Maria RICCIARDI | INSTRUMENTAL ANALYTICAL CHEMISTRY
Maria RICCIARDI INSTRUMENTAL ANALYTICAL CHEMISTRY
cod. 0512400001
INSTRUMENTAL ANALYTICAL CHEMISTRY
0512400001 | |
DEPARTMENT OF CHEMISTRY AND BIOLOGY "ADOLFO ZAMBELLI" | |
EQF6 | |
CHEMISTRY | |
2025/2026 |
OBBLIGATORIO | |
YEAR OF COURSE 3 | |
YEAR OF DIDACTIC SYSTEM 2023 | |
FULL ACADEMIC YEAR |
SSD | CFU | HOURS | ACTIVITY | |
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CHIM/01 | 3 | 24 | LESSONS | |
CHIM/01 | 1 | 12 | EXERCISES | |
CHIM/01 | 2 | 24 | LAB |
Objectives | |
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GENERAL OBJECTIVE. THE COURSE HAS THE MAIN OBJECTIVE OF TRAINING THE CANDIDATE IN KNOWING HOW TO CARRY OUT CHEMICAL ANALYZES OF DIFFERENT MATRICES KNOWLEDGE AND UNDERSTANDING. KNOWLEDGE OF THE MAIN ANALYSIS TECHNIQUES AND UNDERSTANDING OF THE CHEMICAL-PHYSICAL FACTORS RESPONSIBLE FOR PROCESS VARIATIONS ABILITY TO APPLY KNOWLEDGE AND UNDERSTANDING. THE STUDENT WILL BE ABLE TO IDENTIFY AND OPTIMIZE ANALYSIS METHODS FOR EACH CLASS OF ANALYTE AUTONOMY OF JUDGEMENT. CORRECTLY CONDUCT AN ANALYSIS PROCESS. KNOWING HOW TO APPLY THE PRINCIPLES OF THE CHOSEN INSTRUMENTAL TECHNIQUE, EVALUATING BASED ON THE EVIDENCE WHICH PARAMETERS TO OPTIMIZE. COMMUNICATION SKILLS. KNOWING HOW TO WORK IN A GROUP IN A LABORATORY CONTEXT. KNOW HOW TO EXPLAIN THE PROBLEMS CONNECTED TO CHEMICAL ANALYSIS PROCESSES WITH PROPER LANGUAGE. LEARNING ABILITY. THE STUDENT WILL BE ABLE TO APPLY THE KNOWLEDGE ACQUIRED TO REAL CONTEXTS SIMILAR TO THOSE PRESENTED DURING THE COURSE, AND TO DELVE DEEPER INTO THE TOPICS COVERED IN SITUATIONS DIFFERENT FROM THOSE PROPOSED. |
Prerequisites | |
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BASIC KNOWLEDGE OF MATHEMATICS, PHYSICS, CHEMISTRY GENERAL INORGANIC CHEMISTRY, ANALYTICAL CHEMISTRY AND ORGANIC CHEMISTRY |
Contents | |
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LECTURE 1 COURSE OVERVIEW. EVALUATION OF ANALYTICAL TECHNIQUES. ACCURACY. PRECISION. SENSITIVITY AND SELECTIVITY. DETECTION AND QUANTIFICATION LIMITS: DEFINITIONS AND CALCULATION. INSTRUMENT RESPONSE RANGE. CALIBRATION AND STANDARDIZATION. NUMERICAL EXAMPLES. MEASURING INSTRUMENTS. UNITS OF MEASUREMENT. DIMENSIONAL ANALYSIS. ERRORS. CONCENTRATIONS. LECTURE 2 STOICHIOMETRY. BASIC EXERCISES. SOLUTION PREPARATION. SERIAL DILUTIONS. WEIGHING OPERATIONS. MICROLITER SAMPLING. LAB-SCALE OPERABILITY. PROBLEM SOLVING. BUFFER SOLUTIONS: VARIOUS PREPARATIONS. LECTURE 3 ELECTROCHEMISTRY. ELECTROCHEMICAL REACTIONS. EXTRACTION