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School of Science
MATERIALS SCIENCE
Course unit
MATERIAL ANALYTICAL CHEMISTRY WITH LABORATORY OF PREPARATION AND CHARACTERIZATION OF MATERIALS
SCP3049590, A.A. 2019/20

Information concerning the students who enrolled in A.Y. 2017/18

Information on the course unit
Degree course First cycle degree in
MATERIALS SCIENCE
SC1163, Degree course structure A.Y. 2008/09, A.Y. 2019/20
N0
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Number of ECTS credits allocated 9.0
Type of assessment Mark
Course unit English denomination MATERIAL ANALYTICAL CHEMISTRY WITH LABORATORY OF PREPARATION AND CHARACTERIZATION OF MATERIALS
Department of reference Department of Chemical Sciences
Mandatory attendance No
Language of instruction Italian
Branch PADOVA
Single Course unit The Course unit can be attended under the option Single Course unit attendance
Optional Course unit The Course unit can be chosen as Optional Course unit

Lecturers
Teacher in charge STEFANO AGNOLI CHIM/03
Other lecturers DENIS BADOCCO CHIM/01

ECTS: details
Type Scientific-Disciplinary Sector Credits allocated
Core courses CHIM/01 Analytical Chemistry 4.0
Core courses CHIM/03 General and Inorganic Chemistry 5.0

Course unit organization
Period First semester
Year 3rd Year
Teaching method frontal

Type of hours Credits Teaching
hours
Hours of
Individual study
Shifts
Laboratory 6.0 72 78.0 2
Lecture 3.0 24 51.0 No turn

Calendar
Start of activities 30/09/2019
End of activities 18/01/2020
Show course schedule 2019/20 Reg.2008 course timetable

Syllabus
Prerequisites: Inorganic and general chemistry (1st year) and Inorganic and solid state chemistry (2nd year). ability to perform simple stoichiometry calculations (concentration pH of a solution). Basics of Electrochemistry (Faraday law, Nerst equation ). Basic knowledge of the electronic structure of materials (what's the conduction/valenece band? HOMO,LUMO, work function)
Target skills and knowledge: The course will provide he students with the fundamentals of analytical chemistry, in particular the basic principles of modern analytical chemistry and the basics statistical analysis, which are needed in order to interpret correctly analysis results and quantify errors.
The materials preparation laboratory will be focused on:
i) individuation and practical realization of the best synthesis routes (wet chemistry, sol-gel, chemical vapor deposition) for the preparation of materials with selected properties
ii) comprehension of the working principle of simple devices and of the role of materials (electrochemical cell, OLED)
iii) knowledge of some basics techniques for materials characterization (VIS-UV spectroscopy, interferometry)
Examination methods: Oral and written exam. No mid term evaluation.
written reports on the laboratory activities will be evaluated
Analytic Chemistry: about 60 questions with multiple chiose answers
Laboratory of materials preparation: 6-8 open ended questions. It is possible to improve the final score with an oral integration.
Assessment criteria: Part of analytical Chemistry:
written exam typically made up 60 multiple choice questions. the evaluation of the laboratory reports (range: +2,-2) is summed to obtain the final grade.

Part of Laboratory of materials preparation and characterization:
evaluation of the laboratory reports (correctness of information, use of proper technical jargon, data analysis) and of laboratory practice (correct practical implementation of the synthesis protocols, knowledge and respect of safety rules. etc). Written exam with open ended questions.
Course unit contents: Part of analytical Chemistry(4 credits):
Theoretical part
Analytical method. Mathematical statistics applied to analytical methods: probability and distribution, mean, median, mode, standard deviation, variance, range, estimation, tests. Analytical procedure. Errors, precision, bias, accuracy. EURACHEM european regulations. Calibration: standard additions and internal standard. OLS and Theil calibration lines. Confidence and prediction intervals. Quantification and detection limit. Comparison among methods. Preparation of samples.
UV-Vis absorption spectrophotometry: instrument, sources, filters, gratings. Lambert-Beer law. Multicomponent analysis. Isosbestic point. Atomic absorption spectrometry. Flame instruments (AAS). Effects of instrumental parameters. Hollow-cathode lamp. Interferences and their correction. Atomic emission spectroscopy. Ionization methods. Sample introduction. Plasma atomization and ICP coupling. Optical and mass ICP. Instrumental scheme and description. Detector. Applications. Ultra-trace analyses. Analyses on semiconductor surfaces. Sensors. Optical sensor for oxygen. Stern-Volmer equation. Ion-selective sensors. Winkler method for the determination of oxygen in water solution. Laboratory practice. Titrations. Complexometric titration for the determination of the water hardness.

Part of Laboratory of materials preparation and characterization (5 credits):
The sol gel method applied to materials science (precursors, hydrolysis and condensation reactions, gel, drying, aging firing. Deposition techniques: spinning and dip coating)
The chemical vapor deposition: instrumentations, precursors, mass transport inside reactors, surface processes and kinetics.
Laboratory activity will be focused on the preparation of different materials (either as powders or thin films) and simple devices:
-thin films and nanoparticle by sol-gel
-thin films by CVD
- assembly of an OLED
-study of the electrocatalytic properties of materials
-synthesis of a MOF
The characterization of the prepared materials will be carried out by UV-VIS spectroscopies and interferometry.
Planned learning activities and teaching methods: Part of analytical Chemistry:
Experimental part
1. Comparison among two analytical methods: Fe(III) analysis by UV-VIS and AAS
2. Determination of zinc in hairs by AAS
3. Determination of fluoride in toothpastes or mouthwashes by ion-selective electrode
4. Complexometric titration of Ca and Mg and determination of tap water hardness
5. Determination of ε (absorbivity coefficient), of the isosbestic point, and of the acidity constant of phenol red
6. Determination of oxygen in water solution by Winkler method, by the optical sensor, and by the Clark sensor.

Part of Laboratory of materials preparation and characterization:
during the first 8h of class lectures, it will be given the basic information the laboratory experiences and a theoretical background necessary to prepare thin films by CVD and to analyze materials by UV-VIS spectroscopy.
During the laboratory classes, the students will be able to prepare selected materials and to analyze their products by different characterization techniques.
Additional notes about suggested reading: http://www.chimica.unipd.it/case
http://www.chimica.unipd.it/stefano.agnoli
Textbooks (and optional supplementary readings)
  • M.L. Hitchman & L.F. Jensen, Chemical Vapor Deposition: Principles and Applications. --: Academic Press, 1993. Cerca nel catalogo
  • C.J. Brinker and G.W. Scherer, Sol-Gel Science: The Physics and Chemistry of Sol-Gel Processing. --: Academic Press, 1990. Cerca nel catalogo
  • Skoog, West, Holler, Crouch, Fondamenti di Chimica Analitica. --: EdiSES, 2005. II edizione italiana Cerca nel catalogo
  • Harris, Chimica Analitica Quantitativa. --: Zanichelli, 2005. II edizione italiana Cerca nel catalogo

Innovative teaching methods: Teaching and learning strategies
  • Lecturing
  • Laboratory
  • Case study
  • Working in group

Sustainable Development Goals (SDGs)
Affordable and Clean Energy