Analytical chemistry I with lab

A.Y. 2021/2022
Overall hours
Learning objectives
(a) Theory module (Chimica Analitica I)
Getting acquainted with fundamental definitions and concepts in Analytical Chemistry. Learning elements of error analysis and statistics, particularly applied to analytical chemistry. Discussing at a more advanced level, also in terms of activities, acid/base, redox, precipitation and complexation equilibria in aqueous solutions, also applied to the interpretation of titration curves in volumetric analysis. Getting to know at basic level a first family of instrumental analytical techniques, i.e. the electroanalytical ones; in particular conductimetry, potentiometry, voltammetry and amperometry will be discussed, to understand their theoretical background as well instrumental and applicative issues.
(b) Laboratory module (Laboratorio di Chimica Analitica I)
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.
Expected learning outcomes
(a) Theory module (Chimica Analitica I)
- Acquaintance with fundamental definitions and concepts in Analytical Chemistry
- Ability to apply basic error analysis and statistics to estimate reliability and significance of analytical data, also in connection with the laboratory module.
- Ability to manage solution equilibria and electrode potentials also in terms of ionic activities, and to exploit them for prediction and interpretation of titration curves based on acid/base, precipitation, complexation and redox equilibria, as concurrently practiced in the laboratory module.
- Basic knowledge of fundamentals, procedures and applications of electroanalytical techniques (conductimetry, potentiometry, voltammetry, amperometry), some of them possibly practiced in the laboratory module.

(b) Laboratory Module (Laboratorio di Chimica Analitica I)
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 syllabus and organization

Single session

Lesson period
Second semester
a) Theory module (Chimica Analitica I)

The Course teaching activities will be subject to the health safety requirements for the containment of the Covid-19 epidemic, as required by the ministerial indications and by the regulations and by the Rectoral and/or Academic Senate circulars, as well as by the indications of the Director of the Chemistry Department
Therefore, lessons can be provided, with the same programme, in streaming mode (or in mixed mode i.e. streaming + classroom with reduced occupancy) employing a convenient platform like Zoom or Teams, and also making videorecorded lessons available to students on the Ariel course website
. Further interactions with single students or student groups, for explanations, discussions, further advances... could be made using the Teams platform, or the Ariel course website, besides of course email exchanges.
As already specified, in pandemy times (a) the first examination part can be done in telematic oral mode, rather than in written mode, on the same programme; (b) the second examination part, oral in any case, can be done in telematic mode insteadof in presence
Prerequisites for admission
Fundamentals of general and inorganic chemistry, stoichiometry principles, fundamentals of mathematics.
Assessment methods and Criteria
a) Theory module ( Chimica Analitica I)

The theory module implies
· An examination on the first two course parts, written and in presence as regular mode (2 hours; questionnaire including brief open-answer questions, exercises and problems on the subjects treated, grouped in eight sections). In peculiar cases the same examination can also be done in oral mode; in particular, in pandemy times, in telematic oral mode on a convenient platform. In this case the committee will propose to each candidate to answer questions as well as to set up resolutions of short exercises/problems, for the same eight subject sections.
· An oral examination on the third course part (electroanalytical techniques). During pandemy times, it could be done in telematic mode on a convenient platform.
Both examinations must be successfully passed.
The theory course is integrated with the laboratory one, for which the examination mode is described below.

b) Laboratory module (Laboratorio di Chimica Analitica I)

Written Exam (2 hours) based on 5 questions with long open answers. In particular: 2 exercises on stochiometric/analytical calculations + 2 questions related to laboratory experiments and 1 question on the theoretical part of the course.
The laboratory booklet and the two intermediate reports will be evaluated during the laboratory period.
Analytical chemistry I
Course syllabus
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. Recalling fundamental thermodynamic parameters of chemical and electrochemical systems and processes. Chemical potentials, standard states, equilibrium constants. Galvanic chains, Nernst law, electrochemical cells and ion-reversible electrodes, electrode potential scale.

Part 2 Equilibria in solution and volumetric analysis. Titration methods: definitions and classification. Redox equlibria and related titrations; precipitation equlibria and related titrations; acid/base equilibria (including pH calculations and speciation diagrams) and related titrations; complexation equilibria and related titrations (in particular, with EDTA). In all cases examples of prediction/interpretation of titration diagrams for model systems.

Part 3 Electroanalysis. Fundamentals, instrumentation and procedure details, and applicative examples, concerning four important electroanalytical techniques. Conductimetry (direct measurements, conductimetric titrations). Potentiometry (reference electrodes, liquid junction potentials, salt bridges; membrane potentials, ion-selective electrodes, p-Ionometry and particularly pH-metry; potentiometric titrations), Voltammetry (cyclic voltammetry, polarography, pulsed techniques, stripping techniques for trace analysis). Amperometry (amperometric titrations with three or two electrodes; trace water by Karl Fischer method; dissolved oxygen by Clark method). Biosensors and electronic tongues/noses (hints).
Teaching methods
Teaching Resources
Recommended text: Douglas A. Skoog, Donald M. West, F. James Holler, Fundamentals of Analytical Chemistry, Brooks Cole (or corresponding Italian edition).

Pdf files of ppt slides employed by the instructor are made available on the course Ariel website.

Further text of general scope: Daniel C. Harris, Quantitative Chemical Analysis, W.H. Freeman & Co. (or corresponding Italian edition).
For those interested in further progress in the mathematical description of acid/base equilibria and corresponding titration curves: Robert De Levie Aqueous Acid-Base Equilibria and Titrations, Oxford Chemistry Primers.
Laboratory of analytical chemistry I
Course syllabus
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].
Teaching methods
Lessons, numerical/PC exercises, laboratory experiments
Teaching Resources
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.
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
Corso A
Professor: Falciola Luigi
Corso A + B
Professors: Falciola Luigi, Pifferi Valentina
Corso B
Professor: Pifferi Valentina
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
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.