POTENTIAL. MEASUREMENT OF POTENTIAL DIFFERENCE. ELECTROCHEMICAL SERIES OF ELEMENTS. REDOX REACTIONS. OPEN CIRCUIT MEASUREMENTS. CELLS AND BATTERIES. ELECTROLYTES. ELECTRICAL CONDUCTIVITY. GROTTHUSS MECHANISM. CELL AND JUNCTION POTENTIAL. POTENTIOMETRY. NERNST EQUATION. LINEARIZATION. GRAPHICAL REPRESENTATION. IONIC STRENGTH REGULATORS. ELECTRODES AND POTENTIOMETRY. ELECTROACTIVE SPECIES. REFERENCE ELECTRODES: SSE, SCE, NHE AND RELATIVE SCALE. NERNST EQUATION FOR SSE AND SCE. FIRST, SECOND, AND THIRD KIND ELECTRODES. GRAPHICAL REPRESENTATION OF NERNST EQUATION FOR FIRST AND SECOND KIND ELECTRODES. LECTURE 4 INTERFACE AND ELECTRICAL DOUBLE LAYER. CONTACT POTENTIAL. ELECTRICAL CAPACITANCE. OVERPOTENTIALS. MEASURING ELECTRODES: CLASSIFICATION. MEMBRANE ISES. FLUORIDE ISE: RESPONSE MECHANISM. GRAPHICAL REPRESENTATION ACCORDING TO NERNST. EXAMPLE: DETERMINATION OF FLUORIDE IN TOOTHPASTE, FROM STANDARD PREPARATION TO PERCENTAGE CONCENTRATION DETERMINATION. ANION MEASURABILITY CONDITIONS. INTERFERENCES. LECTURE 5 GLASS ELECTRODE: RESPONSE MECHANISM. GRAPHICAL REPRESENTATION ACCORDING TO NERNST. ACID AND ALKALINE ERRORS. INTERFERENCES. TWO- AND THREE-POINT PH METER CALIBRATION: BUFFER SOLUTION PREPARATIONS. LABORATORY EXPERIMENT DEMONSTRATION. EXAMPLES: PH DETERMINATION. DIRECT AND INDIRECT MEASUREMENT. POTENTIOMETRIC TITRATION. LECTURE 6 MEMBRANE INDICATOR ELECTRODES FOR CALCIUM, SODIUM, POTASSIUM, AND AMMONIUM IONS: RESPONSE MECHANISMS. GRAPHICAL REPRESENTATION ACCORDING TO NERNST. INTERFERENCES. ANALYTICAL EXAMPLES. LECTURE 7 GAS-SELECTIVE ELECTRODES OR PROBES. ABSENCE OF DOUBLE ELECTRICAL LAYER. CO AND AMMONIA PROBES. RESPONSE MECHANISMS. GRAPHICAL REPRESENTATION ACCORDING TO NERNST. INTERFERENCES. ANALYTICAL EXAMPLES. LECTURE 8 BIOCATALYTIC MEMBRANE ELECTRODES. POTENTIOMETRIC BIOSENSOR FOR UREA. AMPEROMETRIC BIOSENSORS FOR OXYGEN, GLUCOSE, LACTOSE, AND SUCROSE. RESPONSE MECHANISMS. INTERFERENCES. ANALYTICAL EXAMPLES. DISSOLVED OXYGEN DETERMINATION. BLOOD GLUCOSE ANALYSIS USING LOCAL HEALTH SERVICE DEVICES. LECTURE 9 CALIBRATION AND STANDARDIZATION IN POTENTIOMETRY. STANDARD CURVE METHOD. DEVIATIONS FROM EXPECTED NERNSTIAN LINEARITY. STANDARD PREPARATION AND GRAPHICAL REPRESENTATION OF RESPONSE E VS LOGC. NUMERICAL EXAMPLES. GRAPHICAL IDENTIFICATION OF LINEAR RESPONSE RANGE. IDEAL LINES. MAIN CAUSES OF DEVIATIONS. MATRIX EFFECT. INTERFERENCES. CALCULATION ERRORS IN PREPARATION. LECTURE 10 SPECTROPHOTOMETRY. LIGHT–MATTER INTERACTION. ABSORPTION AND EMISSION OF