55006 - Chemical Toxicological Analysis I

Learning outcomes

At the end of the course the student has the basic theoretical and practical knowledge to perform chemical-toxicological analysis. In particular, the student will be able to: - know the analytical characteristics of pollutants with particular reference to water and soil pollutants - understand the main methods of analysis of pollutants by current legislation - apply specific methodologies and analytical techniques through laboratory pratice in single place.

Course contents

MODULE 1 - ENVIRONMENTAL ANALYSIS IN THE WATER MATRIX

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, stir-bar sorptive extraction (SBSE).

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

• Atomic absorption spectroscopy: principles of the technique. instrumentation. Applications in water analysis.
• UV-VIS absorption spectroscopy: summary of the principles of the technique. Lambert's law Beer and quantitative analysis. Lambert Beer deviations. Instrumentation. Quantitative analysis by first derivative spectroscopy, differential spectrophotometry and by multi-component analysis. Application to chemical-toxicological analysis. Characteristics and limits of the technique.
  
• Chromatographic techniques: Definition of chromatographic parameters. Van Dempter equation. Liquid chromatography: instrumentation, separative approaches, types of elution (isocratic, gradient), types of detectors, qualitative and quantitative analysis. Thin layer chromatography (TLC): instrumentation, detection, qualitative and quantitative analysis, two-dimensional TLC. Gas chromatography: instrumentation, types of elution, detector types. Environmental applications.

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)

General aspects of the chemical toxicology analysis of the air matrix: outline of the main legislative references on the monitoring of air and soil quality.

Air matrix

Air quality monitoring and air quality index. Outdoor pollution: main pollutants. Indoor pollution: main pollutants and their sources. Atmospheric monitoring: sampling strategies, sampling locations, time of sampling, type of sample, sample size. Sampling of aeriforms: samplers (glass containers, plastic bags, canisters). Pollutant sampling: absorption sampling (impregnated filters, denuders, detecting vials and diffusion tube); adsorption sampling (adsorbent tubes and vials, diffusion samplers, SPME); condensation at low temperatures. Direct reading devices. Sampling efficiency. Erosol sampling: HI-VOL sampler; inverted sampler and impactors.

Soil matrix

Main soil components; soil types, soil properties. Sampling: purpose of the sampling, choice of the area to be sampled, number of samples to be taken, location of the sampling. Types of sampler: shirt samplers, ring samplers, core samplers and Beeker sampler.

 

Methods for the preparation of the sample for the soil matrix: extraction with solvent, accelerated extraction with solvent (ASE and PSE), extraction with supercritical fluid (SFE), solid phase extraction (SPE), Molecularly Imprinted Solid-phase Extraction (MISPE), Micro Extraction by Packed Sorbent (MEPS).

Instrumental analytical methods for the determination of contaminants in the air matrix and in the soil matrix (in addition to those already included in module I of the course):

• Physical constants determination: refractive index and rotational power.
• Molecular fluorescence spectroscopy: summary of the principles of the technique, quantum yield, Stokes Shift, instrumentation, quantitative analysis, excimer formation, derivatization.
• Infrared spectroscopy: principles, instrumentation and interpretation of a spectrum.
• Chromatographic techniques. Gas chromatography: instrumentation, types of elution, detector types. Environmental applications.
• Mass spectrometry: ionization techniques, types of sources, mass analyzers and acquisition modes (SRM, MRM). Applications to the qualitative and quantitative analysis of environmental samples of various origins.

Readings/Bibliography

Slides

Teaching methods

The course is divided into 16+16 hours (4+4 CFU) of lectures in which the main instrumental techniques applied to the analysis of environmental samples will be discussed. The course will be accompanied by 24+24 hours (4+4 CFU) of laboratory exercises during which the student will compile a laboratory book. The exercises are intended to provide each student with the possibility of applying analytical methods for the identification and determination in environmental matrices and to personally use the instrumentation necessary for the execution of such analyses.

Assessment methods

The learning assessment aims to assess the theoretical and practical skills acquired by the student during the lectures and laboratory experiences. In particular, the following skills are verified:
- Mastery of instrumental analytical terminology and theoretical bases of teaching subjects
- Ability to carry out the normal laboratory operations of qualitative and quantitative chemical-toxicological analysis
- Specific preparation concerning the uses, reactions, toxicity and analytical procedures of the compounds examined
- Critical ability in the evaluation and interpretation of analytical laboratory results.

The verification is carried out on the basis of an oral exam which consists of some questions concerning both the theoretical part and the practical part of the laboratory. During laboratory exercises, practical tests are carried out, the outcome of which is reported by the student in his own laboratory notebook and which is an integral part of the final score.

Teaching tools

Lectures will be conducted with the support of electronic media (PCs, tablets and connected devices). The practice will be carried out in specially equipped educational laboratories where students will have a single work place, the instrumentation and materials necessary for environmental chemical-toxicological analysis.

Office hours

See the website of Marina Naldi