Advanced course of Nuclear Magnetic Resonance with laboratory

Basic principles of Nuclear Magnetic Resonance: General review of the basic knowledge of Nuclear Magnetic Resonance. Technical description of an NMR spectrometer with reference to the instrument supplied by the Department of Pharmacy. Sample preparation methods. Main solvents for the solubilization of the sample. Use of the Depth Gauge and Spinner. Definition of Locking and Shimming procedures. Main functions of the software dedicated to the NMR spectrometer. Notions on command strings. Instrument preparation before the experiment, data collection, FID processing and Fourier Transform. Safety regulations.

Nuclear Magnetic Resonance Laboratory: Proton spectroscopy (1H-NMR): Sample preparation, manual adjustment of spin, shim and lock. Execution of proton spectra of known substances. FID, Fourier transform and graphic management of the spectrum. Phasing, ppm cut-off determination and spectrum integration. Selective spin decoupling. Chirality in 1H-NMR spectroscopy. Calculation of coupling constants in cis-trans alkenes. Identification of the main functional groups through the study of the spectra produced during the laboratory practice.

Carbon-13 NMR spectrometry (13C-NMR): Sample preparation, manual adjustment of spin, shim and lock. Execution of proton spectra of known substances. FID, Fourier transform and graphic management of the spectrum. Phasing, ppm cut-off determination. Coupling 1H-13C. Decoupled spectra. DEPT sequence. Chemical displacement. Identification of the main functional groups through the study of the spectra produced during the laboratory practice. Other important nuclei (31P, 15N-NMR).

Two-dimensional NMR spectrometry: 1H-1H COSY and TOCSY correlation, NOESY correlation 1H-1H, 1H-13C HETCOR and HMQC correlation, 13C-13C INADEQUATE correlation.