Università Roma Tre

1. Safety elements in the chemical laboratory.
2. Overview of the contents of the Pharmacopoeia and selected monographs.
3. Molecular analysis: a. Melting point. b. Boiling point. c. Refractometry. d. Determination of absolute and relative density. e. Polarimetry.
4. Structural Analysis: a. Preliminary Examinations: evaluation of solubility, factors influencing it, characteristics of solvents, effect of pH. Solubility of substances in acid and base solutions. b. Organoleptic examination. c. Behavior upon calcination. d. Qualitative elemental analysis: Lassaigne's assay. e. Assays for the detection of the aromatic ring and unsaturations. f. Physical properties, solubility, and detection tests for the most common functional groups.
5. Separation and Purification Methods: a. Separation techniques for homogeneous mixtures: 1) Solvent extraction and extraction methods; 2) Crystallization; 3) Distillation; 4) Chromatography: Introduction, classification of chromatographic methods, most frequently used solid, liquid, and chemically bonded stationary phases; chromatographic separation mechanisms. b. Separation techniques for heterogeneous mixtures: 1) Sublimation; 2) Filtration; 3) Centrifugation.
6. Chromatographic separation techniques: a. Paper chromatography (PC) and thin-layer chromatography (TLC). b. Column chromatography (CC). c. High-performance liquid chromatography (HPLC). d. Gas chromatography (GC).
7. Hyphenated techniques: High-performance liquid chromatography and photodiode array detector (HPLC-DAD); -performance liquid chromatography and mass spectrometry (HPLC-MS); Gas chromatography and mass spectrometry (GC-MS).
8. Instrumental characterization and analysis techniques: a. Mass spectrometry. b. Spectroscopic analysis – IR absorption spectroscopy. c. Spectroscopic analysis – NMR spectroscopy: 1H NMR and 13C NMR (overview). c. Classroom exercises on IR and NMR spectroscopy involving active student participation.
Laboratory sessions focused on topics covered during lectures.

- Caliendo, G. Manuale di Analisi Qualitativa, Ed. EdiSES: For separation and purification methods, molecular and structural analysis
- Cavrini, V.; Andrisano, V. Principi di Analisi Farmaceutica, Ed. Esculapio: For chromatography and coupled techniques
- Silverstein, R. M.; Webster, F. X.; Kiemle, D. J.; Bryce, D. L. Identificazione Spettrometrica di Composti Organici, Ed. Ambrosiana: For mass spectrometry, for IR and NMR spectroscopy
- Chiappe, C.; D’Andrea, F. Tecniche Spettroscopiche e Identificazione di Composti Organici, Ed. ETS: For mass spectrometry, for IR and NMR spectroscopy
- Carrieri, A. Manuale di Analisi Quantitativa dei Medicinali, Ed. EdiSES: For chromatography and for the spectrometric identification of organic compounds