ANALYTICAL CHEMISTRY AND QUALITY CONTROL - Spectroscopy
the student must have clear the concepts of molecular bonds, molecular weight, functional groups and polarity of the molecules, concepts provided in the previous courses of general and inorganic chemistry and organic chemistry
The principle aim of the course is to provide students with the skills to perform qualitative and quantitative analysis according to codified procedures, using the most common instrumental techniques. The main skills acquired will be:
• To know the principles, the instrumentation of the most common spectroscopic techniques to perform qualitative and quantitative analyzes;
• To know the chromatographic separation techniques and the different chromatographic retention mechanisms;
• To know the instrumentation for gas chromatography and for liquid chromatography;
• To know the principles of nuclear spectroscopy techniques and know how to analyze spectra related to this technique;
• To know the quality control standards for the validation of a method.
A) Nuclear magnetic resonance spectroscopy
- Principles of nuclear magnetic resonance
- Nuclear magnetic resonance for hydrogen
- Nuclear magnetic resonance for carbon in continuous wave
- Magnetic resonance in Fourier transform
- Two-dimensional magnetic resonance techniques
- Analysis of one-dimensional NMR spectra
- Molecular recognition exercises through NMR spectra
- B) Mass spectrometry
- Principles of mass spectrometry
- Instrumentation for mass spectrometry
- Analysis of mass spectrometry spectra
- C) Chromatographic purification and analysis techniques
- Principles of chromatography. Stationary phases and mobile phases: adsorption chromatography on flat surface (TLC) and on column (eluents and methods to highlight the compounds present)
- Distribution chromatography, exclusion, ion exchange and affinity
- Gas chromatography. Parts of the instrument. Injector, column (oven), detector, Gas carrier
- Structural specifications of the stationary phases used
- Qualitative and quantitative analysis; parameters that can influence an analysis
- Analysis with GC-MS instrument
- Examples of separation of complex mixtures
- High performance liquid chromatography (HPLC). Parts of the instrument: injector, column, detector and eluent. Characteristics of the direct and inverse stationary phases and eluents generally used
- Theory of UV-vis spectroscopy and fluorescence for the determination of substances
D) Quality control
- General quality control: the ISO 9001 and ISO 17025 reference standards
- Quality control methods: development and validation
- Gas chromatography: head space for the determination of residual solvents in the finished product; determination of the progress of a reaction with a mixture of dodecylbenzene isomers
- UHPLC: research of residual monomers in acrylic polymers in reverse emulsion
- HPLC: evaluation of the content of a reaction by-product and measurement of the ratio of the two isomers of the finished product
- FT-IR spectrometry: determination of the iodine number in a mixture of regenerated exhausted vegetable oils; control of a ternary mixture of reaction solvents
- NMR technique: evaluation of the substitution efficiency of a natural polymer
Lesson slide on E-learning
BOOKS: “Guida pratica alla interpretazione di spettri NMR”. Aut. Antonio Randazzo - Editore Loghia.
“Strumenti per il laboratorio chimico/biologico”. Aut. S. Polesello, A. Polesello, S. Guenzi, C. Roscioli – Editore: Tecniche Nuove (Mi)