Analytical Chemistry with Lab

A.Y. 2024/2025
12
Max ECTS
112
Overall hours
SSD
CHIM/01
Language
Italian
Learning objectives
(a) Theory module (Chimica Analitica I)
Getting acquainted with fundamental definitions and concepts in Analytical Chemistry. Learning elements of error analysis and statistics, particularly applied to analytical chemistry. Discussing at a more advanced level, also in terms of activities, acid/base, redox, precipitation and complexation equilibria in aqueous solutions, also applied to the interpretation of titration curves in volumetric analysis. Getting to know at basic level a first family of instrumental analytical techniques, i.e. the electroanalytical ones; in particular conductimetry, potentiometry, voltammetry and amperometry will be discussed, to understand their theoretical background as well instrumental and applicative issues.

(b) Laboratory module (Laboratorio di Chimica Analitica I)
Knowledge of the procedures, the experimental protocols and the fundamental calculations in Analytical Chemistry. Basic knowledge of colorimetric titrations and of the fundamental electroanalytical techniques: conductimetry, potentiometry, amperometry. Basic knowledge of fundamentals of product quality and chemical process controls.
Expected learning outcomes
(a) Theory module (Chimica Analitica I)
- Acquaintance with fundamental definitions and concepts in Analytical Chemistry
- Ability to apply basic error analysis and statistics to estimate reliability and significance of analytical data, also in connection with the laboratory module.
- Ability to manage solution equilibria and electrode potentials also in terms of ionic activities, and to exploit them for prediction and interpretation of titration curves based on acid/base, precipitation, complexation and redox equilibria, as concurrently practiced in the laboratory module.
- Basic knowledge of fundamentals, procedures and applications of electroanalytical techniques (conductimetry, potentiometry, voltammetry, amperometry), some of them possibly practiced in the laboratory module.

(b) Laboratory Module (Laboratorio di Chimica Analitica I)
Use of the basic analytical techniques: colorimetric titrations and fundamental electroanalytical methodologies. Use of an electronic spreadsheet for data treatment. Principles of statistical data treatment and error theory. Principles of quality control of the chemical products and processes.
Single course

This course can be attended as a single course.

Course syllabus and organization

Single session

Lesson period
Second semester
Prerequisites for admission
Fundamentals of general and inorganic chemistry, stoichiometry principles, mathematical principles.
Assessment methods and Criteria
The exam score is calculated by adding the scores of the various parts described below, for a total of 32 points corresponding to the maximum grade of 30 cum laude.(a) Theory module (Chimica Analitica I)

a) Theory module (Chimica Analitica I)

The theory module implies
· An examination on the first two course parts (up to 10.5 points), written and in presence as regular mode (2 hours; questionnaire including brief open-answer questions, exercises and problems on the subjects treated, grouped in eight sections).
· An oral examination on the third course part (electroanalytical techniques) (up to 5.5 points).

Both examinations must be successfully passed (minimum 6 points for the first one; minimum 3 points for the second one).


(b) Laboratory module (Laboratorio di Chimica Analitica I)

Written Exam (1.5 hours) based on 4 questions with long open answers. In particular: 2 exercises on stochiometric/analytical calculations + 1 question related to the quality control and 1 question on the theoretical part of the course (up to 11 points, minimum 8 points, of which at least 5 in the first two exercises).
Behaviour in the lab, the laboratory booklet and the two intermediate reports will be evaluated during the laboratory period. (up to 5 points).
Analytic chemistry
Course syllabus
Part 1 Propedaeutic concepts Analytical Chemistry: definition, history, significance. Analytical methods. Sequence of steps in a typical quantitative analysis. Sampling. Elements of theory of errors applied to analytical chemistry; criteria for data treatment and statistical tests. Concentration scales, ionic strength, activities, activity coefficients. Recalling fundamental thermodynamic parameters of chemical and electrochemical systems and processes. Chemical potentials, standard states, equilibrium constants. Galvanic chains, Nernst law, electrochemical cells and ion-reversible electrodes, electrode potential scale.

Part 2 Equilibria in solution and volumetric analysis. Titration methods: definitions and classification. Redox equlibria and related titrations; precipitation equlibria and related titrations; acid/base equilibria (including pH calculations and speciation diagrams) and related titrations; complexation equilibria and related titrations (in particular, with EDTA). In all cases examples of prediction/interpretation of titration diagrams for model systems.

Part 3 Electroanalysis. Fundamentals, instrumentation and procedure details, and applicative examples, concerning four important electroanalytical techniques. Conductimetry (direct measurements, conductimetric titrations). Potentiometry (reference electrodes, liquid junction potentials, salt bridges; membrane potentials, ion-selective electrodes, p-Ionometry and particularly pH-metry; potentiometric titrations), Voltammetry (cyclic voltammetry, polarography, pulsed techniques, stripping techniques for trace analysis). Amperometry (amperometric titrations with three or two electrodes; trace water by Karl Fischer method; dissolved oxygen by Clark method). Biosensors and electronic tongues/noses (hints).
Teaching methods
Frontal lessons integrated with Wooclap
Teaching Resources
Recommended text: Douglas A. Skoog, Donald M. West, F. James Holler, Fundamentals of Analytical Chemistry, Brooks Cole (or corresponding Italian edition).

Pdf files of ppt slides employed by the instructor are made available on the course Ariel website.

Further text of general scope: Daniel C. Harris, Quantitative Chemical Analysis, W.H. Freeman & Co. (or corresponding Italian edition).
For those interested in further progress in the mathematical description of acid/base equilibria and corresponding titration curves: Robert De Levie Aqueous Acid-Base Equilibria and Titrations, Oxford Chemistry Primers.
Laboratory of analytic chemistry
Course syllabus
Lessons [16 hours] Concentration and concentration scales. Dilutions. Laboratory materials and reagents. Instrumentation for mass and volume measurements. Analytical methods characteristics, prediction and analysis methodologies. Safety regulations. Good laboratory practice. General principles of qualitative analytical chemistry. General principles of acid-base, precipitation, complexometric and redox titrations. General principles of conductimetry, potentiometry and pH-metry, amperometry. Survey of experimental procedures.
Lessons second part [12 hours]
Quality control of the chemical products and processes. The seven basic tools: Flow charts, Control charts, Scatter diagrams, Cause-and-effect diagrams (Ishikawa), Pareto charts, Histograms, Check sheets. Hints about the Quality Control ISO 9001 Norm.
Numerical exercises [8 hours] Calculations concerning solution preparation and titrations. Excel electronic spreadsheet use for experimental data treatment.
Numerical exercises second part [8 hours]
Excel electronic spreadsheet use for the preparation and implementation of the quality control tools.
Teaching methods
Lessons integrated with WOOCLAP, numerical/PC exercises, exercises integrated with MOODLE platform, laboratory experiments
Teaching Resources
Lessons Power Point presentations, model electronic spreadsheets, solved exercises, laboratory experimental procedures. All this material is available and downloadable from the MyARIEL web site.
Recommended text: Douglas A. Skoog, Donald M. West, F. James Holler, Fundamentals of Analytical Chemistry, Brooks Cole.
Kaoru Ishikawa, Guide to Quality Control, Asian Productivity Organization.
Analytic chemistry
CHIM/01 - ANALYTICAL CHEMISTRY - University credits: 6
Lessons: 48 hours
Laboratory of analytic chemistry
CHIM/01 - ANALYTICAL CHEMISTRY - University credits: 6
Practicals: 12 hours
Laboratories: 20 hours
Lessons: 32 hours