CHARACTERIZATION TECHNIQUES IN INORGANIC CHEMISTRY

Degree course: 
Corso di First cycle degree in CHEMICAL AND INDUSTRIAL CHEMISTRY
Academic year when starting the degree: 
2022/2023
Year: 
3
Academic year in which the course will be held: 
2024/2025
Course type: 
Supplementary compulsory subjects
Credits: 
6
Period: 
First Semester
Standard lectures hours: 
48
Detail of lecture’s hours: 
Lesson (48 hours)
Requirements: 

A deep knowledge of the topics tackled during the courses of General Chemistry, as well as of the fundamentals of Mathematics and Physics, is a beneficial prerequisite.

Final Examination: 
Orale

The final examination is a two-step procedure:
1. The students are expected to write a report describing what they carried out during the practical exercitations, in terms of data collection and treatment, results obtained and their interpretation, also on the basis of the explanations provided by the professor during front lectures and practical exercitations. The report is satisfactory if it witnesses that the students understood what they did during the practical exercitations.
2. An interview, during which the students will be examined on all the topics tackled during the front lectures and on the critical aspects possibly present in the report at point 1. The students are admitted to the interview only after delivering the report. The interview is satisfactory if it is worth a mark amounting at least to 18/30.

Assessment: 
Voto Finale

Front lecturing aims at increasing students’ knowledge and comprehension in the field of characterization techniques for solid-state (mainly but not exclusively) inorganic materials.
The practical exercitations enable the students to i) apply the topics tackled during the front lessons; ii) test their comprehension skills; iii) get acquainted with instruments that are often present in the R&D or quality control areas of a chemical industry. Treating and interpreting the data collected during the practical sessions should help the students learning to judge in autonomy.
Writing a report at the end of the practical sessions should aid the students rationalizing the obtained results and improving their communication skills.

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.

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.

The teaching activities comprise front lectures (30 hours), with the aid of slides, and practical exercitations in small groups (18 hours).

The professor is available to meet the students any working day, preferably by appointment. Her office is located on the third floor of the building in via Valleggio 9, Como.

Professors