ENERGY. ELECTROMAGNETIC RADIATION. CONSTRUCTIVE AND DESTRUCTIVE INTERFERENCES. ELECTRONIC, VIBRATIONAL, AND ROTATIONAL TRANSITIONS. RADIATIVE AND NON-RADIATIVE PROCESSES. RELAXATION. LUMINESCENCE. ATOMIC AND MOLECULAR TRANSITIONS. ATOMIC ABSORPTION SPECTRA. MOLECULAR ABSORPTION SPECTRA. ATOMIC SPECTROSCOPY. MOLECULAR SPECTROSCOPY. LECTURE 11 UV-VIS SPECTROPHOTOMETRY. COLORED SUBSTANCES. MAIN CHROMOPHORES. EFFECT OF CONJUGATION. CHLOROPHYLLS. LAMBERT–BEER LAW: DERIVATION, LIMITS, AND DEVIATIONS. APPLICATION. GRAPHICAL REPRESENTATION: ABSORBANCE AND TRANSMITTANCE. ADDITIVITY OF ABSORBANCES. EXAMPLES. CUVETTES. SOLVENT SELECTION. LINEARITY DEVIATIONS: PHYSICAL AND CHEMICAL FACTORS. SINGLE-BEAM SPECTROPHOTOMETERS WITH SINGLE/DOUBLE OPTICAL PATH. DOUBLE-BEAM SPECTROPHOTOMETERS. PHOTOMETRIC ERROR. WAVELENGTH SELECTION. SPECTROPHOTOMETER COMPONENTS. SOURCES. PRISM AND GRATING MONOCHROMATORS. BANDWIDTH SELECTION. FILTERS. PHOTOMULTIPLIER TUBES (PMT). PHOTOELECTRIC EFFECT. PHOTODIODE ARRAY DETECTOR. SEMICONDUCTOR DOPING. N-P JUNCTION. DAD. APPLICATIONS. LECTURE 12 UV-VIS SPECTROPHOTOMETRY. CALIBRATION USING STRAIGHT LINE. CORRELATION A VS C. GRAPHICAL IDENTIFICATION OF LINEAR RESPONSE RANGE. STANDARD ADDITION METHOD. ALGEBRAIC APPROACH. APPLICATION EXAMPLES: IRON DETERMINATION WITH FERROZINE, CHROMIUM WITH DIPHENYLCARBAZONE, NITRATE NITROGEN IN WATER: FROM STANDARD PREPARATION TO UNKNOWN CONCENTRATION DETERMINATION. LABORATORY EXPERIMENT ILLUSTRATION. POTABLE WATER SAMPLE COMPLIANCE WITH LEGISLATIVE DECREE 18/2023. SPECTROPHOTOMETRIC TITRATIONS. LECTURE 13 UV-VIS SPECTROPHOTOMETRY. ANALYTICAL METHODS FOR WATER. IRSA-APAT-CNR. ENVIRONMENTAL CONSOLIDATED ACT. LEGISLATIVE DECREES 18/2026 AND 152/2006. SPECTROPHOTOMETRIC DETERMINATION OF ALUMINUM, BORON, CHROMIUM, LEAD, IRON, AND COPPER. COLORIMETRIC METHODS IN CLINICAL CHEMISTRY. NADP(H)-BASED ASSAYS. ENZYMATIC METHODS FOR GLUCOSE, LACTATE, UREA, FREE AND TOTAL CHOLESTEROL, TRIGLYCERIDES, IRON. COLORIMETRIC METHODS IN FORENSIC CHEMISTRY. CHEMILUMINESCENCE. LUMINOL. LECTURE 14 ATOMIC SPECTROSCOPY: ABSORPTION AND EMISSION. AAS SPECTROPHOTOMETER. HDL AND HR-CS SOURCES. BANDWIDTH. DOPPLER EFFECT. ATOMIZATION METHODS: FLAME. BURNERS. NEBULIZERS. FUELS AND OXIDANTS FOR F-AAS. INTERFERENCES. MATRIX EFFECTS. FLAME ALIGNMENT. BLANK AND BACKGROUND CORRECTION. FURNACE: ELECTROTHERMAL ATOMIZATION. GRAPHITE TUBE. FURNACE ALIGNMENT. SAMPLE LOADING. GF-AAS AUTOSAMPLERS. TEMPERATURE PROGRAMMING. BLANK AND BACKGROUND CORRECTION. COMPARISON BETWEEN F-AAS AND