Corso di laurea in Chimica e Tecnologie Chimiche

The course will provide students with: i) the knowledge and skills of
"problem solving" on the quantitative determination of analytes in
complex matrices; ii) chemical analytical skills necessary for the
performance of an instrumental analysis and presentation of analytical
results.

Learning the techniques of sample preparation and the principles of
operation of the major instrumental techniques of chromatography and
atomic spectroscopy. Expertise to use scientific instrumentation used in
laboratories for analysis, to make quantitative determinations to be
expressed according to statistical calculations.

The evaluation consists of two parts weighted by the credits
corresponding to: A) Lectures (7 credits) The examination is held, as a
rule, as written exam with 4-5 questions, each covering a topic of
program referred to in paragraph 5 above, plus 1-2 numerical exercises
related to laboratory exercises, in particular, on the development and
statistical evaluation of the uncertainty of the analytical result. Will be
evaluated both the understanding of the arguments that the ability to
connect an interdisciplinary various subjects. B) The activities carried outi n the laboratory (3 credits) will be evaluated on the basis of the reports prepared for each experience with particular regard to the accuracy of the results, critical reading of the same and to the understanding of the theoretical principles that are the basis of the experiments / measurements performed

L'esame si svolge, di norma, come segue: La valutazione (in trentesimi) si compone di due parti pesate per i CFU corrispondenti: A) Lezioni Frontali (7 CFU) L'esame si svolge, di norma, come esame scritto con 4-5 domande, ciascuna riguardante un argomento del programma di cui al precedente punto 5, più 1-2 esercizi numerici relativi alle esercitazioni di laboratorio, in particolare sull’elaborazione statistica e valutazione dell’incertezza del risultato analitico. Verrà valutata sia la comprensione degli argomenti svolti che la capacità di collegare i vari temi interdisciplinarmente. B) L’attività svolta in laboratorio (3 CFU)verrà valutata sulla base delle relazioni elaborate per ciascuna esperienza con particolare riguardo all’accuratezza dei risultati, alla lettura critica degli stessi e alla comprensione dei principi teorici che stanno alla base degli esperimenti/misure svolti

Curriculum: CHEMISTRY. The course will outline the theoretical and the
experimental use of the main chemical analytical instrumentation in the
modern chemical laboratory. The approach will be two-fold: on the one
hand, we will illustrate the principles and operation of chemical and
physical analytical instruments emphasizing the type of samples
analyzed. The second approach reverses this perspective and starts the
real analytical problem, then the material and the analytical problem to
be solved. We then explain the choice of the most appropriate analytical
methodology, the campionament, sample preparation, analysis and
processing of the results.
Topics:
The stages of the chemical analysis instrument: from sampling to
measurement of an instrument signal, until the presentation of the
analytical result.
Sample preparation for analysis: attack and dissolution of samples for
elemental analysis. Methods of extraction, clean-up and separation for
compositional analysis. Multiphase equilibrium distribution: liquid-liquid,
gas-liquid and liquid-solid (adsorption). Extraction yields in the presence
of multiple equilibria. Simple extraction, multiple, continuous, continuous
countercurrent. Examples. Solid Phase Extraction (notes).
Elements of electronics for analytical instruments: electric circuits,
voltage dividers, current dividers, filters, semiconductor devices,
operational amplifiers, radiation detectors, analog and digital signals,
analog digital converters.
Inorganic elemental analysis: atomic absorption spectroscopy, atomic
emission spectroscopy and fluorescence equipment (optical materials,
sources, wavelength selectors, detectors). Effect of bandwidth and the
slit on the measures. Interference. Atomization systems: flame, graphite
furnace, plasma. Fields of application, limits, yields, interference and
measurement strategies. Memory effect; method hydride; technical
correction matrix: deuterium lamp, Zeeman effect. Applications and
comparison of spectroscopic techniques.
Inorganic mass spectrometry
Analysis by isotope dilution
X-ray fluorescence
Surface analysis techniques: photoelectron spectroscopy
Elemental analysis for organic combustion (CHNSX, TC, TOC, TN, TKN,
TOX)
Luminescence: physico-chemical bases of the phenomena fluorescence,
phosphorescence and chemiluminescence. Instruments for the
measurement of fluorescence and phosphorescence. Applications.
Chromatography: Application of equilibrium distribution of gas-liquid and
liquid-liquid. The chromatographic elution process and the properties of
the chromatographic peaks: resolution, selectivity, capacity factor and
efficiency. The kinetic theory of chromatography, principles of fluid
dynamics and the Van Deemter equation.
Gas chromatography (GC) columns and stationary phases, flow
parameters and fast-GC, Kovats indices and McReynolds constants.
Injector for GC. GC detectors: FID, PID, ECD, thermal conductivity, mass
spectrometry. Derivatization reactions.
Liquid chromatography (LC): pumps, injectors, columns, stationary and
mobile phases, binary and ternary gradients. Detectors for LC:
s p e c t r o p h o t o m e t r i c , s p e c t r o f l u o r o m e t r i c , r e f r a c t i v e i n d e x ,
electrochemical. Derivatization reactions.
Ion chromatography: principles of separation and conductivity detection.
Chiral chromatography, ion pairing, size exclusion and ion: Principles,
stationary phases and eluents, applications.

