Core Facility Elemental, Molecular and Materials Analysis
 
 

Nuclear Magnetic Resonance Spectroscopy exploits the behavior of nuclear spins in strong magnetic fields. Using a spin choreography directed by radio frequency pulses, useful information regarding the physical and electronic environment about the nuclei in molecules is obtained, which in turn gives insight into the structure of molecules (including dynamic processes) and their reactivity.   

The Core Facility EMMA is equipped with three NMR spectrometers of varying field strength, and both liquid and solid samples can be measured for a wide range of nuclei. The NMR Spectrometers are fully automated and run on a "self-service" basis with the exception of solid samples. If you require a special or solid-state measurement, please contact us.

For time consuming experiments please make a reservation with Albert (600 MHz) (see bottom of page).

Join our NMR lab! on Clustermarket.

Other techniques to consider: MS, CHNS Analysis.

Instruments

BRUKER 400 MHz NMR Spectrometers

Kurt (O26/4302)

BRUKER AVANCE NEO 400 w/Bruker iProbe TBO BBFO/F/H with Z-Gradient Probehead

Observable Nuclei

  • optimized for:  31P to 199Hg and 17O to 109Ag
  • 1H and 19F

Temperature Range

  • Standard: +20 °C to +80 °C (-80 °C up to +150 °C upon request)

Autosampler

  • 60 positions

  • Routine Measurements
  • X (e.g. 13C) Observation with simultaneous 1H and 19F decoupling.
  • Measurements with solvent suppression
    • Reaction Monitoring
    • Biological samples in H2O
  • VT-Experiments

Emmy (N26/126)

BRUKER AVANCE NEO 400 

Probeheads

Dissolved Samples:

Bruker BBFO Probehead with Z-Gradient

  • Observable nuclei: 1H, 19F, 31P through 109Ag
  • 1H  or 19F decoupling

Solid-State Samples:

Bruker CP-MAS (H/X) VTN (standard bore) 

  • Observable nuclei: 31P to 15N
  • High-power 1H Decoupling 
  • Max. Spin Rate: 15 kHz

Bruker SEI HRMAS Probehead with Gradient (standard bore)

  • Observable nuclei: 1H or 13C (with 1H decoupling)
  • Max. Spin Rate: 5 kHz

Temperature Range (Liquid Samples)

  • Standard: +20 °C to +80 °C (-80 °C up to +150 °C upon request)

Autosampler (liquid samples)

  •     60 positions

Liquid-State 

  • Routine Measurements 
  • Reaction Monitoring
  • X-Nuclei experiments (e.g. 2H, 7Li, 11B, 29Si)

Solid-State 

  • Characterization of inorganic and organic solids and gels

BRUKER 600 MHz NMR Spectrometer

Albert (N26/126)

BRUKER AVANCE NEO 600 w/Bruker iProbe BBO Cryoprobe (Liquid-N2 cooled)

Observable Nuclei

  • 1H, 19F, 31P to 15N

Temperature Range

  • Standard: +20 °C to +80 °C (-40 °C up to +150 °C upon request)

Autosampler

  • 24 positions

  • 2D-Experiments - in particular inverse experiments
  • Solvent suppression 
  • Kinetic studies
  • Time-cosuming experiments - see Reservations tab below for details
  • High-sensitivity measurements, e.g. 13C-experiments with low-solubility or very limited amount analytes
  • DOSY experiments for mixture analyses
  • 2D-NOESY/ROESY experiments

Useful Infomation

  • Day time: from 7:00 to 19:00
  • Night time: from 19:00 to 7:00
  • Standard experiments (e.g. 1H or 19F with 16 scans, 13C with 200 scans, H,H-COSY) that take less than 12 minutes can be performed without booking a spectrometer.
  • Longer running experiments (e.g. 13C with 2.000 scans) will be automatically enqueued as night time measurements.
  • The weekend time is treated like night time, marked experiments will be run preferentially.
  • Please note the indicator in the lower right corner of the ICON NMR program that states the total occupied time for day and night time experiments.
  • If the night time queue extends 12 hours, all additional experiments will be shifted to the next night.
  • To ensure a reasonable sample throughput during day time, we demand using 16 scans as a standard setting for 1H and 19F experiments on Kurt and Emmy.
  • 13C experiments with 200 scans and 31P with 50 scans can be run during day time if necessary, but should be preferentially enqueued for the night. Toggle the sun symbol (next to your experiment selection) to the moon symbol therefore.

Avoid cluttering the day time queue with lots of experiments or unnecessarily high numbers of scans !

  • You should not use more than 20 minutes of measurement time at once.

For time-consuming measurements (kinetics experiments, titrations, high number of scans) please reserve instrument time through our Reservation System.

Sample Preparation

  • Usable NMR-tubes are 5 mm in diameter and 7" or 8" in length. Longer tubes cannot be handled.
  • For high-sensitivity measurements and variable temperature (VT) experiments, high grade tubes (e.g. Norell 502-178) are required.
  • Samples need to be homogenous and fully dissolved in a deuterated solvent (CDCl3, DMSO-d6, D2O, Acetone-d6, etc.)
  • Filling height of 40 mm is highly advised (equals ~ 0.6 mL of solution).
  • Less filling height easily leads to problems in the measuring process. A little over is no problem.
  • Undissolved material generally leads to line broadening and can fault the measurement. Filtration over 0.45 µm PTFE syringe filters is beneficial.
  • For long-running experiments in chlorinated solvents (DCM-d2, CDCl3), specialty PTFE tube caps are highly recommended, as they reduce solvent evaporation significantly.

Sample Submission

  • Institute members (bachelor/master students, Ph.D. candidates, Postdocs) can use the self-service and set up experiments on their own.
  • External users need to contact the NMR-Service and hand in their appropriately prepared samples together with a service form.
  • Solid Samples: Contact Christian Tontsch for training in preparing samples for solid-state measurements.

Submission Forms

  • For non-automated, special measurements carried out by us, please fill out the following forms and send to them to us via eMail:

Other Important Documents

Terms of Use

Price List

Information on how to transfer your data is available at the instrument workstations.

Data download is limited to the campus network.

Christian Tontsch