Analytical chemistry I with lab

A.Y. 2017/2018
Lesson for
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.

Course structure and Syllabus

Active edition
Yes
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 B
Professor: Guglielmi Vittoria
Analytical chemistry I
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: conductimetry, potentiometry, voltammetry, amperometry.

Acquired skills
Criteria for evaluating the reliability of analytical data; ability to interpret acido/base, precipitation, complexation and redox equilibria, particularly concerning titration curves; basic knowledge of the fundamental electroanalytic techniques (conductimetry, potentiometry, voltammetry, amperometry)

Course content
Part 1 Propedaeutic concepts Analytical Chemistry: definition, history, significance. Analytical methods. Sequence of steps in a typical quantitative analysis. Sampling. 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 Volumetric analysis. Titration methods: definitions, classification, standards. Acid/base, precipitation, complessation and redox titrations: mathematical descriptions of the corresponding equilibria and titration diagrams; in particular, De Levie method for easy unapproximated simulation of acid/base equilibria and titration curves even in very complex cases.

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.

Reference material
- Lecture notes and model spreadsheets provided on the instructor's website.
Recommended textbook
- Douglas A. Skoog, Donald M. West, F. James Holler, Fundamentals of Analytical Chemistry, Brooks Cole. (or, as an alternative: Daniel C. Harris, Quantitative Chemical Analysis, W.H.Freeman & Co.)


Prerequisites
Fundamentals of general and inorganic chemistry, basic stoichiometry, elements of mathematical analysis and of numerical methods.

Assessment method
Written examination (3 hours) on the whole program, divided into 3 sections, corresponding to the 3 parts of the course. The sections concerning propaedeutic concepts and volumetric analysis include several questions requiring short answers, plus a lot of short numerical exercises/little problems (requiring a pocket scientific calculator). The electroanalysis section includes three subsections with many questions requiring short answers (on i) conductimetry; ii) potentiometry; iii) voltammetry & complements).


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
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 pasta), complexation (water hardness) and redox (iron determination) titrations [16 hours]. Amperometry: dead stop end point amperometric detection of Vitamin C in real samples [4 hours].

Suggested prerequisites
General and inorganic chemistry Course with Lab

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 or ARIEL sites.
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.

Assessment method
Written Exam (2 hours): 4 questions with long open answers (1 exercise on stochiometric/analytical calculations; 2 questions related to laboratory experiments; 1 question related to 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
Falciola round: http://users.unimi.it/ELAN
Guglielmi round: instructor ARIEL site
Lesson period
Second semester
Lesson period
Second semester
Assessment methods
Esame
Assessment result
voto verbalizzato in trentesimi
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