SCC0610 - CHARACTERIZATION TECHNIQUES IN INORGANIC CHEMISTRY

The main topics of the course can be subdivided into two distinct but strictly related parts. A) First part, front lectures, 30 hours: • Diffraction • Historical hints on the discovery of X-rays and the birth of X-ray diffraction. • Lab instrumentation for powder X-ray diffraction: the diffractometer and its main components (X-ray source, slits, monochromator, sample-holder, detector). • Large scale facilities: synchrotrons. • Sample preparation for powder X-ray diffraction: grinding and/or disaggregation, sample-holder choice and filling. • Introduction to qualitative analysis (phase identification, also within a mixture, polymorphs discrimination) on solid-state samples by means of powder X-ray diffraction. Examples of application of qualitative analysis by powder X-ray diffraction at the industrial level (pharmaceutical, dyes and pigments, cement industries, etc.), in mineralogy, in the forensic field, to study artworks, at customs, etc. • Crystallographic databases. • Introduction to variable-temperature powder X-ray diffraction to study the thermal behaviour of solid-state samples in terms of thermal expansion, phase transition, solvent loss, decomposition, etc. • Introduction to qualitative analysis (element identification) on solid-state samples by means of X-ray fluorescence. • Introduction to thermogravimetric analysis: instrumentation, reading and interpreting a thermogram, case studies, applications. • Introduction to differential scanning calorimetry: instrumentation, reading and interpreting a thermogram, case studies, applications. • Introduction to atomic force microscopy. • Introduction to the X-ray absorption techniques: theoretical background, retrievable information, selected cases of study B) Second part, practical exercitations to apply some of the topics tackled during the first part, 18 hours: • Sample preparation and deposition for powder X-ray diffraction experiments. • Powder X-ray diffraction data acquisition by means of a lab facility. • Qualitative analysis of the data (collected on monophasic and polyphasic samples) through a dedicated database. • Study of the thermal behaviour of a handful of materials (examples of thermal expansion, phase transition, solvent loss): data acquisition, data treatment through dedicated software, interpretation of the results. • X-ray fluorescence data acquisition for qualitative analysis and pertinent interpretation. • Thermograms interpretation.