Teacher
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D'ANNIBALE Alessandro
(syllabus)
Analytical techniques and methods - Procedures and protocols - Concatenation of actions in the definition of an analytical problem - Guide criteria in the choice of an analytical technique - Precision - Accuracy - Required sensitivity and detection limit - Calibration and construction of a dose-signal curve - correlation diagrams - Pearson coefficient - Non-linear dose-signal relationships and transformation algorithms - Dynamic range - Preparation of standards starting from stock solutions - Signal correction strategies - Blank preparation (procedural and matrix blank solution) - External standard method - Standard addition method and unknown concentration calculation procedures - Internal standard method - Sources of errors in the analytical chain (sampling - sample preparation - analysis) - Types of matrix - Alternative sample treatment procedures - Elimination of interferents - Elimination strategies of the matrix effect (separative approaches, matrix modifiers, selective precipitation, masking methods, saturation methods and matrix matching) - Wet decomposition in an open environment - Decomposition assisted by microwave - Decomposition and for combustion - Quality control in the laboratory - Control Papers (eg. Shewhart chart and Westgart rules) - Validation of a method - Validation by comparison and correlation diagrams - Repeatability and reproducibility - Reference materials and certified reference materials (CRM) - Suppliers and CRM selection criteria - Definition and measurement of uncertainty - Horwitz equation - Compound standard uncertainty and extended uncertainty - Calculation of the LOD and LOQ - Reference parameters for the validation of a method - Measurement range - Dynamic range - Accuracy and exactness - Selectivity - Sensitivity - Robustness and solidity - Sampling - general information on errors connected to this phase - representativeness and homogeneity - integrity - Objectives and phases of a sampling - Current regulations regulating food sampling (horizontal and vertical) - Batch extraction strategies (simple, stratified or systematic randomization) Sample reduction strategies (cone and surface quarters) - Batch, sub-batch, primary sample definitions , aggregate sample, aliquot and sample unit - Examples of sampling strategies for matr Solid and liquid foodstuffs - Sampling procedures for packaged and bulk products - Sampling and sample storage devices (characteristics and materials of the containers) - Transport plan and reception procedures - Sample compliance criteria - Sampling of gases and volatile species - liquid sampling - Preparation of the laboratory sample - Determination of the number of samples to be analyzed - Chemistry laboratory - Classification of commercial chemicals - CLP regulation - GHS labeling and H and P phrases - Pictograms - Safety data sheets - Handling and storage of reagents - Water purification - deionization and reverse osmosis - glass equipment (graduated and non-graduated glassware) - devices for measuring and dispensing liquids (class A and class B) - Scales for mass measurements and associated measurement errors - Errors in measurements - Systematic and random errors - Identification and elimination of systematic errors - Treatment of random errors - Statistical parameters of dispersion - Confidence limits - Student's t - Identification of outliers - Grubbs test - Dixon test - Significance of the differences between sample means - F test - Analysis of variance - Significant figures in the measurement of quantities - Concentration expressions (molarity, formality and normality) - Preparation of solutions with known titre - Cross rule in dilutions - Extraction techniques in the liquid phase (liquid distribution - liquid: separating funnel, steam distillation, SDE extractor; liquid phase extraction under pressure - PLE solid-liquid partition: the Soxhlet system, ultrasonic or microwave extraction); solid phase extraction (SPE, SPME, Purge and Trap); extraction in supercritical (SFE) and sub-critical (ASE) phase - Nature of electromagnetic radiation - Wave and corpuscular properties of electromagnetic radiation - Energy of a photon - Interactions between radiation and matter - Energy transitions - Maxwell Boltzmann's law - Absorption - Rules selection - Emission - Fluorescence and phosphorescence - Luminescence - UV-Vis spectroscopy - Characteristic electronic transitions - Impact of the structure on the spectral behavior - Chromophores and Auxochromes - Hyperchromic and hypochromic effect - Hypsochromic and batochromic shift - Relation between absorbance and transmittance - Relation between absorbance and concentration: Lambert-Beer law - Molar extinction coefficient - Deviations from the Lambert-Beer law - Isosbestic point - UV-Vis spectrophotometers - Light sources - Monochromators with filters and dispersing elements (prism and diffraction and reflection gratings) - Interference and diffraction - Detectors - Photocells - Photomultipliers - Solid state detectors (photodiodes) - diode array detectors - Types of spectrophotometers (single beam, double beam, multi-channel) - Bandwidth of the bandwidth - Photometric resolution and linearity - Baseline stability - General applications and food analysis: pKa determination, kinetic studies, enzymatic assays - Determination of free amino acids, proteins, total and reducing sugars, fatty acids, total lipids and polyphenols Line atomic spectra - Principles of atomic spectroscopy - Principal electronic transitions - Spectral line widening (Lorentz, Doppler effect) - Resonance wavelength - Maxwell-Boltzmann law - - Absorption, emission and fluorescence - Atomic absorption: instrumentation - Chopper and oscillating mirrors - Light sources (HCL, EDL) - Atomization techniques: Flame, Electrothermal (graphite oven), Thermal decomposition of hydrides (some elements of the IV, V and VI groups), Chemical reduction (CV, cold vapors, only for Hg), Inductively coupled plasma (ICP) - Applications to food analysis - Spectral interferences - Non-spectral interferences (chemical, physical, ionization interferences) - Interference mitigation strategies - Continuous source systems - Zeeman systems - Smith system -Hieftje - Coverage of elements by AAS - Atomic Emission Spectrometry (AES) - Inductively Coupled Plasma (ICP) - ICP-AES - ICP-MS - Quadrupole Mass Analyzers - introduction to chromatographic methods of analysis - Solute-phase interactions - Planar and column chromatography - Classification based on the separation mechanism (Adsorption, Partition, Ion exchange, Molecular exclusion and Affinity) - Direct and inverse phase chromatography - Eluotropic series of solvents - General principles of chromatography - Distribution coefficient - capacity factor - selectivity - efficiency: HETP and number of theoretical plates - Speed theory: Van Deemter's law - Resolution - Examples of chromatographic parameters calculation - HPLC - principles - Pumping systems - injectors - columns - detectors (UV, diode-array, refractive index, ELSD, coulometric, fluorescence) - solvents and phase modifiers - isocratic and gradient elutions - HPLC-MS- ESI and ISI - HPLC applications in the agro-food sector - Gas Chromatography - Principles and Equipment - Packed Columns and Capillaries (PLOT and WCOT) - Injectors and Alternating Systems sample introduction actives - Isothermal and gradient elutions - Detectors (FID, ECD, NPD, TCD, MS) - GC applications to the agro-food sector - Electrophoresis - migration velocity and electrophoretic mobility - Titration curves of charged analytes - Vertical and horizontal electrophoretic devices - Power supplies - Ohm's law and Joule effect - Free phase electrophoresis - Zonal electrophoresis - Factors affecting resistance in anti-convective media - Paper electrophoresis - agarose and polyacrylamide gel electrophoresis - Degree of cross-linking and porosity of polyacrylamide gel - discontinuous systems and gradient gels - stroke markers and face ratio - SDS-PAGE - molecular weight determination - IEF-PAGE - determination of the isoelectric point - two-dimensional electrophoresis - Preparative electrophoresis - Protein staining (Coomassie, Silver staining) and nucleic acids (methylene blue, ethidium bromide and silver staining) - Activity staining (zymograms) - Food sector applications
(reference books)
• Lecture notes • Harris “Chimica analitica quantitativa” ed. Zanichelli; • Wilson & Goulding “Biochimica Applicata” ed. Cortina; • Rubinson & Rubinson “Chimica analitica Strumentale” Zanichelli.
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