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Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR
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A table-top PXI based low-field spectrometer for solution dynamic nuclear polarization.

Joshua R Biller1, Karl F Stupic1, J Moreland1

  • 1Physical Measurement Laboratory, National Institute of Standards and Technology, Boulder, CO, USA.

Magnetic Resonance in Chemistry : MRC
|October 20, 2017
PubMed
Summary
This summary is machine-generated.

A new portable dynamic nuclear polarization (DNP) instrument was developed for studying proton (¹H) polarization enhancements at low magnetic fields. This instrument achieved significant ¹H enhancements (~65) in aqueous solutions using the Overhauser effect.

Keywords:
1HDNPHyperpolarizationLabVIEWNitroxidePXIResonator efficiency

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Area of Science:

  • Magnetic Resonance Spectroscopy
  • Physical Chemistry
  • Instrument Development

Background:

  • Dynamic Nuclear Polarization (DNP) enhances nuclear spin polarization.
  • Low-field DNP studies are valuable for various chemical and biological applications.
  • Previous DNP instruments were often limited in portability and field range.

Purpose of the Study:

  • To develop a portable DNP instrument for studying proton (¹H) polarization enhancements.
  • To investigate the Overhauser mechanism at low magnetic fields (6.7 mT).
  • To assess the instrument's performance with varying radical concentrations and power levels.

Main Methods:

  • Construction of a DNP probe set for low magnetic fields (6.7 mT).
  • Utilized a modified Alderman-Grant resonator (241 MHz) for electron transition saturation.
  • Employed a Litz wire solenoid for enhanced ¹H signal detection (288 kHz).
  • System based on the PCI eXtensions for Instrumentation platform.

Main Results:

  • Observed maximum ¹H enhancements (ε) of ~65 at 6.7 mT for 14N-CTPO radical in aqueous solution.
  • Found concentration dependence, with peak enhancement at 5.5 mM.
  • Noted decreased enhancement at higher concentrations (10.3 mM) due to lower resonator efficiency.
  • Identified capacitor heating effects at high power (42 W) and long pump times reducing enhancement.

Conclusions:

  • The developed portable DNP instrument is effective for low-field ¹H polarization studies.
  • The instrument's core design is adaptable for multi-frequency DNP experiments.
  • Further optimization of resonator efficiency and thermal management could improve performance.