GF-AAS. DETECTION LIMITS. SPECTROSCOPIC, CHEMICAL, AND IONIZATION INTERFERENCES. RELEASING AGENTS AND IONIZATION SUPPRESSORS. ROUTINE AND EXTRAORDINARY SPECTROPHOTOMETER MAINTENANCE. LECTURE 15 ATOMIC ABSORPTION SPECTROSCOPY: APPLICATIONS—LEAD, ALUMINUM, AND IRON IN FLAME AND FURNACE. COLD VAPOR MERCURY. ARSENIC VIA HYDRIDE FORMATION. AAS ACCESSORIES. PERISTALTIC PUMPS. CONCENTRATION CALCULATIONS IN UNKNOWN SAMPLES USING CALIBRATION AND STANDARD ADDITIONS. LABORATORY EXPERIMENT: DETERMINATION OF ZINC, CALCIUM, SODIUM, AND MAGNESIUM IN GROUNDWATER, FROM STANDARD PREPARATION TO UNKNOWN CONCENTRATION DETERMINATION. LECTURE 16 ATOMIC EMISSION SPECTROSCOPY. ICP-OES. PLASMA. GENERATORS. TORCH. INJECTORS. NEBULIZERS. SEQUENTIAL AND SIMULTANEOUS DETECTION. CCD. AXIAL AND RADIAL OPTICAL SYSTEMS. ICP ACCESSORIES. ANALYTICAL LINE SELECTION. ROUTINE AND EXTRAORDINARY SPECTROPHOTOMETER MAINTENANCE. ICP-MS. COMPARISON OF DETECTION LIMITS AMONG ICP, F-AAS, AND GF-AAS. LECTURE 17 CHROMATOGRAPHY. BASIC CONCEPTS: PRINCIPLES AND CLASSIFICATION. COLUMNS AND PHASES. CHROMATOGRAPHIC BED. SURFACE ENERGY. ACTIVE SITES. GC AND LC. INTERACTION MECHANISMS BETWEEN MOBILE AND STATIONARY PHASE SOLUTES: ADSORPTION, PARTITIONING, ION EXCHANGE, SIZE EXCLUSION, AFFINITY. CHROMATOGRAM. RETENTION TIMES. COLUMN CAPACITY FACTORS. HETP. CHROMATOGRAPHIC VELOCITY THEORY: VAN DEEMTER EQUATION. EFFICIENCY AND SELECTIVITY. RESOLUTION. PEAK SHAPES. INTERNAL STANDARD METHOD. CALCULATION EXAMPLES OF RESPONSE FACTOR FOR NON-SPECIFIC DETECTORS. CALIBRATION CURVE FOR CHROMATOGRAPHIC DATA. LECTURE 18 GC. SAMPLE PRETREATMENTS. DERIVATIZATIONS VIA ORGANIC SYNTHESIS. SILYLATING, ACYLATING, ALKYLATING AGENTS. TRIGLYCERIDE TRANSESTERIFICATION. GC DIAGRAM. COMPONENTS AND ROLES. PACKED AND CAPILLARY COLUMNS: WCOT, SCOT, PLOT. GC STATIONARY PHASES: SOLID AND LIQUID. INERT SUPPORTS FOR BPC. FS POROSITY. PARTITIONING LIQUIDS. BPC PREPARATION VIA ORGANIC SYNTHESIS. CHIRAL COLUMNS. GC MOBILE PHASES. OVEN. ISOTHERMAL AND TEMPERATURE GRADIENT. INJECTORS: SPLIT, SPLITLESS, ON-COLUMN, AND PTV. LECTURE 19 GC. DETECTORS: UNIVERSAL AND NON-SPECIFIC. TCD, FID, NPD, ECD, MS—OPERATING MECHANISMS. LOD AND LOQ. APPLICATIONS: ATMOSPHERIC GAS DETERMINATION, METHANOL IN DISTILLATES, FAME IN VARIOUS MATRICES, DIESEL ANALYSIS. LABORATORY EXPERIMENT: DETERMINATION OF METHANOL CONTENT IN A DISTILLATE, FROM STANDARD PREPARATION TO PERCENTAGE CONCENTRATION DETERMINATION. COMPLIANCE WITH SPECIFICATIONS. LECTURE 20 HPLC. HPLC BLOCK DIAGRAM. RECIPROCATING