Microcoil based micro-NMR spectrometer and method

• US 6,788,061 B1
• Filed: 09/23/2002
• Issued: 09/07/2004
• Est. Priority Date: 08/01/2000
• Status: Expired due to Term

• Current Assignee: Board of Trustees of The University of Illinois
• Original Assignee: Board of Trustees of The University of Illinois
• Inventors: Magin, Richard L., Peck, Timothy L., Webb, Andrew G., Sweedler, Jonathan V.
• Primary Examiner(s): ARANA, LOUIS M
• Application Number:
  US10/252,655
• Time in Patent Office: 715 Days
• Field of Search: 324/321, 324/318, 324/322, 324/300, 324/307, 324/309
• US Class Current: 324/321
• CPC Class Codes: G01R 33/302 Miniaturized sample handling arrangements for sampling small quantities, e.g. flow-through microfluidic NMR chips
• CPC Class Codes: G01R 33/46 NMR spectroscopy

Abstract

The present invention provides and NMR apparatus comprising an analyte sample holder having a containment region that holds a volume of less than about 1 microliters of the analyte sample, a coil, which encloses the containment region of the analyte sample holder and the analyte sample contained therein, the coil operatively associated with the analyte sample contained in the containment region of the analyte sample holder such that the coil can transmit and/or receive energy from the analyte sample in the containment region of the analyte sample holder, and a magnet to provide a static magnetic field in which the coil and the analyte sample in the containment region of the analyte sample holder are located, wherein the coil and the magnet provide for the obtainment of an NMR spectrum having a spectral line width resolution of less than about 0.1 parts per million.

Claims

1. An NMR apparatus for analyzing and elucidating the chemical structure of an analyte sample, the apparatus comprising:

an analyte sample holder having a containment region that holds a volume of less than 1 microliter of the analyte sample;

a coil operatively associated with the analyte sample contained in the containment region of the analyte sample holder such that the coil can transmit and/or receive energy from the analyte sample in the containment region of the analyte sample holder; and

a magnet creating a substantially constant magnetic field throughout the containment region of the analyte sample holder;

wherein the coil and the magnet provide for the obtainment of an NMR spectrum of the analyte sample in the containment region of the analyte sample holder having a spectral line width resolution of less than about 0.1 parts per million.

2. The NMR apparatus of claim 1, wherein the magnet masses less than 50 kg.

3. The NMR apparatus of claim 1, wherein the magnet is a superconducting solenoid, and is positioned about the containment region of the analyte sample holder.

4. The NMR apparatus of claim 1, wherein the coil encloses the containment region of the analyte sample holder.

5. The NMR apparatus of claim 1, wherein the coil is solenoidal.

6. The NMR apparatus of claim 5, wherein the containment region of the analyte sample holder is positioned outside of the solenoidal coil.

7. The NMR apparatus of claim 1, wherein the coil has an inside dimension of less than about 1 mm.

8. The NMR apparatus of claim 1, wherein the containment region holds a volume of less than about 1 μ

l of the analyte sample.

9. An NMR apparatus for analyzing and elucidating the chemical structure of an analyte sample, the apparatus comprising:

an analyte sample holder having a containment region with a capacity of less than about 1 microliter;

a coil having an inside dimension of less than about 1 mm, the coil being operatively associated with the analyte sample contained in the containment region of the analyte sample holder such that the coil can transmit and/or receive energy from the analyte sample in the containment region of the analyte sample holder; and

a magnet massing less than about 50 kg, the magnet being positioned about the containment region of the analyte sample holder;

wherein the microcoil and the magnet provide for the obtainment of an NMR spectrum of the analyte sample in the containment region of the analyte sample holder having a spectral line width resolution of less than about 0.1 parts per million.

10. A method of analysis and elucidation of the chemical structure on an analyte using NMR, the method comprising:

providing an analyte sample of less than 1 microliter;

providing a coil;

generating a static magnetic field about the analyte sample;

detecting energy emitted from the analyte sample with the coil, and

analyzing the detected energy as a time or frequency domain spectrum having a spectral line width resolution of less than about 0.1 parts per million.

11. The method of claim 10, wherein the static magnetic field is generated with a magnet that masses less than 50 kg.

12. The method of claim 10, wherein the static magetic filed is generated with a superconducting solenoid magnet, and that is positioned about the containment region of the analyte sample holder.

13. The method of claim 10, wherein the coil encloses the containment region of the analyte sample holder.

14. The method of claim 10, wherein the coil is solenoidal.

15. The method of claim 14, wherein the containment region of the analyte sample holder is positioned outside of the solenoidal coil.

16. The method of claim 10, wherein the coil has an inside dimension of less than about 1 mm.

17. The method of claim 10, wherein the containment region holds a volume of less than about 1 microliter of the analyte sample.

18. The method of claim 10, wherein the coil, the magnetic field, and a size of the sample are selected such that the principle constraint on the spectral line width resolution is the noise in the coil.