Nuclear Magnetic Resonance

Structural & Morphology Characterization (HF magnetic field imaging)

Nuclear Magnetic Resonance (NMR) is a non-destructive technique in which nuclear spin is manipulated to reveal molecular structure and dynamics information with atomic resolution.  In the case of magnetic resonance imaging (MRI) and microscopy, a picture of the spin density can be generated with 3D pixel (voxel) dimensions down to ~ 10 µm in each direction.  Nearly all elements have at least one isotope whose nucleus has non-zero spin (a quantum mechanical property, given the symbol I), and thus NMR can potentially probe a wide variety of materials in gas, liquid, solution, and solid phases. 

Solid NMR can be used to retrieve information on phase structure in semicrystalline materials, to verify the extent of phase segregation in polymer blends, to measure molecular mobility at different length scales as a function of temperature, composition etc. It is also possible to study synthesis as well as functionalization reactions of polymers and/or inorganic substrates. 

At KIT/ KNMF, our high field NMR system operates at 11.7 T, corresponding to a 1H resonance frequency of 500 MHz.  One caveat to NMR / MRI is that it is a relatively insensitive technique.  For reasonable measurement times, typical limit of detection values include:  low µM concentration for small molecules (< 1500 Da), a few milligrams of material for large molecules in solution (e.g. proteins up to ~ 30 kDa), and several milligrams of material for solid samples.

At CNR the NMR Laboratory consists of two Spectrometers: Varian Mercury 400 MHz, equipped with a ID 1H-19F, 31P-15N bradband probe, and Agilent DD2 NMR System 500 MHz equipped with liquid (Agilent OneMNR), semisolid (Agilent Nanoprobe) and solid state (3.2 mm Agilent T3 triple resonance HXY MAS) probes.

          provided at NFFA-Europe laboratories by:
500 MHz NEO Spectrometer
Liquid state NMR spectroscopy; (Semi)solid state NMR spectroscopy; Magnetic resonance imaging; 2
Micro5 Microimaging probe (10 mm 1H, 5 mm 1H/13C); HRMAS probe (4 mm, 1H/13C/2D); BBFO liquid state probe (1H/19F - 31P-109Ag)
Liquid state samples - from 0.2 to 3 mL, temperature range -10 to 80 °C; Semis-solid samples - from 1 to 100 mg, or from 0.04 - 0.1 mL, temperature range -10 to 80 °C
External magnetic field = 11.7 T
Magnetic resonance imaging capabilities. Sample must be confined in either 10 or 5 mm NMR glass sample tubes. Typical image resolution 50 micormeters isotropic possible within reasonable measurement time.