Curriculum: CHEMISTRY. The course will outline the theoretical and the
experimental use of the main chemical analytical instrumentation in the
modern chemical laboratory. The approach will be two-fold: on the one
hand, we will illustrate the principles and operation of chemical and
physical analytical instruments emphasizing the type of samples
analyzed. The second approach reverses this perspective and starts the
real analytical problem, then the material and the analytical problem to
be solved. We then explain the choice of the most appropriate analytical
methodology, the campionament, sample preparation, analysis and
processing of the results.
Topics:
The stages of the chemical analysis instrument: from sampling to
measurement of an instrument signal, until the presentation of the
analytical result.
Sample preparation for analysis: attack and dissolution of samples for
elemental analysis. Methods of extraction, clean-up and separation for
compositional analysis. Multiphase equilibrium distribution: liquid-liquid,
gas-liquid and liquid-solid (adsorption). Extraction yields in the presence
of multiple equilibria. Simple extraction, multiple, continuous, continuous
countercurrent. Examples. Solid Phase Extraction (notes).
Elements of electronics for analytical instruments: electric circuits,
voltage dividers, current dividers, filters, semiconductor devices,
operational amplifiers, radiation detectors, analog and digital signals,
analog digital converters.
Inorganic elemental analysis: atomic absorption spectroscopy, atomic
emission spectroscopy and fluorescence equipment (optical materials,
sources, wavelength selectors, detectors). Effect of bandwidth and the
slit on the measures. Interference. Atomization systems: flame, graphite
furnace, plasma. Fields of application, limits, yields, interference and
measurement strategies. Memory effect; method hydride; technical
correction matrix: deuterium lamp, Zeeman effect. Applications and
comparison of spectroscopic techniques.
Inorganic mass spectrometry
Analysis by isotope dilution
X-ray fluorescence
Surface analysis techniques: photoelectron spectroscopy
Elemental analysis for organic combustion (CHNSX, TC, TOC, TN, TKN,
TOX)
Luminescence: physico-chemical bases of the phenomena fluorescence,
phosphorescence and chemiluminescence. Instruments for the
measurement of fluorescence and phosphorescence. Applications.
Chromatography: Application of equilibrium distribution of gas-liquid and
liquid-liquid. The chromatographic elution process and the properties of
the chromatographic peaks: resolution, selectivity, capacity factor and
efficiency. The kinetic theory of chromatography, principles of fluid
dynamics and the Van Deemter equation.
Gas chromatography (GC) columns and stationary phases, flow
parameters and fast-GC, Kovats indices and McReynolds constants.
Injector for GC. GC detectors: FID, PID, ECD, thermal conductivity, mass
spectrometry. Derivatization reactions.
Liquid chromatography (LC): pumps, injectors, columns, stationary and
mobile phases, binary and ternary gradients. Detectors for LC:
s p e c t r o p h o t o m e t r i c , s p e c t r o f l u o r o m e t r i c , r e f r a c t i v e i n d e x ,
electrochemical. Derivatization reactions.
Ion chromatography: principles of separation and conductivity detection.
Chiral chromatography, ion pairing, size exclusion and ion: Principles,
stationary phases and eluents, applications.

Recommended readings
The basic material recommended for the course are the handouts
provided by the teacher.
The recommended basic texts for the course are:
DC Harris, "Quantitative Analytical Chemistry" 2005 Zanichelli
Kellner - Mermet - Eight - Widmer, "Analytical Chemistry", Edises 2003
Skoog, Holler, Crouch, "Instrumental Analytical Chemistry", Edises 2009
It 'strongly advised to use the following material for insights and
additions:
Wilson & Wilson's Comprehensive Analytical Chemistry, Elsevier
Treatise on Analytical Chemistry, McGraw-Hill, second edition.
Both works are available at the Library "G.Ponzio" Departments of
Chemical
Finally are listed below websites of interest:
http://www.chemguide.co.uk/analysismenu.html
http://freevideolectures.com/Course/3029/Modern-Instrumental-Methodsof-
Analysis #
http://www.internetchemistry.com/chemistry/analytical_chemistry.htm
http://www.asdlib.
org/onlineArticles/ecourseware/Spudich/Spudich_ASDL_Chem520.pdf
http://www.chromacademy.com/ (registration required)