55006 - Chemical Toxicological Analysis I

Learning outcomes

At the end of the course the student will have the basic theoretical and practical knowledge to carry out chemical-toxicological analyses. In particular the student is able to: - know the analytical characteristics of pollutants with particular reference to water and soil pollutants - understand the main methods of analysis of pollutants under existing law - apply specific methodologies and analytical techniques through single seat exercises.

Course contents

Program of lectures and laboratory experiments

Chemical-toxicological analysis aims and problems. Peculiar characteristics of the chemical-toxicological analysis applied to the environmental monitoring.

Method validation referred to the environmental application: validation parameters according to the international guidelines.

Sampling method and pretreatment of environmental matrices: classical methods of extraction, solid phase extraction (SPE), MicroExtraction by Packed Sorbent (MEPS), Disposable Pipette tip Extraction (DPX), Stir Bar Sorptive Extraction (SBSE), Single Drop MicroExtraction (SDME) and Dispersive Solid Phase MicroExtraction (DSPME).

Instrumental separation techniques: liquid chromatography (HPLC, UHPLC, and nano-LC) and capillary electrophoresis (CE). Specific principles of each analytical technique and instrumentations. Application to environmental samples or samples of different typologies.

Types of detection, principles of their operation, coupling to separation techniques and effects on analytical performance.

UV-Vis absorption spectroscopy: instrumentation, quantitative analysis, calibration curve, first derivative spectrophotometry, differential spectrophotometry and by multicomponent analysis. Applications to the chemical-toxicological analysis of complex matrices.

Molecular fluorescence spectroscopy: instrumentation, quantitative analysis, analysis by quenching. Coupling to separative techniques: native fluorescence, pre-and post-colomn derivatization. Applications to environmental monitoring.

Mass spectrometry: ionization techniques (ESI, APCI, MALDI), types of sources, mass analyzers (QqQ, TOF, Iontrap, Orbitrap) and acquisition Mode (SRM, MRM). Analysis of samples of different origin and composition.

Instrumental chiral analysis: enantioselective separations, chiral stationary phases, chiral selectors. Quantitative applications.

Readings/Bibliography

Slides discussed during the course. 
Papers from the scientific literature discussed during the course. 
Handout of the laboratory experiments.

ONLY FOR CONSULTATION:
- Holler J.F., Crouch S.R. “Fondamenti di Chimica Analitica” di Skoog & West, EdiSES s.r.l., 2015.

- Skoog D.A., Holler J.F., Crouch S.R., Sabbatini L. “Chimica Analitica Strumentale”, EdiSES s.r.l., 2009.

- Hage D.S., Carr J.D. "Chimica Analitica e Analisi Quantitativa", Piccin, 2012.

Teaching methods

The course consists of lectures (32 h, 4CFU) during which the main instrumental techniques, required for the analysis in environmental matrices will be discussed. The course deals also with laboratory activities (48 h, 4 CFU), during which the student will prepare a laboratory handbook. The laboratory activities offer the student the opportunity of carrying out different analyses for identification and determination in environmental matrices and of firsthand using the instrumentation required to perform such analyses.

Assessment methods

The assessment of the learning aims to assess practical skills and theoretical knowledge acquired by the student while attending the lectures and the laboratory experiences. In particular the following skills will be evaluated:

- Mastery of the advanced instrumental analytical terminology and of the theoretical basis of the discussed topics;

- Ability to perform routine laboratory procedures for the quali-quantitative analysis;

- Specific training on the uses, reactions, toxicity and analytical procedures of the examined compounds;

- Critical capacity in the evaluation of the laboratory analytical results.

The assessment of the learning is done on the basis of an oral examination consisting of some questions about both the theoretical and the practical parts. During the laboratory experiences it is planned to carry out practical tests the results of which are reported by the students within his/her own laboratory notebook which is controlled periodically by the teacher and which is part of the final score.

Teaching tools

Lectures will be carried out by means of the common electronic media (pc, tablet and similar devices). The practical activities will be developed in specially equipped laboratories where students can have a single place of work, instrumentation and materials necessary for the environmental analysis.

Office hours

See the website of Laura Mercolini