Knolewdge acquired:
Improvement of the knowledge on features, performances and applications of the most used instrumental analytical methodologies. The course improves the methods described in the Analytical Chemistry II course and adds new techniques used in environmental and pollution studies.
Competence acquired
The course is focused on the improvement of the knowledge of the most largely used instrumental analytical methods applied to environmental studies and anthropic contamination monitoring, HPLC, IC, SFC and SEC chromatographic methods, gel- and capillary-electrophoresis, flow injection analysis, sensors and biosensors, bioanalytical approaches;
Skills acquired (at the end of the course):
Together with the Analytical Chemistry II course, this course allows a basic knowledge of the majority of instrumental analytical methodologies.
This knowledge is propaedeutical to the activities carried out inside the Environmental Analytical Chemistry I course, second level degree (Laurea Magistrale) in Chemical Sciences.
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Teaching Methods
CFU:6
Total hours of the course (including the time spent in attending lectures, seminars, private study, examinations, etc...):
150
Hours reserved to private study and other indivual formative activities:
Contact hours for: Lectures (hours):
54
Contact hours for: Laboratory (hours):
0
Contact hours for: Laboratory-field/practice (hours):
0
Seminars (hours): 0
Stages: 0
Intermediate examinations: 0
Further information
Availability within the usual working timeframe at the Department (9:00-18:00), according with teacher engagements and, possibly, after phone call (phone number 055 457 3314) or e-mail (maria.minunni@unifi.it) contact.
Type of Assessment
Oral examination
Course program
Liquid-phase chromatography: adsorption, partition, ion exchance, size esclusion.
High Performance Liquid Chromatography (HPLC): principles, instrumental set, applications. Isocratic and gradient separations. Pumping systems. Sample injection systems.
Bonded-phase HPLC. Normal- and reversed-phase chromatography. Stationary phases in HPLC. Eluent kinds for partition normal- and reversed-phase HPLC. Use of organo-siloxanes (C1, C8, C18) as stationary phase in reversed-phase HPLC. Snyder polarity index. Examples of the effect of eluent on HPLC normal- and reversed-phase HPLC. Step separations. Gradient separation with linear or non-linear gradient. HPLC detectors. Ion conductivity detectors. Spectrophotometric and fluorescence detectors. Refractometer detectors. Electrochemical detectors.
Ion chromatography. Principles of ion exchange separations. Selectivity coefficient. Anion and cation exchange processes. Instrumental setup of an ion chromatograph system. Ion exchange resins: macro-porous, micro-porous, pellicular.
Cross-linked polystyrene-divinylbenzene (PS-DVB) resins. Functional groups for anion and cation exchange. Conductivity, amperometric, voltammetric, polarographic detectors. UV-Vis spectrophotometric detectors. Post-column derivatization systems. Determination of heavy-metals by PAR derivatization.
Size-Exclusion Chromatography (SEC). Principles and features. Performances and applications of SEC. Examples of SEC separations.
Supercritical-Fluid Chormatography (SFC). Features, performances and applications. Mobile phases in SFC. Separation examples. Critical temperature, critical pressure and critical point for some chemical components: CO2, N2O, NH3, n-butane. Separation of PAH by SFC. FID detectors for SFC. Coupling systems with GC-MS detectors. Spectrophotometric, spectrofluorimetric and thermo-ionic detectors. Comparison among SFC, HPLC and GC separations.
Electro-separations. Principles and applications of electrophoresis. Migration mean-rate. Temperature effects on convection. Electrophoresis in gel matrices and in capillary systems. pH effect on protein separation. Iso-electric point. Gel-elettrophoresis. Separation of proteins and DNA or RNA fragments (outline). Electro-focusing methods. Discountinuous gels and pore-gradient gels. Detection of migration zones in Gel-Electrophoresis. Immobilization by ibridization. Iso-electric focusing. Capillary Electrophoresis. Principles and features. Electro-osmotic flow. Contemporaneous separation of anions and cations. Capillary Micellar Electrokinetic Chromatography.
Fourier Transform instrumentation.
Flow Injection Analysis (FIA). Method principles and applications. Examples of automised analytical procedures. Process flow charts. Steady-state and transient systems. Controlled dispersion of the sample band in FIA systems. Delay time. Half-height time. One-channel and multi-channel FIA. Two-channel FIA. Examples and applications. Instrumental setup, features, performances and applications.
Peak resolution in FIA systems.
Sensor and biosensors and their application to environmental analysis; Bioanalytical approaches to environmental problems.