ANALYTICAL CHEMISTRY
Learning outcomes of the course unit
The Course of Analytical Chemistry aims to provide students with a solid background on the skills needed for the understanding and application of the most popular analytical techniques independently and in a multidisciplinary approach with other subjects offered by the program in Chemistry and Pharmaceutical Technology.
Among the areas of Analytical Chemistry, the course aims at training the student's four main areas: 1) calculations for the preparation of solutions and samples, expression of the analytical result, basics of statistical treatment of the data, 2) equilibria in solution, pH, solutions buffer, titration, 3) molecular and atomic spectroscopic methods, and 4) knowledge of the main separation techniques (GC, HPLC, CE) and the main detectors. The course aims to teach the student to develop the ability to liaise between the topics covered in class and interdisciplinary topics taught in other courses, to develop the ability to propose solutions to analytical problems and develop an analytical-technical language of communication.
Prerequisites
Students should have the basis of general chemistry.
Course contents summary
BASIC CONCEPTS
EVALUATION OF ERRORS: SYSTEMATIC ERRORS, CASUAL ERRORS.
ACID-BASE EQUILIBRIA. PH. BUFFER SOLUTION. TITRATIONS.
ANALYTICAL METHOD VALIDATION: ICH GUIDELINES.
SAMPLE TREATMENT
SPECTROPHOTOMETRIC METHODS: UV-VIS, FLUORESCENCE, IR
CHROMATOGRAPHIC METHODS: GASCHROMATOGRAFY, LIQUID CHROMATOGRAPHY.
CAPILLARY ELECTROPHORESIS
MASS SPECTROMETRY: ELECTRON IMPACT SOURCE, CHEMICAL IONIZATION, ELECTROSPRAY.
Course contents
Analytical Chemistry
BASIC CONCEPTS: unit of measurement, solutions, concentrations, dilution calculations. Preparation of standard solutions. Conversion between the different ways of expressing concentrations.
Errors in chemical: DEFINITION OF RANDOM ERROR, systematic error, blunder. CALCULATION OF RANDOM ERROR, SD AND METHODS FOR REPORT THE ANALYTICAL DATA. SYSTEMATIC EVALUATION OF ERROR.
Definition of acids and bases. Autoprotolysis and ionic product of water. Calculating the pH of solutions of acids and strong bases. Definition of weak acids and bases. Dissociation constant. Calculating the pH of solutions of acids and weak bases. Polybasic acids. Calculation of pH of polyprotic acids.
Distribution curves of the species at equilibrium as a function of pH. Percentage of ionization of molecules of pharmaceutical interest as a function of pH. Acid-base indicators.
Calculation of the pH of salt solutions.
Buffer solutions. Calculation of the pH of buffer solutions. Buffering capacity.
Principles of volumetric analysis. Acid-redox titrations base.Titolazioni. Complexometric titrations. Titration of precipitation.
Instrumental Analytical Chemistry
Introduction to analytical chemistry: qualitative analysis and quantitative analysis. Classical methods and instrumental methods of analysis.
Validation of analytical methods. Quality parameters: accuracy (trueness and precision), limit of detection, limit of quantification, calibration curves and linearity range, sensitivity, selectivity.
Development of an analytical method.
Techniques to sample processing: Calculation of the extraction yield.
Solvent extraction, extraction in gas phase, solid phase microextraction, solid phase extraction (SPE), supercritical fluid extraction (SFE), extraction with microwaves.
Introduction to spectrophotometric methods. Definition of radiation. Energy levels. Interaction between radiation and matter: absorption, emission, fluorescence. Lambert-Beer's law. Instrumentation for spectrophotometric methods: sources, wavelength selectors, sample holder, the detectors. Sources: tungsten, deuterium, hollow cathode lamp. Selectors wavelength filters and monochromators. Detectors: photomultiplier tubes and elettromoltiplicatori.
Atomic absorption spectroscopy: principles and instrumentation. Atomizer flame. Interference with flame atomizer. Electrothermal atomizer. Applications.
Molecular absorption spectroscopy UV-Vis: principles and instrumentation. Electronic transitions. Definition of chromophore groups and auxocromi. Batocromico effect, effect ipsocromico, hyperchromic effect and hypochromic effect. Effect of the solvent. Applications: qualitative and quantitative analysis.
Molecular IR absorption spectroscopy: principles and instrumentation. Types of vibration. Identification of functional groups in organic molecules.
Introduction to the methods of chromatographic analysis. Principle of chromatographic separation. Classification of chromatographic methods. Parameters characterizing the chromatographic peak. Qualitative and quantitative analysis. Resolution. Efficiency. Factors determining peak broadening (Van Deemter equation).
Optimization of conditions for analysis of complex mixtures: isocratic or gradient elution in liquid chromatography, elution isothermal or programmed temperature gas chromatography.
Gas chromatography: principles and instrumentation. Injection mode. Types of columns and stationary phases. Detectors: a thermal conductivity, flame ionization, electron capture. Applications.
Liquid chromatography: principles and instrumentation. Mechanisms: adsorption, distribution (direct phase and reverse phase), ion exchange, size exclusion. Types of columns and stationary phases. Selection of the mobile phase. Detectors: a refractive index, molecular absorption UV-Vis, fluorescence, conductivity. Applications.
Capillary electrophoresis: principles and applications.
Mass spectrometry: principles and instrumentation. Source electron impact, chemical ionization, electrospray. Coupling GC-MS and HPLC-MS. Applications: qualitative and quantitative analysis.
Recommended readings
D.C. Harris “Chimca analitica quantitativa” Zanichelli
Holler, Skoog, Crouch, Chimica Analitica Strumentale, EdiSES
Teaching methods
During the lectures will be shown the theoretical aspects of the techniques and analytical methods provided by the program. The theoretical aspects will be supplemented by examples of applications in the clinical-pharmaceutical industry. The course will be supplemented by exercises in the classroom in order to provide students with a means of learning and debate the issues raised.
The lectures are supplemented by handouts, exercises, and recorded lessons available on the websites of the Campusnet Teacher Lisa Elviri (http://farmacia.unipr.it/cgi-bin/campusnet/docenti.pl/Show?_id=elviri) and LEA WEB Learning in University (http://lea.unipr.it/course/index.php) Farmacia.
Assessment methods and criteria
The student will have the opportunity to: support three written tests in progress and upon successful go directly to the final oral examination or a written exam at the end of the course and if successful access the oral examination.
The written exams will include both exercises that questions of description and connection of the arguments.
The student must have as a minimum the basic knowledge on all points of the proposed program for the Course of Analytical Chemistry and properties of scientific language. We will also evaluate the student's ability to interconnect the various topics covered during the course and in an interdisciplinary manner, as well as the ability to affronare and solve analytical problems inherent in the issues carried out.
