Chemical and Toxicological Analysis 1

A.Y. 2019/2020
Overall hours
Learning objectives
The aim of the course is to provide the student with the basic knowledge necessary to understand the principles of the most common methods of classical and instrumental quantitative analysis.
These skills, in general terms, are the following:
· Know the problems related to sampling, to the processing of samples to be prepared for analytical procedures, to interference;
· Knowing how to use the most appropriate analytical techniques (in relation to those treated);
· Knowing how to organize and carry out laboratory activities in conditions of personal and environmental safety.
The basic theoretical aspects are treated in the 1st Module; in the 2nd Module the laboratory tutorials are carried out.
Expected learning outcomes
The student will be able to critically discuss most common quantitative analytical techniques, including both classic and instrumental methods. He will also acquire knowledge and skills required to:
· solve the problems associated with sampling and treatment of samples
· select suitable analytical techniques to solve a given analytical problem
· describe an analytical procedure and correctly report an analytical result
· organize and carry out laboratory activities following high quality and safety standards.
Course syllabus and organization

Single session

Lesson period
Second semester
Course syllabus
INTRODUCTION · Revision of the basic stoichiometric knowledge useful in chemical analysis · The analytical process as a decision-making sequence · Classification of analysis methods
DATA MEASUREMENT AND DATA PROCESSING · Meaning and classification of experimental errors · Statistical treatment of experimental data: errors in analytical chemistry, statistics of errors, tests of significance, error propagation, significant figures, calibration (external calibration, standard additions, internal calibration), least squares fitting, characteristics of an analytical procedure (accuracy, precision, specificity and selectivity, linearity range, LOD, LOQ, robustness).
PRELIMINARY STEPS OF THE ANALITICAL PROCESS· Sampling · Preliminary analytical operations · Sample preparation· Analytical process: errors in analytical process, sampling, sample treatment and clean-up, reference materials.
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.

INTRODUCTION TO THE LABORATORY · Laboratory description · Mass and volumetric measures · Safety in the laboratory
MEASUREMENT METHODS · Calculation of equivalence point by means of graphic methods · Method of calibration curve · Standard additions analysis · Correlation and regression of two variables, Least square methods, calibration curve, LOD, LOQ.
VOLUMETRIC ANALYSIS · Titration of hydrogen peroxide in a disinfectant solution ·Determination of Cl- concentration in a hair shampoo ·Determination of SO2 concentration in a white wine·Review of the operations used for the analysis
INSTRUMENTAL ANALYSIS · Excel poftware programs for titration curves, calibration curves and evaluation of some statistical parameters · UV-VIS Spectrophotometric determinations of various analytes in water (method of calibration curve, LOD and LOQ): ammonium ions, sulphates and phosphates · pH measurements of aqueous solutions and titration of phosphoric acid in Cola· TLC Separation of components in a pharmaceutical tablet · Voltammetric determinations of metals in different materials.
Prerequisites for admission
Knowledge of fundamentals of general chemistry and analytical chemistry.
Teaching methods
Teaching Unit 1: Lessons: 48h (6 CFU)
Teaching Unit 2: Laboratory Tutorials: 80h (5 CFU)
Teaching Resources
· C. Rubino, I. Venzaghi, R. Cozzi - Le basi dell'analisi chimica (Teoria) Ed. Zanichelli, 2012
· C. Rubino, I. Venzaghi, R. Cozzi - Le basi dell'analisi chimica (Laboratorio) Ed. Zanichelli, 2012
· R. Cozzi, P. Protti, T. Ruaro - Elementi di analisi chimica strumentale - Ed. Zanichelli, 2013
· D. C. Harris - Chimica analitica quantitativa (seconda edizione italiana) Ed. Zanichelli, 2005
Assessment methods and Criteria
The final examination will consist of an oral test (1 hour). The basic stoichiometric knowledge useful in chemical analysis (2 questions or exercises) will be initially evaluated. All the theoretical subjects presented during Lessons and Laboratory tutorials will be critically discussed as well (2-3 questions).
Module 1
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 6
Lessons: 48 hours
Professor: Pinto Andrea
Module 2
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 5
Practicals: 16 hours
Single bench laboratory practical: 64 hours
on demand, to be scheduled via email
Via L. Mangiagalli 25, first floor, room 1066