INSTRUMENTAL ANALYTICAL CHEMISTRY I
Learning outcomes of the course unit
The course aims to provide students with a thorough knowledge of major instrumental analytical techniques, including spectroscopic techniques, separation techniques, hyphenated techniques and electroanalytical techniques.
A critical discussion of equipments, procedures and interpretation of test results is emphasised.
General and Inorganic Chemistry
Organic Chemistry I
Course contents summary
Introduction to instrumental analytical methods
Classification of analytical techniques
Criteria for the choice of analytical methods.
Method performance characteristics: linearity, sensitivity, limit of detection, limit of quantitation, accuracy (trueness and precision), selectivity.
Calibration methods: external standard method, standard addition method, internal standard method.
Fundamentals of spectrophotometry.
Molecular Absorption and Fluorescence UV-vis Spectrophotometry.
The nature of electronic transitions. Instrumentation for molecular absorption UV-vis spectrophotometry: sources, monochromators (prism, diffraction grating), detectors. Photodiode array detector. Definition of trasmittance and absorbance. Lambert-Beer law and deviations. Applications to quantitative analysis. Instrumentation for molecular fluorescence UV-vis spectrophotometry. Effect of temperature on the fluorescence quantum yield.
Molecular Absorption IR Spectrophotometry.
Modes of molecular motion; vibrational modes and absorption regions. Factors that influence the frequency of absorption. Characteristic IR absorption frequencies. Instrumentation: FT-IR spectrophotometer. Applications of IR spectrophotometry to the characterization of organic compounds.
Atomic Absorption Spectrophotometry.
Atomic spectra. Instrumentation: hollow cathod lamp, atomizers (flame atomizer, graphite furnace). Spectral and non spectral interferences. Background correction systems.
Atomic Emission Spectrophotometry.
Instrumentation: ICP source, high-resolution monochromators, detectors.
X-ray Fluorescence Spectroscopy.
Fundamentals. Instrumentation: wavelength dispersion system (WDS), energy dispersive X-ray fluorescence (EDXRF).
Fundamentals and instrumentation
Fundamentals. Instrumentation: electron ionization source, chemical ionization source, analyzers (magnetic sector, quadrupoles, ion trap, time-of-flight), detector.
Theory and application of voltammetry: linear scanning voltammetry, differential pulse voltammetry, anodic stripping voltammetry.
Theory and application of chromatography. Gas chromatography and liquid chromatography.
Chromatographic parameters. Retention time. Capacity factor. Selectivity factor. Resolution. Band broadening and column efficiency: van Deemter curve for gas chromatography and liquid chromatography.
Gas-solid chromatography (GSC). Gas-liquid chromatography (GLC). Stationary phases for GSC and GLC. Instrumentation: injectors, columns, detectors. Capillary columns. Universal and selective detectors. Gas chromatography-mass spectrometry. Isothermal gas chromatography. Temperature-programmed gas chromatography. Internal standard calibration method for quantitative determinations.
Mechanisms of separation: adsorption chromatography, partition chromatography, ion chromatography, size-exclusion chromatography. Instrumentation for HPLC: injection valve, columns, pumps, detectors. Isocratic elution, gradient elution. Liquid chromatography- mass spectrometry: electrospray source.
Theory and application of electrophoresis. Gel electrophoresis. Capillary zone electrophoresis. Electroosmotic flow. Instrumentation (modes of injection, detectors).
D.C. Harris, Chimica Analitica Quantitativa, Zanichelli, 1992.
D.A. Skoog, J.J. Leary, Chimica Analitica Strumentale, SES, 1995.
D.A. Skoog, D.M. West, F. J. Holler, Fondamenti di Chimica Analitica, EdiSES, 1998.
K.A. Rubinson, J.F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002.
Lectures. Students are always expected to participate actively in all forms of training.
Examination is in the form of a formal written exam and an oral exam individualy.