ANALYTICAL CHEMISTRY WORKSHOP

Degree course: 
Corso di First cycle degree in ENVIRONMENTAL AND NATURAL SCIENCES
Academic year when starting the degree: 
2023/2024
Year: 
1
Academic year in which the course will be held: 
2023/2024
Course type: 
Basic compulsory subjects
Language: 
Italian
Credits: 
6
Period: 
Second semester
Standard lectures hours: 
80
Detail of lecture’s hours: 
Lesson (16 hours), Exercise (16 hours), Laboratory (24 hours)
Requirements: 

There are no rules of prerequisites but it is useful to have basic notions of mathematics, (exponential notation, logarithms, equation of first and second degree).

Final Examination: 
Orale

The objective of the final exam is to verify the level of achievement of the educational objectives, first of all by assessing the possession of the basic cognitive elements and then the student's ability to use them independently to solve real problems.
The exam will consist of a written test (2h), an oral test and the evaluation of the field work report.
This report, to be delivered within the times defined during the course and indicated on the e-learning web site, will not be corrected and evaluated “a priori”, but exclusively during the oral exam. The Student, therefore, will have to deliver a paper that precisely follows the indications on the compilation of the reports present on the e-learning, under penalty of a negative, non-appealable, evaluation.
Written test:
- 2 numerical exercises on solving laboratory problems, including field activities;
- 1 question of theory and laboratory practice.
Each test will be awarded 10 points: to access the oral exam it is necessary to obtain at least 5 points for each single question.
The oral exam will consist of:
1) discussion of the written test
2) brief exposition of practical/theoretical topics of the course
3) discussion of practical laboratory test reports
The resulting assessment will appropriately take into account written, oral and laboratory reports: the relative weight of the tests is distributed so that the laboratory part weights for 15/30, while the theoretical part, written and oral, for the remaining 15/30. The assessment will take into account the expressive ability and the use of correct terminology, but above all the student's ability to connect the various topics of the course will be taken into account, not as a mere answer to a specific question, but as an answer to a specific environmental problem. Therefore, the critical capacity will be emphasized rather than the theoretical knowledge of the topics.

Note: the written text is valid only for the booking session.

Assessment: 
Voto Finale

Acquisition of
• Analytical Chemistry laboratory ability and introduction to theory and practice of modern instrumental analytical techniques.
• Field sampling ability, including pre-treatment and conservation of analytical samples
• judgment autonomy to evaluate and critically interpret, chemical and phyical-chemical experimental data according to analyzed environment.
• adequate skills in statistical treatment and evaluation of analytical data
• “on field” teamwork ability and evaluation of referenced data.

The course is structured in a theoretical part (16h), a part of compulsory exercises preparatory to laboratory activities (16h) and a laboratory part which includes an "in-door" preparatory laboratory (24h) and a field laboratory (24h) . Attendance at the laboratories is compulsory in accordance with the teaching regulations of the course.
The purpose of the in-door laboratory is to provide the chemical "tools" sufficient to carry out the sequence of operations foreseen by the analytical protocol adopted and evaluate the results, even with simple statistical tools, evaluating the possible interaction with the lithological structure of the area of sampling.
The theoretical part is structured in lectures on topics related to laboratory applications. See the extended program for details of the hours and lessons provided in flipped learning mode.
- General introduction to the course; the analytical protocol
- Chemical equilibria in analytical chemistry: acid-base, complexation, redox; Titration concept; introduction to acid-base titrations.
- Introduction to chromatographic techniques; ion chromatography; calibration lines.
- Introduction of spectroscopic techniques; Lambert-Beer law, calibration lines.
- Characteristic chemical-physical parameters of natural water: temperature, pH, conductivity, dissolved oxygen.
The preparatory exercises precede the laboratory experiences and are intended to introduce the student to correct laboratory practices, including safety protocols:
- NOMENCLATURE: chemical equipment nomenclature; laboratory safety
- TITRATION: primary secondary standards, NaOH and HCl: application lesson on titrations, primary and secondary standards; explanations first laboratory experience: NaOH titration and HCl titration.
- HARDNESS + WINKLER: titrations by complexation and by oxidation-reduction; explanation of laboratory experiences: determination of total hardness and determination of dissolved oxygen.
- WATER ANALYSIS, GENERALITIES, SAMPLING: introduction to the protocol for water analysis according to EEA; sampling: protocol and practical modalities.
- WATER ANALYSIS, ION BALANCE; BICARBONATE LAB - GRAND PLOT - IC: end of water analysis protocol; potentiometric analysis of alkalinity, Gran's method; IC analysis of natural waters.
- PORTABLE INSTRUMENTS: use of field instruments.
- PREPARATION OF “Gavirate”, “Gravedona”, “Ventina” EXITS.
The laboratory includes the following experiences and field trips:
- use of analytical instruments for measuring volumes; use of technical balance and analytical balance;
- acid-base titrations
- titrations by complexation: determination of hardness
- use of portable instrumentation, use of portable kits for determining alkalinity and hardness;
- potentiometric titration of carbonates in natural waters, ion chromatography, Winkler, COD.

