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

MODULE 1 - WATER ENVIRONMENTAL ANALYSIS 

4 ECTS, 40 hours (2 ECTS frontal lessons, 16 hours; 2 ECTS laboratory exercises, 24 hours)

General aspects of the chemical toxicological analysis of the water matrix: reference legislation; type of water (classification based on origin, use and destination); classification of the main water contaminants.

Water sampling procedures and storage methods.

Sample preparation methods: liquid-liquid extraction (LLE), solid phase extraction (SPE), micro-extraction (SPME) in solid phase and stir bar sorptive extraction(SBSE). 

Instrumental analytical methods for the determination of contaminants in the water matrix:

Atomic spectroscopy (absorption and emission spectroscopy): principles of the technique. Instrumentation. Applications in water analysis.

UV-VIS absorption spectroscopy: summary of the principles of the technique. Instrumentation. Quantitative analysis by derivative spectrophotometry, differential spectrophotometry and by multi-component analysis. Application to chemical-toxicological analysis. Characteristics and limits of the technique.

Molecular fluorescence spectroscopy: summary. Quenching. Applications.

Chromatographic techniques: liquid chromatography and gas chromatography. Theory and practice, instrumentation, types of detection and their influence on analytical parameters. Application to environmental and biological samples.

 

MODULE 2 - ENVIRONMENTAL ANALYSIS IN AIR AND SOIL MATRICES

4 ECTS, 40 hours (2 ECTS frontal lessons, 16 hours; 2 ECTS laboratory exercises, 24 hours)

Outline of the main legislative references concerning the monitoring of air and soil quality, with a specific focus on analytical methods and requirements.

Analytical method validation referred to environmental applications (air and soil samples): validation parameters according to the main international guidelines.

Air

Emissions, pollution, waste disposal.

Workplace health and indoor/outdoor pollution.

Air matrix sampling techniques: outdoor/indoor sampling, active/passive samplers.

Pre-treatment of air samples: adsorption/desorption, bubblers, impingers, denuders, derivatisation.

Instrumental analytical methods for the determination of air contaminants: UV-Vis spectrophotometry also coupled to chromatographic techniques (HPLC, GC).

Soil

Soil, soil slurry, waste: characteristics and features.

Types of samples and sampling procedures.

Preliminary treatment of soil samples (solids or fluids), pre-treatment techniques and procedures: solvent extraction, accelerated solvent extraction (ASE and PSE), supercritical fluid extraction (SFE), solid phase extraction (SPE), molecularly imprinted solid phase extraction (MISPE), microextraction with packed sorbent (MEPS).

Instrumental analytical methods for the determination of contaminants in soils: UV-Vis spectrophotometry also coupled to chromatographic techniques (HPLC, GC), solid state analysis (IR, FT-IR, Raman, XRF).

Mass spectrometry: ionisation techniques, types of sources, mass analysers and acquisition modes (SRM, MRM). Applications to the qualitative and quantitative analysis of environmental samples of different nature.

Chiral instrumental analysis: enantioselective separations, chiral stationary phases, chiral selectors. Qualitative and quantitative applications to the analysis of contaminants in air and soil.

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 is divided into 2 modules. Each module consists of lectures (16 h, 2 CFU) during which the main instrumental techniques, required for the analysis in environmental matrices will be discussed. The course deals also with laboratory activities (24 h, 2 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 Marina Naldi

See the website of Michele Protti