Analytical chemistry I with lab

A.Y. 2018/2019
12
Max ECTS
120
Overall hours
SSD
CHIM/01
Language
Italian
Learning objectives
Acquisition of procedures and basic calculations in Analytical Chemistry; mastery titrations and colorimetric techniques of electroanalytical base.
Expected learning outcomes
Applying basic statistics to estimate reliability and significance of analytical data, also in connection with the laboratory module.
Managing solution equilibria and electrode potentials, also in terms of ionic activities, and application for prediction and interpretation of titration curves based on acid/base, precipitation, complexation and redox equilibria, with full instrumental monitoring or end point detection by colorimetric indicators, also in connection with the laboratory module.
Basic knowledge of fundamental electroanalytic techniques (conductimetry, potentiometry, voltammetry, amperometry) also in connection with the laboratory module.
Course syllabus and organization

Single session

Lesson period
Second semester
Analytical chemistry I
Course syllabus
Goals
Fundamental definitions and concepts in Analytical Chemistry; Elements of statistics applied to analytical chemistry; interpretation of acid/base, precipitation, complexation and redox equilibria, with application to volumetric analysis; electroanalysis fundamentals: conductimetry, potentiometry, voltammetry, amperometry

Acquired skills
Applying basic statistics to estimate reliability and significance of analytical data, also in connection with the laboratory module.
Managing solution equilibria and electrode potentials, also in terms of ionic activities, and application for prediction and interpretation of titration curves based on acid/base, precipitation, complexation and redox equilibria, with full instrumental monitoring or end point detection by colorimetric indicators, also in connection with the laboratory module.
Basic knowledge of fundamental electroanalytic techniques (conductimetry, potentiometry, voltammetry, amperometry) also in connection with the laboratory module.


Course content [required]
Part 1 Propedaeutic concepts Analytical Chemistry: definition, history, significance. Analytical methods. Sequence of steps in a typical quantitative analysis. Sampling (hints). Elements of theory of errors applied to analytical chemistry; criteria for data treatment and statistical tests. Concentration scales, ionic strength, activities, activity coefficients. Equilibrium constants, standard states. Nernst law, galvanic cells, ion-reversible electrodes, electrode potential scale.

Part 2 Equilibria in solution and volumetric analysis. Titration methods: definitions, classification, standards. Acid/base, precipitation, complessation and redox titrations: mathematical description of the corresponding equilibria and elaboration and interpretation of titration diagrams for model systems. Speciation diagrams and Pourbaix diagrams.

Part 3 Electroanalysis. Conductimetry, potentiometry (ion-selective electrodes, pH-metry, p-Ionometry, redox potential, water hardness), voltammetry (cyclic voltammetry, polarography, pulsed techniques, stripping techniques for trace analysis), amperometry (trace water by Karl Fischer method, dissolved oxygen by Clark method), biosensors and electronic tongues/noses (hints). Fundamentals, instrumentation, protocols (standardization, direct measurements, instrumental titrations). Model cases in the analytical laboratory and in fundamental and applied research.

Suggested prerequisites
General and Inorganic Chemistry and General and Inorganic Chemistry Laboratory; Mathematics courses.


Reference material
Recommended general scope textbook: Douglas A. Skoog, Donald M. West, F. James Holler, Fundamentals of Analytical Chemistry, Brooks Cole (or corresponding Italian edition)
Supporting material and model electronic spreadsheets provided by the instructor (available on her website under password)
Other general scope textbook: Daniel C. Harris, Quantitative Chemical Analysis, W.H. Freeman & Co. (or corresponding Italian edition)
For a deeper insight and attractive treatment of acid base equilibria and corresponding titration curve: Robert De Levie, Aqueous Acid-Base Equilibria and Titrations, Oxford Chemistry Primers.

Prerequisites
Fundamentals of General and Inorganic Chemistry; basic stoichiometric calculations: elements of mathematical analysis and of numerical methods.

Assessment method
The global mark of the Analytical Chemistry and Laboratory of Analytical Chemistry I Course will be assigned combining the marks obtained for the theoretical and experimental modules (details concerning the latter evaluation are provided in the corresponding
Concerning the evaluation of the theoretical module, it will consist in
A 3-hour written examination concerning the program Part 1 and 2 (mainly problems and exercises, plus several short questions)
A 15-minutes oral examination concening the program Part 3 (electroanalytical techniques). Students can register for this interview, enabling them to complete the examination and to receive their global mark for the entire course, after having passed both the above written examination and the laboratory module examination.