- exit at Gavirate (u 4h*).
- Gravedona exit (u 8h*).
- exit Alpe Ventina – Chiareggio (u 12h*).

*Note: outings may be modified or subject to passing educational tests and/or replaced by integrated laboratories in the event of a lack of adequate hospitality facilities or for serious organizational reasons
The topics covered, as well as acquiring the necessary knowledge for dealing with both basic and advanced issues relating to the application of analytical protocols useful for water analysis, will also allow developing the ability to apply the acquired knowledge to problems related to the context environment and to acquire skills in terms of communication skills, the ability to critically approach and autonomously judge the scientific topics covered.

The theoretical part is structured in lectures on topics related to laboratory applications:
- General introduction to the course; the analytical protocol (3h).
- Chemical equilibria in analytical chemistry: acid-base (flipped learning), complexation (flipped learning), redox (flipped learning); titration concept; introduction to acid-base titrations (4h).
- Introduction to chromatographic techniques; ion chromatography; calibration lines (3h).
- Introduction of spectroscopic techniques; Lambert-Beer law, calibration lines (flipped learning) (3h).
- Characteristic chemical-physical parameters of natural water: temperature, pH, conductivity, dissolved oxygen (3h).

The preparatory exercises precede the laboratory experiences and are intended to introduce the student to correct laboratory practices, including safety protocols:
- NOMENCLATURE: chemical equipment nomenclature; laboratory safety (2h)
- TITRATION: primary secondary standards, NaOH and HCl: application lesson on titrations, primary and secondary standards; explanations first laboratory experience: NaOH titration and HCl titration (2h).
- HARDNESS + WINKLER: titrations by complexation and by oxidation-reduction; explanation of laboratory experiences: determination of total hardness and determination of dissolved oxygen (2h).
- WATER ANALYSIS, GENERALITIES, SAMPLING: introduction to the protocol for water analysis according to EEA; sampling: protocol and practical methods (2h).
- WATER ANALYSIS, ION BALANCE; BICARBONATE LAB - GRAND PLOT - IC: end of water analysis protocol; potentiometric analysis of alkalinity, Gran's method (flipped learning); IC analysis of natural waters (2h).
- PORTABLE INSTRUMENTS: use of field instruments (2h).
- PREPARATION OF EXITS “Gavirate”, “Gravedona”, “Ventina” (2h).
The laboratory includes the following experiences and field trips:

- use of analytical instruments for measuring volumes; use of technical balance and analytical balance (4h);
- acid-base titrations: HCl and NaOH (4h+4h)
- titrations by complexation: determination of Calcium and Magnesium ions in commercial mineral waters (4h);
- use of portable instruments (T, pH, conductivity, DO, colorimetric kits), use of portable kits for determining alkalinity and hardness (4h);
- potentiometric titration of carbonates in natural waters, ion chromatography, Winkler, COD (4h).

- exit at Gavirate (u 4h*).
- Gravedona exit (u 8h*).
- exit Alpe Ventina – Chiareggio (u 12h*).

*Note: outings may be modified or subject to passing educational tests and/or replaced by integrated laboratories in the event of a lack of adequate hospitality facilities or for serious organizational reasons

Convenzionale

The educational objectives of the course will be achieved through an interdisciplinary approach, which is divided into frontal lessons (16h) on theoretical topics, also using the "flipped learning" teaching method if the topics resume topics already covered in the General Chemistry course of the 1st semester, laboratory exercises (16h) preparatory to laboratory experiences, a series of practical laboratory experiences (24h) and practical internships in the area (24h), to familiarize the student with the problems of environmental analysis in the field. The practical experiences in the field will be developed both in lake and mountain environments, paying particular attention to the problems of sample collection and analysis, the processing of analytical data and the drafting of a repeatable analysis protocol.
Field lessons and laboratory exercises are essential for the achievement of practical recognition skills. These activities are mandatory and provided with the co-presence of doctoral students or master's students. For students with certified particular problems (work, certified illness, disability, minor children, etc.) the study trip activities will be replaced by supplementary activities to be agreed individually according to the problems. Students who, in the absence of valid reasons, should not participate in the aforementioned activities, will have to pass a supplementary laboratory test. If they fail, they will have to repeat the laboratory.

Student reception:
study of the teacher, CUBO via Valleggio, 9, Como;

appointment by e-mail on the address of the course labanaliticafcb@uninsubria.it

Slides texts: see-e-learning

Recommended reference text (the chapters being studied are shown on the e-learning page of the course)
- F.W. Fifield & P.J.Haines; Environmental Analytical Chemistry, Blackwell Science

Recommended texts not mandatory
- D.C. Harris, Elements of Analytical Chemistry, Zanichelli

- S.E. Kegley and J Andrews, "The Chemistry of Water", University Science Book.

- L.H. Keith, "Environmental Sampling and Analysis: A Practical Guide", Lewis Publ.