Chemical and Toxicological Analysis 1
A.Y. 2023/2024
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.
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.
· 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.
Lesson period: Second semester
Assessment methods: Esame
Assessment result: voto verbalizzato in trentesimi
Single course
This course can be attended as a single course.
Course syllabus and organization
Single session
Responsible
Lesson period
Second semester
Course syllabus
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.
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.
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: 64h (5 CFU); Class Tutorial: 16h (1CFU)
Teaching Unit 2: Laboratory Tutorials: 64h (5 CFU); Class Tutorial: 16h (1CFU)
Teaching Resources
Slides of the lectures and laboratory tutorial procedures are available on ARIEL website.
Recommended texts:
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
Recommended texts:
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).
Specific procedures for exams to students with disabilities or specific learning disabilities (DSA) will be applied. Here the complete information:
https://www.unimi.it/en/study/student-services/services-students-specific-learning-disabilities-sld
https://www.unimi.it/en/study/student-services/services-students-disabilities
In case you need specific procedures, please inform the teacher by mail at least 10 days before the exam, including in the addresses [email protected] or [email protected]
Specific procedures for exams to students with disabilities or specific learning disabilities (DSA) will be applied. Here the complete information:
https://www.unimi.it/en/study/student-services/services-students-specific-learning-disabilities-sld
https://www.unimi.it/en/study/student-services/services-students-disabilities
In case you need specific procedures, please inform the teacher by mail at least 10 days before the exam, including in the addresses [email protected] or [email protected]
CHIM/08 - PHARMACEUTICAL CHEMISTRY - University credits: 11
Practicals: 16 hours
Single bench laboratory practical: 64 hours
Lessons: 48 hours
Single bench laboratory practical: 64 hours
Lessons: 48 hours
Educational website(s)
Professor(s)