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Instrument Development for the User Program


William Brey

Peter Gor'kov

Kiran Shetty

Nathaniel Falconer

Richard Desilets

Jason Kitchen

Many of the NMR sample probes available to users of the NHMFL NMR facility have been developed by the NMR instrument development group. The 900 MHz ultra-wide bore and other unique magnets at the NHMFL often require probes and electronics that are not commercially available. Also, NMR scientists who use the facility often have experimental requirements that are not met by commercial equipment. Our in-house probe and hardware development currently address the three areas outlined below. We also enter collaborations with other institutions. Below are brief descriptions of some of the hardware we have provided for MagLab users.


Development of Probes for 900 MHz UWB

The ultra-wide bore 900 MHz magnet at NHMFL presents a unique opportunity for high-field solid state NMR and in vivo magnetic resonance microscopy. We have developed a "Low-E" probe for solid state NMR on the 900 UWB that is used to determine structures of membrane-bound proteins associated with infectious diseases such as influenza. Another probe uses the wide bore of the 900 to allow magic angle spinning (MAS) experiments at low temperatures to study phase transitions and other temperature-dependent behavior in new and interesting materials. Imaging is another important capability of the 900's wide bore. In collaboration with the MRI program at the AMRIS facility at the University of Florida, we are developing coils and animal support systems that will enable the 900 UWB to be used to study animals as large as adult rats.

900 MHz 3.2 mm 1H—X transmission line MAS probe for material science
900 MHz low-E 1H—X static probe for biological solids
900 MHz probe development for imaging of mice

HTS Probe for Natural Products

In a collaboration with Bruker Biospin we have developed a probe with extraordinary sensitivity for solution NMR studies of chemicals produced by biological organisms. This probe, which now operates at UF's AMRIS NMR facility, is based on high temperature superconductor (HTS) technology. It is the first HTS probe to use a 1-mm sample tube, and also the first HTS probe to have triple resonance capability, allowing it to be used for mass-limited proteins as well as smaller molecules.

1 mm HTS 1H—13C—15N solution NMR probe for natural products

Low-E Probes for Biological Solid-State NMR

We have developed a new approach to solve the problem of sample heating in solid state NMR for protein structure determination. These probes have overcome a significant experimental hurdle to the success of solid-state NMR of these heat-sensitive samples. This approach, named "Low-E" because the heat-generating electric field is reduced, has been used both for static and magic angle spinning probes. Low-E probes have been constructed for the 900 MHz ultra-wide bore and other NHMFL magnets, as well as for the AMRIS in Gainsville and for other laboratories in the US and Europe.  This technology is being developed with our expertise for commercial use by Bruker Biospin.

900 MHz low-E 1H—X static probe
750 MHz low-E 1H—X MAS probe
600 MHz low-E 1H—X static probes
600 MHz low-E 19F—1H static probe
600 MHz low-E 31P—1H static probe
400 MHz low-E 1H—X static probe
Reasons for using low-E probes
Sample heating and low-E design
Changing coils & nuclei
Sample supplies

29 mm Family of Narrow Probes for High Field 830 MHz and Resistive Magnets

A family of probes for solid state applications in narrow 31 mm bore magnets, both superconductive and resistive, allows users to take advantage of the benefits to sensitivity and resolution of high magnetic fields for spectroscopy, among other things, of quadrupolar nuclei. These 29 mm probes come equipped with magic angle spinning (MAS), and with a wide choice in rotor size — 2, 4, or 7 mm. Spinning at up to 50 kHz, the MAS probes have been used in narrow bore magnets from the 19.6 T to the 45 T Hybrid.

830 MHz 2mm fast MAS probe for quadrupolar nuclei
830 MHz 4mm MAS probe for quadrupolar nuclei
830 MHz 7mm MAS probe for quadrupolar nuclei
830 MHz variable temperature static probe, low- & mid- gamma
830 MHz stray field imaging (STRAFI) probe
830 MHz fourier transform STRAFI probe

NMR in Resistive and Hybrid Magnets

We are developing instrumentation that will open NHMFL's hybrid and resistive magnets for wider NMR applications. This program aims to provide experimental NMR capability for materials chemistry and biology on the 36T series hybrid currently in development at the NHMFL.  RF sample probes for a 1H frequency as high as 1.6 GHz and a system that reduces static field fluctuations in resistive magnets are being designed and tested.

25 Tesla high-resolution 4mm MAS probe
Flux stabilization insert
Sample loading insert