Calorimetry and thermal analysis, laboratory

A.Y. 2020/2021
6
Max ECTS
48
Overall hours
SSD
CHIM/02
Language
Italian
Learning objectives
The course presents the theoretical principles of Calorimetry and Thermal Analysis (Isothermal Calorimetry, DSC, Thermogravimetry, TMA, DMA) and the corresponding instrumentation with the help of laboratory training and exercises of data treatment. As for the specific application to the cultural heritage, the course includes techniques of micro-sampling and the investigation based on the artificial aging of materials.
Expected learning outcomes
The student acquires the basic expertise to collect micro-samples for the experimental investigation and to plan programs of artificial aging that may reproduce the spontaneous or damage-induced degradation of the materials. The laboratory experience adds some awareness of the sensitivity of the experimental approach and the importance of combining Calorimetry and Thermal Analysis with other kinds of investigation.
Course syllabus and organization

Single session

Responsible
Lesson period
First semester
The lessons will be held on the Microsoft Teams platform and can be followed both synchronously on the basis of the timetable published on the University website and asynchronously because they will be recorded and left available to students on the same platform.
Sporadic face-to-face orientation meetings are also scheduled, if the regulations concerning social distancing allow it. The methods and criteria for participating, that require a reservation with a special app, will be published in time on the Ariel pages of the course, as well as all the teaching material (updated and divided by lesson and / or tutorial) and notices relating to any update linked to the evolution of the legislation imposed by Covid-19
The experiments planned at the Calorimetry Laboratory will be carried out in the presence where the legislation imposed by Covid-19 allows it. Alternatively, the "virtual experiment" method will be applied and data collected from previous experiments will be used.

Program and reference material
The program and the reference material will not change

Verification of learning and evaluation criteria:
The exam will take place orally using the Microsoft Teams platform. A presentation of a laboratory report and a brief dissertation (10-minute PowerPoint presentation) on a topic chosen by the student is planned.
The following will be generally evaluated: knowledge of the theoretical principles of calorimetry and thermal analysis; the consistency of the laboratory report; the degree of study of the topic chosen by the student and the inherent bibliographical choice.
Course syllabus
Front Lectures:
Fundaments of Thermodynamics: enthalpy and heat capacity
Fundaments of Chemical Kinetics: progress degree of a given process
Relationship between process rate and associate heat flux
Experimental detection of the heat flux: various kinds of calorimeters
Differential Scanning Calorimetry (DSC): examples of current instruments
The calorimetric trace: base line, signal, underlying area
Thermo-Gravimetry Analysis (TGA): how a thermo-balance works. TGA and DTG trace
Combined TG and DSC: advantages of the combination and uses to characterize materials
Calorimetric and thermal analysis applications for the characterization of the aging of materials associated with processes of: protein denaturation (parchments); crystallization (fats and oils); glass transition (amorphous materials); gelation (polysaccharides), aggregation, oxidation, decomposition.
Principles of Thermo-Mechanical and Dynamico-Mechanical Analysis (TMA and DMA): current instruments
Laboratory:
Preparation and execution of an DSC experiment on material of interest in the field of cultural heritage
Preparation and execution of a (TGA) experiment on material of interest in the field of cultural heritage
Processing of DSC and TG traces obtained.
Prerequisites for admission
Mathematics, General Chemistry, Analytical Chemistry, Physics
Teaching methods
Front lectures, Calorimetry Laboratory, IT exercises on data analysis.
Teaching Resources
The teaching material consists of handouts provided during the course. Added to this are the slides presented during the lessons (pdf files) and scientific articles. Details and downloadable material are available on the teacher's website http://users.unimi.it/thalasa/dimitrios2.htm and on ARIEL. Finally links to websites for chemical education and textbooks are indicated.
Assessment methods and Criteria
The assessment of the actual achievement of the expected learning results by the student takes place through an oral exam with presentation of a laboratory report and a brief dissertation (10-minute PowerPoint presentation) on a topic chosen by the student.
The following will be generally evaluated: knowledge of the theoretical principles of calorimetry and thermal analysis; the consistency of the laboratory report; the degree of study of the topic chosen by the student and the inherent bibliographical choice.
To take the exam, you must register by the deadline set on the SIFA (http://www.unimi.it/).
The evaluation is expressed by a mark out of thirty.
The vote is communicated to each individual student by automated e-mail from the university minutes.
CHIM/02 - PHYSICAL CHEMISTRY - University credits: 6
Lessons: 48 hours
Professor: Fessas Dimitrios