Chemical and Toxicological Analysis 1

UNIT 1:
INTRODUCTION TO THE COURSE- Review of basic stoichiometry knowledge useful in chemical analysis- The analytical process as a decision-making sequence- Classification of analytical methods
DATA MEASUREMENT AND DATA PROCESSING- Meaning and classification of experimental errors- Treatment of analytical data: expression of uncertainty of a single measurement and propagation of uncertainty in computational sequences.
PRELIMINARY STEPS OF THE ANALITICAL PROCESS- Preliminary analytical operations- Sample preparation.
VOLUMETRIC ANALYSIS · The volumetric analysis technique· Classification· Preparation of solutions and analytical methods· Error sources· Solubility and solubility product, common ion effect, effects of secondary solution equilibria.
GRAVIMETRIC ANALYSIS · The gravimetric analysis technique· Classification· Preparation of solutions and analytical methods· Error sources· The precipitation process, types of precipitates and their characteristics, homogeneous precipitation, impurities in precipitates, digestion, double precipitation, masking reagents, washing, drying and ignition, calculus for gravimetric analysis.
PRECIPITATION TITRATION· Precipitation reactions and conditions for titration· Principal titration methods in Argentometry· Calculation examples
REDOX TITRATION · Oxidizing and reducing agents· Redox reactions, electrochemical cells· Redox indicators · Redox titration curves· Titration agents · Calculation examples
ACID BASE NEUTRALIZATION TITRATION · Acid-base conjugate couples· buffer solutions· theory of acid-base neutralization titrations· acid-base titration curves, species in a buffer solution as a function of pH· polyprotic acids and bases titration curves for polyprotic acids and bases.
COMPLESSOMETRIC TITRATION · Coordination compounds · Conditions for performing a complexometric titration · Titration methods with EDTA · Metal ion masking and demasking · Calculation examples
OPTICAL METHODS OF ANALYSIS· Electromagnetic radiation · Energy of molecules and atoms · Interactions between electromagnetic radiation and matter, color · Optical analysis techniques, absorption and emission spectroscopy
UV / VISIBLE SPECTROPHOTOMETRY · The absorption of UV or visible radiation· Lambert-Beer law, deviations from the Lambert-Beer law · error in spectrophotometric measurements, derivative spectra, · ·spectrophotometers (light sources, filters and monochromators, sample cuvettes, detectors, instrument configurations)· Quantitative analysis, select the wavelength.
ATOMIC ABSORPTION SPECTROPHOTOMETRY · Atomic absorption of electromagnetic radiation · spectrophotometers (light sources, filters and monochromators, atomizers, detectors, instrument configurations) · Quantitative analysis
ATOMIC EMISSIONS SPECTROPHOTOMETRY · Flame emission· Plasma and flame spectrophotometry: general principles, spectrophotometers (light sources, filters and monochromators, atomizers, detectors, instrument configurations), ICP-spectrophotometer, ICP-OES, ICP-MS.
CHROMATOGRAPHIC METHODS · General principles of chromatographic separation and separation mechanisms · Classification of chromatographic techniques · Equations and parameters· The theoretical plate model of chromatography· Van Deemter equation, selectivity, efficiency, resolution, capacity, peak symmetry· Planar (TLC) and low pressure (column) chromatography· instrumentations and detectors.

TEACHING UNIT 2

CLASS TUTORIALS
Exercises on the topics covered in the classroom and applied to problems of interest to the chemical-toxicological analysis laboratory;
Insights into the different steps preceding the analysis of a sample: laboratory safety, sampling, laboratory glassware for instrumental analysis, calculations needed to make dilutions;
Introduction to the analytical method according to ICH regulations, calibration and calibration of an analytical instrument;
Use of excel spreadsheet for calibration line construction and calculation of unknown concentration of an analyte;
Insights into the analysis of optically active substances.
Discussion of case studies from scientific articles in the field of chemical-toxicological analysis based on the use of analytical instruments discussed in class.

LABORATORY TUTORIALS
VOLUMETRIC ANALYSIS: Application of a volumetric method for titration of polyprotic acid/base species (e.g., carbonates).
GRAVIMETRIC ANALYSIS: Gravimetric determination of sulphates in water.
SPECTROPHOTOMETRIC ANALYSIS: Spectrophotometric/colorimetric determination of inorganic and organic contaminants (e.g., total nitrites and phenols in water).
THIN-LAYER CHROMATOGRAPHY. Applications for qualitative and semiquantitative analysis in cases of chemical-toxicological interest (e.g., screening of active ingredients in pharmaceutical preparations, pesticides, PCBs).
STATISTICAL TREATMENT OF RESULTS: Statistical treatment of measurements obtained from practical experiments.
SEMI-QUANTITATIVE ANALYSES of water: determination/research of ammonia, sulphites and phosphates.