Learning objectives
<br />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. <br />A critical discussion of equipments, procedures and interpretation of test results is emphasised.
Prerequisites
<br />General and Inorganic Chemistry<br />Organic Chemistry I<br />Physical I<br />Physical II<br />Analytical Chemistry
Course unit content
<br />Introduction to instrumental analytical methods <br />Classification of analytical techniques <br />Criteria for the choice of analytical methods.<br />Method performance characteristics: linearity, sensitivity, limit of detection, limit of quantitation, accuracy (trueness and precision), selectivity. <br />Calibration methods: external standard method, standard addition method, internal standard method.<br /> <br />Spectroscopic techniques<br />Fundamentals of spectrophotometry.<br />Molecular Absorption and Fluorescence UV-vis Spectrophotometry.<br />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.<br />Molecular Absorption IR Spectrophotometry.<br />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.<br />Atomic Absorption Spectrophotometry.<br />Atomic spectra. Instrumentation: hollow cathod lamp, atomizers (flame atomizer, graphite furnace). Spectral and non spectral interferences. Background correction systems. <br />Atomic Emission Spectrophotometry.<br />Instrumentation: ICP source, high-resolution monochromators, detectors.<br />X-ray Fluorescence Spectroscopy.<br />Fundamentals. Instrumentation: wavelength dispersion system (WDS), energy dispersive X-ray fluorescence (EDXRF).<br />X-ray Diffraction.<br />Fundamentals and instrumentation <br />Mass Spectrometry.<br />Fundamentals. Instrumentation: electron ionization source, chemical ionization source, analyzers (magnetic sector, quadrupoles, ion trap, time-of-flight), detector. <br /> <br />Electroanalytical techniques<br />Theory and application of voltammetry: linear scanning voltammetry, differential pulse voltammetry, anodic stripping voltammetry.<br /> <br />Separation techniques<br />Theory and application of chromatography. Gas chromatography and liquid chromatography. <br />Chromatographic parameters. Retention time. Capacity factor. Selectivity factor. Resolution. Band broadening and column efficiency: van Deemter curve for gas chromatography and liquid chromatography.<br />Gas chromatography<br />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. <br />Liquid chromatography<br />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.<br />Electrophoresis<br />Theory and application of electrophoresis. Gel electrophoresis. Capillary zone electrophoresis. Electroosmotic flow. Instrumentation (modes of injection, detectors). <br />
Bibliography
<br />D.C. Harris, Chimica Analitica Quantitativa, Zanichelli, 1992. <br />D.A. Skoog, J.J. Leary, Chimica Analitica Strumentale, SES, 1995. <br />D.A. Skoog, D.M. West, F. J. Holler, Fondamenti di Chimica Analitica, EdiSES, 1998. <br />K.A. Rubinson, J.F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002.
Teaching methods
<br />Lectures.<br /> <br />Written and oral examination
