Dave Kiemle, Instructional Support Specialist
B-18 Jahn Laboratory
470-6883
dkiemle@syr.edu

Nuclear Magnetic Resonance (NMR) Spectrometry

NMR spectroscopy is among the most powerful analytical techniques for the elucidation of chemical structure.  It has the capability of providing detailed information about structure and dynamics of molecules as well as how atoms are connected to each other.   NMR can identify different nuclei in a molecule and analyze large proteins and other large molecules using three dimensional (3-D) techniques.  This instrument provides powerful information for the researcher to indentify compounds, study the structure-function relationship of atoms or the molecules in which they are contained.

The college currently operates 2 Bruker NMR spectrometers, an AVANCE III 600 MHz and an AVANCE 300 MHz  Both instruments are capable of multi-dimensional NMR experiments and are non-destructive to the sample.

The Bruker 600 MHz analyzer utilizes a 14.1 Tesla superconducting magnet and has a sample temperature range of -70 to 150 C. The system has a NMR CASE autosampler that allows for up to 25 samples to be run unattended. This NMR spectrometer is ultrasensitive and equipped with 3 channels with gradients and has the capability of analyzing solid, liquid and intermediate (gel) samples.

Probes

Liquid State:

• SmartProbe- BBFO (Broad Band Flourine Observation) with single axis gradients.  The probe automatically tunes for all nuclei and has the highest sensitivity on both multinuclear and proton channel.
• 5mm TXI ¹H/¹³C/¹⁵N  a triple resonance probe with single axis gradients.
• 1mm TXI ¹H/¹³C/¹⁵N  a triple resonance probe with single axis gradients. Ultimate sensitivity for the smallest of samples. The probe only needs ~ 25ng of material, Homonuclear 2D spectra can be acquired with ~ 250ng, heteronuclear with ~ 2ug of sample.

Solids/Gel samples:

• HRMAS/CPMAS (Doty) 4mm rotor size probe that can handle samples that are either crystalline or amorphous materials. 

Tuning Options:
¹H/X/Y - Double-broadband X & Y channels
¹H/X - broadband X channel (limited range)

We typically analyze prepared samples but can train appropriate users to operate the equipment.  Assistance on experiment design and interpretation of results is also available.  The instrument is scheduled via email Dave Kiemle.

FEES:                   $6 / Hr – internally (minimum charge of $4.00 per sample)

                            $8 / Hr – externally

                            Long runs > 16 hrs are charged $5/hr

The 300 MHz instrument is a walk-on system and students are encouraged to fully operate the equipment. The system has a NMR CASE Autosampler that allows for up to 25 samples to be run unattended. It also has an Autosampler for the solids that can run up to 20 samples.

Probes:

Liquid state - BBFO Broad banded Observe with automatic tuning for all nuclei including ¹⁹F.

Solid State -7mm Broad Band CPMAS solid state probe. Spinning speed of 7000 Hz, and a new 7mm Broad Band CPMAS solid state probe. Spinning speed of 9000 Hz

FEES:  $2.00 per sample for ¹H, $4 per sample for other nuclei, long runs $4.00 per hour. Minimum monthly charge of $20.00. Solid state is $8 / Hr, minimum of $20.00 per sample.

CONTACT:   Dave Kiemle at dkiemle@esf.edu   or 470-6883/6846