Design and construction of a microcoil NMR probe for the routine analysis of 20-μL samples†

  1. Ian D. Henry1,
  2. Gregory H.J. Park1,
  3. Ravi Kc1,
  4. Brian Tobias2,
  5. Daniel Raftery1,*

Article first published online: 7 FEB 2008

DOI: 10.1002/cmr.b.20101

Issue

Concepts in Magnetic Resonance Part B: Magnetic Resonance Engineering

Concepts in Magnetic Resonance Part B: Magnetic Resonance Engineering

Volume 33B, Issue 1, pages 1–8, February 2008

Additional Information

How to Cite

Henry, I. D., Park, G. H.J., Kc, R., Tobias, B. and Raftery, D. (2008), Design and construction of a microcoil NMR probe for the routine analysis of 20-μL samples. Concepts Magn. Reson., 33B: 1–8. doi: 10.1002/cmr.b.20101

Author Information

  1. 1

    Department of Chemistry, Purdue University, West Lafayette, IN 47907

  2. 2

    Pfizer, Inc., 9725 Scranton Road, San Diego, CA 92121

*Department of Chemistry, Purdue University, West Lafayette, IN 47907

  1. †

    This work has been presented at the following conferences: 2006 Chicago Area NMR Discussion Group Meeting, 2007 Pittsburgh Conference, 2007 NOBCChE National Conference, and the 2007 Experimental NMR Conference.

Publication History

  1. Issue published online: 11 APR 2008
  2. Article first published online: 7 FEB 2008
  3. Manuscript Accepted: 10 SEP 2007
  4. Manuscript Revised: 27 AUG 2007
  5. Manuscript Received: 19 JUL 2007

Funded by

  • National Institutes of Health. Grant Number: 5R01-RR-018294-04

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Keywords:

  • 1H NMR;
  • microcoils;
  • transmission lines;
  • HF;
  • laser etching

Abstract

Recent advances in microcoil NMR have provided commercially available, robust methodologies for analyzing mass and volume limited samples in the low microliter regime, and the technology has been applied in a number of areas. Unfortunately, due to constraints on sample size and the limited solubility of some compounds of interest, the application of this approach to certain areas of development, such as the structural analysis of chromatography eluates, is restricted. A current challenge is to provide an option within a previously unexplored sample size regime (tens of microliters) while still taking advantage of the increase in mass sensitivity afforded by solenoidal microcoil NMR. In this article, we present the design and construction of a microcoil NMR probe with a custom detection cell for the routine analysis of 20-μL samples. The detection cell is comprised of a CO2-laser-heated HF-etched borosilicate active volume with fused silica transfer lines added to provide sample input and output. This setup produces an enlarged sample bubble within the detection coil and provides easy connection with 1/16 in. standard LC connections, lending itself to applications with HPLC-NMR, online SPE and similar separation techniques, as well as higher-throughput robotic automation. NMR performance characteristics determined using standard compounds showed the probe exhibited reasonable resolution (<0.01 ppm), although sensitivity was less than optimal due to tuning constraints. Future improvements and opportunities are also discussed. © 2008 Wiley Periodicals, Inc. Concepts Magn Reson Part B (Magn Reson Engineering) 33B: 1–8, 2008

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