Learning objectives
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.
Prerequisites
Organic and Bioorganic Chemistry
Course unit content
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.
Spectroscopic techniques
Fundamentals of spectrophotometry.
Molecular Absorption and Fluorescence UV-vis Spectrophotometry. 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). Non spectral interferences.
Atomic Emission Spectrophotometry. Instrumentation: ICP source, high-resolution monochromators, detectors.
Mass Spectrometry. Fundamentals. Instrumentation: electron ionization source, chemical ionization source, analyzers (magnetic sector, quadrupoles, ion trap, time-of-flight), detectors.
Separation techniques
Theory and application of chromatography. Gas chromatography and liquid chromatography.
Chromatographic parameters. Retention time. Capacity factor. Selectivity factor. Resolution. Band broadening and column efficiency.
Gas 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.
Liquid chromatography. Mechanisms of separation: adsorption chromatography, partition chromatography, ion chromatography, size-exclusion chromatography. Instrumentation for HPLC: injection valve, columns, pumps, detectors. Isocratic elution, gradient elution.
Bibliography
K.A. Rubinson, J.F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002.
Holler, Skoog, Crouch, Chimica Analitica Strumentale, II edizione, EdiSES, 2009
Teaching methods
Academic teaching. Interactive teaching.