Language of instruction
Italian

Attendance policy
Attendance is strongly recommended

Mode of teaching:

Traditional


Website:
http://users.unimi.it/ECEA
Laboratory of analytical chemistry I
Course syllabus
Goals
Knowledge of the procedures, the experimental protocols and the fundamental calculations in Analytical Chemistry. Knowledge of colorimetric titrations and of the basic electroanalytical techniques: conductimetry, potentiometry, amperometry.

Acquired skills
Use, also at experimental level, of the basic analytical techniques: colorimetric titrations and fundamental electroanalytical methodologies. Use of an electronic spreadsheet for data treatment. Principles of statistical data treatment and error theory.

Course Content
Lessons [16 hours] Concentration and concentration scales. Dilutions. Laboratory materials and reagents. Instrumentation for mass and volume measurements. Analytical methods characteristics, prediction and analysis methodologies. Safety regulations. Good laboratory practice. General principles of acid-base, precipitation, complexometric and redox titrations. General principles of conductimetry, potentiometry and pH-metry, amperometry. Survey of experimental procedures.
Numerical exercises [8 hours] Calculations concerning solution preparation and titrations. Excel electronic spreadsheet use for experimental data treatment.
Laboratory experiments [48 hours]
1) Volumetric analysis with colorimetric indicators: preparation of standard solutions, acid/base titrations (KHPh, TRIS, vinegar, bicarbonates), complexation titrations (water hardness with EDTA), precipi¬tation titrations (chlorides with Mohr and Fajans methods), redox titrations (iodine, ascorbic acid) [24 hours].
2) Electroanalysis: Conductimetry: conductimeter calibration, direct measurement of specific con¬ducti¬vi¬ty, conductimetric titrations [4 hours]. Potentiometry: ion-selective electrode assembling, calibra¬tion and use for direct p-Ion determination; pH-meter standardization and direct pH measurements; potentiometric acid/base (HCl, HCl+CH3COOH, unknown aminoacid detection), precipitation (chlorides in egg pasta), complexation (water hardness) and redox (iron determination) titrations [16 hours]. Amperometry: dead stop end point amperometric detection of Vitamin C in real samples (tablets and fruit juices) [4 hours].

Suggested prerequisites
General and inorganic chemistry Course with Lab, Mathematics Courses.

Reference Material
Lessons Power Point presentations, model electronic spreadsheets, solved exercises, laboratory experimental procedures. All this material is available and downloadable from the instructors' web site.
Recommended text: Douglas A. Skoog, Donald M. West, F. James Holler, Fundamentals of Analytical Chemistry, Brooks Cole.
Alternatively: Daniel C. Harris, Quantitative Chemical Analysis, W.H. Freeman & Co.


Prerequisites
Fundamentals of general and inorganic chemistry, stoichiometry principles, fundamentals of mathematics.

Assessment method
Written Exam (2 hours) based on 4 questions with long open answers. In particular: 2 exercises on stochiometric/analytical calculations + 2 questions related to laboratory experiments and/or the theoretical part of the course.
The laboratory booklet and the two intermediate reports will be evaluated during the laboratory period.

Language of instruction
Italian

Attendance Policy
Obligatory

Mode of teaching
Traditional

Website
http://users.unimi.it/ELAN
Analytical chemistry I
CHIM/01 - ANALYTICAL CHEMISTRY - University credits: 6
Lessons: 48 hours
Laboratory of analytical chemistry I
CHIM/01 - ANALYTICAL CHEMISTRY - University credits: 6
Laboratories: 48 hours
Lessons: 24 hours
Shifts:
Corso A
Professor: Falciola Luigi
Corso A + B
Professor: Falciola Luigi
Corso B
Professor: Pifferi Valentina
Professor(s)
Reception:
Every Day from Monday to Friday, 9-18, by appointment
by Professor's Office in via Golgi 19, Building 5A, West Wing (Electrochemistry), III floor, room 3114-O
Reception:
From Monday to Friday, between 8.30 and 18.30, by appointment (to be requested by email))
Normally in my office (Chemistry Department, West Wing, First Floor). Currently, on account of the pandemy, on the Teams platform in videoconference mode.