PUMPS. RHEODYNE VALVE. COLUMNS AND PRE-COLUMNS. DETECTORS. SAMPLE PRETREATMENTS. DERIVATIZATIONS VIA ORGANIC SYNTHESIS. ELUOTROPIC SERIES. ISOCRATIC AND GRADIENT ELUTION. LSC. LLC. BPC. DETERMINATION OF WATER- AND FAT-SOLUBLE VITAMINS. DRUG ANALYSIS. SIZE EXCLUSION. GPC STATIONARY PHASES. ION EXCHANGE. ION CHROMATOGRAPHY. IC STATIONARY PHASES. CONDUCTIVITY AND CONDUCTOMETRY. DEIONIZERS. SUPPRESSOR COLUMNS. SELF-REGENERATING SUPPRESSORS (SRS): OPERATION. WATER ANALYSIS. LAB DEMO: ANION PROFILE DETERMINATION IN POTABLE WATER, FROM STANDARD PREPARATION TO CONCENTRATION DETERMINATION. LAB DEMO: CAFFEINE DETERMINATION IN COMMERCIAL PRODUCTS. LECTURE 21 SELECTION OF ANALYTICAL METHOD. REGULATIONS AND LEGAL PARAMETERS. LEGISLATIVE DECREE 152/2006. UNI 14899 STANDARD: SAMPLING AND SAMPLING PLAN. SAMPLE REPRESENTATIVENESS. SAMPLING GRIDS. SAMPLE PRETREATMENTS: FILTRATION, GRINDING, SIEVING, EXTRACTIONS, LEACHING TESTS, LIQUID/SOLID RATIO DEFINITION AND EVALUATION, MINERALIZATIONS. LABORATORY SAMPLE. AIR SAMPLERS. CORE SAMPLING. LIQUID PROBES. SAMPLE STORAGE. WET DIGESTION. OXIDATIVE MW MINERALIZATION. SOLVENT EXTRACTION. SOXHLET EXTRACTION. SPE EXTRACTION. HYPHENATED TECHNIQUES: SPE-GC-NPD. STATIC HEADSPACE. DYNAMIC HEADSPACE. PURGE & TRAP. SPME. RECOVERY FACTORS. SAMPLE FORTIFICATION. |
Teaching Methods | |
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LECTURES IN THE CLASSROOM WITH PROJECTION OF TEACHING MATERIALS IN ELECTRONIC FORM. LABORATORY TESTS AND EXERCISES IN CLASS ON THE ACTIVITIES CARRIED OUT IN THE LABORATORY. |
Verification of learning | |
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THE EXAM IS WRITTEN AND LASTS 4 HOURS. THREE OPEN-ENDED QUESTIONS WILL BE FORMULATED, WHICH CAN BE WIDELY ARGUED AND WILL RELATE TO THE CONTENTS OF THE COURSE. ONE OF THE QUESTIONS WILL BE RELATED TO LABORATORY TESTS, DONE OR DISCUSSED IN CLASS.. A MAXIMUM OF 11 POINTS WILL BE AWARDED FOR EACH RESPONSE DEEMED EXHAUSTIVE IN TERMS OF THE COMPLETENESS OF THE THEORETICAL AND/OR EXPERIMENTAL INFORMATION PROVIDED BY THE CANDIDATE. FOR THEORETICAL INFORMATION, STUDENTS SHOULD REFER TO LECTURE NOTES AND/OR TEXTBOOKS; FOR EXPERIMENTAL INFORMATION, ALSO TO THE LABORATORY EXPERIENCES. THE EVALUATION OF THE ANSWERS, AS LONG AS THEY ARE RELEVANT TO THE QUESTION, WILL TAKE INTO ACCOUNT WHAT IS EXPRESSED BY THE CANDIDATE IN WRITTEN FORM, PROVIDED IT IS NOT REDUNDANT. KEEPING IN MIND THAT A STANDARD PAGE CONTAINS BETWEEN 250 AND 300 WORDS, THE FOLLOWING POINTS WILL BE AWARDED: 4 POINTS IF THE