Nuclear Magnetic Resonance

Nuclear Magnetic Resonance Spectroscopy is based on the observation of transitions between energy levels of the nuclei of certain atoms. The separation of said energy levels occurs when the sample is subjected to a very intense magnetic field. The observation of the transitions is carried out using electromagnetic radiation that is in the radio frequency range. The equipment installed in the Service is capable of performing any type of experiment collected in the extensive library of microprograms of the Bruker company or any variation of them that the user desires, provided that the pertinent modification is indicated and, very especially, the necessary phase programming. A wide range of mono and bidimensional spectra can be performed as standard experiments.

High-resolution 1H spectra can be routinely performed with all the usual variations in this technique: double resonance, solvent suppression, relaxation time determination, Overhauser nuclear effect (nOe) measurements, etc. In 13C spectra, spectra with total decoupling are considered routine experiments. DEPT experiments with an angle of 45, 90 or 135 degrees, etc. 31P and 19F experiments can also be routinely performed. The acquisition of spectra of the rest of the nuclei that can be observed with any of the available probes will be considered, in principle, as non-routine experiments, and it is necessary to contact the Service in advance to see the availability of the time necessary to make the adjustments required by said experiments.

Two-dimensional experiments: The following experiments are optimized: proton homonuclear correlation (COSY 45 or 90) Two-dimensional J-resolved spectra, NOESY, ROESY, TOCSY. H/C correlation spectra. The standard experiment performs the correlation to a bond. If a different correlation is desired, the user must indicate the type of experiment and the adjustment constant to be focused on.

Instrumental Facilities

Bruker NEO400 Spectrometer

Equipped with:

  • 400 MHz AscendTM superconducting magnet (proton)
  • NEO 400 Advance Console
  • Variable temperature unit BCU I
  • BBF/H/D probe i-probe
  • Automatic Sample Case Changer 24 positions
  • Software support for data acquisition and processing TopSpin 4.1

Year of acquisition: 2019

 

Bruker AVANCE DPX400 Spectrometer

Equipped with:

  • 400 MHz Superconducting Magnet (Proton) Ultrashield
  • Console Avance III 400
  • Variable temperature unit BCU II
  • CrioSonda prodigy BBO/H/D
  • Automatic Sample Case Changer 24 positions
  • Software support for data acquisition and processing TopSpin 3.6

Year of acquisition: 1997

These two devices can also be operated with any of the following probes.

  • QNP probe for 5 mm tubes with coil for gradients in ze with automatic tuning of 13C, 31P and 19F
  • Reverse acquisition probe for 5 mm tubes with coil for gradients in ze with tuning in the range of 31P to 109Ag
  • Direct acquisition probe for 10 mm tubes with X-core tuning in the range of 31P to 109Ag

Bruker AVANCE DPX600 Spectrometer

Equipped with:

  • 600 MHz Superconducting Magnet (Proton) Ultrashield
  • Two wideband channels and third channel with 300 W of power
  • Variable temperature unit BCU 05
  • Software support for data acquisition and processing TopSpin 2.1
  • TBI probe for 5 mm tubes with triple resonance zeta gradient coil for 1H/13C/BB
  • TBO probe for1H-15N-13C-31P

Year of acquisition: 2001

Applications

This technique has a clear and immediate application in the structural elucidation of compounds possessing magnetically active nuclei (organic compounds and biomolecules), but it can also be applied to the monitoring of non-instantaneous reaction kinetics, the obtaining of physical parameters (rotational barriers) and the quantitative analysis of simple mixtures of compounds. Areas of interest

  • Organic Chemistry
  • Physical Chemistry
  • Inorganic Chemistry
  • Analytical Chemistry
  • Pharmacology
  • Toxicology
  • Food Technology
  • Biology
  • Biochemistry
Sample requirements

This equipment works with samples dissolved in deuterated solvents, and they must arrive perfectly dissolved. If their use is necessary, the Service has small quantities of the most common deuterated solvents, although their cost is not included in the price of the analysis.

The special conditions of the samples, such as their instability, toxicity, volatility, flammability, must be indicated on the analysis request form so that the Service can adopt the appropriate measures.

For one-dimensional 1H and 19F experiments, a sample size of about 2-15 mg is recommended for medium-sized molecules (300 amu). For 13C experiments, a sample size of about 50-60 mg is recommended. For 31P experiments, samples of 5-20 mg are needed.

More information

Manuel Marcos – Sonia Escudero
+34 986 813 884 – 986 812 119

mmarcos@uvigo.es – soniae@uvigo.es