate and a nozzle defined on an ejection surface of said substrate;

providing an insulating layer over at least an interior surface of said channel and interior and exterior surfaces of said nozzle to electrically isolate said surfaces from said substrate;

introducing a fluid into said channel through said entrance orifice;

positioning said nozzle adjacent to a first electrode;

applying a first voltage to said first electrode

providing a second electrode in electrical contact with said fluid;

providing a third electrode in electrical contact with said substrate; and

ejecting said fluid from said channel through said nozzle by applying a second voltage to said second electrode that is different from said first voltage and a third voltage to said third electrode that is different from said second voltage.

2. The method of claim 1 further comprising applying said third voltage at a value approximately halfway between said first and second voltages.

3. The method of claim 1, further comprising:

providing at least one fourth electrode on said ejection surface of said substrate, said at least one fourth electrode being electrically isolated from said substrate; and

applying at least one voltage to said at least one fourth electrode wherein said at least one voltage is chosen to alter a general direction and/or form of said electrospray.

4. The method of claim 1, further comprising:

sensing at least one attribute of said electrospray with a corresponding at least one electrospray attribute sensor;

comparing said at least one sensed electrospray attribute with a corresponding at least one optimal spray attribute set point;

determining, based on said step of comparing, at least one voltage and at least one appropriate electrode; and

applying said determined at least one voltage to said at least one appropriate electrode.