ADVANCED COURSE OF NUCLAR MAGNETIC RESONANCE WITH LABORATORY

Università degli Studi
"G. d'Annunzio"

Chieti - Pescara

Single discipline educational activity

Course Sheet

Course code:

010RMNL

Academic Year of enrolment:

2021

Year of supply:

2023/2024

Type of Course:

Elective Course

Degree:

Course of Single Cycle Degree 5 years in MEDICINAL CHEMISTRY AND PHARMACEUTICAL TECHNOLOGY

Disciplinary Sector:

Organic Chemistry

Language:

Italian

Location:

CHIETI

Credits:

Programme Year:

Professor and Collaborators:

CIULLA MICHELE

Cycle:

Second semester

Obligatory attendance:

Yes

Minimum hours of attendance:

Hours of classroom activity:

Individual study hours:

Prerequisites:

The student must have acquired the certification of frequency for the course of Physical Methods in Organic Chemistry for the CdS in CTF, or have acquired the certification of frequency for the course of Analysis of Medicines II for the CdS in Pharmacy.

Objectives

At the end of the course the student will acquire:

1. Knowledge and understanding

The student:
- will know and understand the fundamentals and the technical-practical applications of proton nuclear magnetic resonance and carbon.
- will know the instrumentation and the main parts from which it is composed.
- will know the software and command procedures of the NMR instrument.
- will know the main advanced techniques of Nuclear Magnetic Resonance.
- knows the safety rules to be followed in an NMR laboratory.

2. Applying knowledge and understanding

The student:
- is able to prepare a sample to perform an NMR analysis.
- is able to set the instrument for the optimization of the NMR analysis.
- can apply graphic and computational changes to the resulting spectrum, which are useful for improving resolution and interpretation of the same.
- will be able to apply complex techniques in order to solve problems that may arise in research or work areas.

3. Making judgments

The student is able to integrate the knowledge acquired during the course with that of the physical-organic chemical strand that characterizes the Degree Course in CTF. The student will be able to interpret spectral data useful for solving typical problems in research and research fields. These skills are stimulated and developed during practical laboratory exercises, in which the student will participate in the production and interpretation of spectra phases.

4. Communication

The student will be able to communicate what has been learned clearly and rigorously. The student is stimulated to interpersonal communication typically during classroom lessons.

5. Lifelong learning skills

The student will have developed autonomous learning skills related to NMR spectroscopic techniques through the consultation of databases, bibliographic material and scientific literature available online.

Contents

Basic principles of Nuclear Magnetic Resonance: theoretical and practical notions.
Nuclear Magnetic Resonance Laboratory:
Proton spectroscopy (1H-NMR): preparatory and analytical aspects;
Carbon-13 NMR spectrometry (13C-NMR): preparatory and analytical aspects;
Two-dimensional NMR spectrometry: development of advanced NMR methods.

Extended Syllabus

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.

Recommended Bibliography

• Silverstein, Webster, Kiemle “Identificazione spettrometrica di composti organici” Seconda edizione, Casa Editrice Ambrosiana.
• Chiappe, D’Andrea “Tecniche spettroscopiche e identificazione di composti organici”, Edizioni ETS
• Friebolin, Basic One- and Two-Dimensional NMR Spectroscopy, 4th ed., Wiley-VCH

Methods of Provision

Conventional

Teaching Methods

The course consists of 12 hours of classroom lectures and 15 hours of practical laboratory.

Evaluation methods

Verification of learning:

The exam consists of a test with multiple choice questions, and / or short questions. The contents of the test will focus on the practical part carried out in the laboratory.

Università degli Studi
"G. d'Annunzio"

Chieti - Pescara

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