67031 - Instrumental Analytical Chemistry and Laboratory Laboratory

Learning outcomes

The laboratory class is aimed to provide educational experiences which challenge students to act in an instrumental chemistry laboratory. Students are required to follow experiments and encouraged to familiarise to both instrumental aspect and analytical methodology of the proposed analytical technique. Each experiment session must ends with the motivated evaluation of the analytical data, performed with the appropriate statistical test.

 

Course contents

Terms associated with instrumental analysis. Principal types of real analysis. Numerical criteria for selecting analytical methods. Steps in solving an analytical problem. General rules for sampling and sample preparation. Quality assurance of analytical measurements.

    Statistics of instrumental analysis. Sensitivity and detection limit. Calibration graph in instrumental analysis. Regression and correlation. Confidence limits for a concentration determined by using an unweighted regression line. Standard addition. 

    Elements of an analytical instrument. Signals. Transducers and detectors. Signal to noise ratio.

   Spectrometric techniques. A deeper look to UV-Vis molecular absorption spectrometry: instrumentation and analytical measurements. Atomic spectrometry. Flame atomic absorption spectrometry. Electrothermal atomizers. Flame emission spectrometry. Inductively coupled plasmas.

   Chromatographic techniques. Column processes and band broadening. Plate height equation. Gascromatography. High-performance liquid chromatography. Ion chromatography. 

  Electroanalytical techniques. Electrogravimetric analysis. Ion-selective electrode potentiometry. Voltammetry with applications.

  The combined techniques in analytical chemistry.

  Some practical examples of instrumental analysis in action in everyday life.

Laboratory Experiments

The following experiments will be the subject of the laboratory class:

 

1. Conductivity and Potentiometry. Evaluation of the cell constant. Titration of strong acid with strong base using glass electrode and evaluation by means of      Gran's plot.

2. High Performance Liquid Cromatography (HPLC) 1. Parameters optimization

3. High Performance Liquid Cromatography (HPLC) 2.  Analysis of real samples.

4. Cyclic voltammetry. Determination of iron(III)hexacyanoferrate. Determination of diffusion coefficient of iron(III) hexacyanoferrate in solution.

5. Atomic Absorption Spectroscopy (AAS). Determination of Fe in a sample of wine by two methods: method of standard addition, and method of calibration curve.

6. UV-Vis Molecular Absorption Spectroscopy. Extractive separation of metals. Determination of the extraction curve.Spectroscopic determination of pKa.

 

 

 

Readings/Bibliography

1. D.C. Harris, Chimica Analitica Quantitativa, Zanichelli, 2005
2. K. A. Rubinson, J. F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002
3. J.C. Miller and J.N. Miller, Statistics and Chemometrics for Analytical Chemistry, 6th ed., Prentice Hall (UK), 2010
4. A.D. Skoog, J.F. Holler and S.R. Crouch, Chimica Analitica Strumentale, Edises, 2009

Assessment methods

Oral exam. Evaluation of laboratory experiments.

The experiment reports will be compiled by the group manager after all the experiments have been done, and they should be filled up using the experimental data contained in the laboratory notebook of each component of the group.

Teaching tools

Laboratory classes starts with a series of short lectures for the laboratory experiences. The laboratory classes are scheduled on afternoon, where students are grouped several team of four student each: the manager, the chemist, the hardware, the software.  The group schedule is determined at the beginning of each academic year. Students should have a bound laboratory notebook for recording all the data at the time of the observation during laboratory classes. The recording of data on loose pieces of paper or in a preliminary note book is expressly forbidden.

Office hours

See the website of Marco Taddia

See the website of Barbara Ballarin

See the website of Sergio Zappoli

See the website of Marco Giorgetti