RESPONSE CONTAINS FEWER THAN 30 WORDS 5 IF FEWER THAN 65 6 IF FEWER THAN 100 7 IF FEWER THAN 170 8 IF FEWER THAN 250 9 IF FEWER THAN 350 10 IF FEWER THAN 500 11 POINTS IF THE CANDIDATE WRITES AN ESSAY WELL OVER 500 WORDS, DEMONSTRATING AN IN-DEPTH STUDY OF THE TOPIC DISCUSSED. LABORATORY EXPERIENCES WILL ALSO BE TAKEN INTO ACCOUNT. THOSE WHO HAVE NOT ATTENDED AT LEAST 75% OF THE LABORATORY SESSIONS WILL NOT BE ALLOWED TO TAKE THE FINAL EXAM, IN ACCORDANCE WITH THE REGULATIONS OF THE DEGREE PROGRAM. THIS RULE DOES NOT APPLY TO STUDENTS WHO HAVE BEEN EXEMPTED (E.G., DUE TO COVID). THE LABORATORY EXPERIENCES COUNT AS MIDTERM TESTS AND ARE EVALUATED BASED ON THE EXPERIMENTAL RESULTS OBTAINED IN THE LAB. EACH STUDENT MUST INDEPENDENTLY PREPARE A SOLUTION OF KNOWN CONCENTRATION, WHICH WILL THEN BE VERIFIED INSTRUMENTALLY. 10 POINTS WILL BE AWARDED IF THE SOLUTION IS CORRECTLY PREPARED, OTHERWISE ZERO POINTS. CANDIDATES WHO HAVE OBTAINED AN AVERAGE OVERALL SCORE HIGHER THAN 6/10 WILL RECEIVE EXTRA POINTS ON THE FINAL GRADE, AS STATED SEVERAL TIMES DURING THE COURSE. ONE EXTRA POINT WILL BE AWARDED FOR AN AVERAGE BETWEEN 6 AND 7, TWO POINTS FOR AN AVERAGE BETWEEN 7 AND 8, THREE POINTS FOR AN AVERAGE BETWEEN 8 AND 9, AND FOUR POINTS FOR AN AVERAGE EQUAL TO OR GREATER THAN 9. LABORATORY SCORES WILL BE POSTED ON THE PROFESSOR'S WEBSITE FROM TIME TO TIME, AND A RECORD OF THE OVERALL SCORES WILL BE KEPT. A CANDIDATE WHO EXCEEDS THE MAXIMUM AVERAGE SCORE OF 30/30 WILL BE AWARDED 30 CUM LAUDE. |
Texts | |
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1.A. PELOSO, PROBLEMI DI CHIMICA GENERALE, CORTINA ED., PADOVA, 2006. 2.SKOOG D. A, HOLLER, F. J., CROUCH, S. R., CHIMICA ANALITICA STRUMENTALE, 2A ED. EDISES 2009 3.D. HARRIS, CHIMICA ANALITICA QUANTITATIVA, ZANICHELLI, BOLOGNA, 2004. 4.CHIMICA ANALITICA CLINICA, C. D'OVIDIO, U. DE GRAZIA, P. LANUTI, M. LOCATELLI, M. MARCHISIO, G.M. MERONE, E. ROSATO, F. SAVINI, A. TARTAGLIA, ED. EDISES 2021 5.SPETTROMETRIA DI MASSA, DI J. H. GROSS. ED. EDISES 2016, PER LA PARTE RELATIVA 6.LEZIONI DI ELETTROCHIMICA, BRUNO MAZZA, EDISES ED. 2019, PER PARTE RELATIVA 7. SKOOG D. A, HOLLER, F. J., CROUCH, S. R., CHIMICA ANALITICA STRUMENTALE, 2A ED. EDISES 2009. |
More Information | |
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RECOMMENDED ATTENDANCE OF THE CLASS COURSE, THE LABORATORY TESTS ARE OBLIGATORY. WHO IS NOT PRESENT OVER 25% OF THE LABORATORY TEST IS NOT ADMITTED TO THE FINAL EXAM. |
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