84748 - CHIMICA ANALITICA 3

Learning outcomes

At the end of the course the student acquires theoretical and instrumental fundamentals to use analytical technologies and methodologies of separation science, spectrophotometry and mass spectrometry. The student will be able to choose most suited methodology to face simple problems of analytical chemistry, to find in them the critical aspects, and to show how to optimize quality of the analytical results thereby obtained.

Course contents

Required background: the student should have good knowledge of the fundamentals of analytical chemistry and physical chemistry acquired through the CFUs of the courses previously followed.

 Program Module 1:

• Course presentation.
• Fundamentals of analytical spectroscopy. Absorption and emission spectra, molecular and atomic spectra. Qualitative and quantitative analysis in analytical spectroscopy. The Beer-Lamber law: derivation and deviations from linearity. Absorbance measurements. Errors in absorbance measurements. Emission spectroscopy: photoluminescence, chemiluminescence.
• Instrumental basics in analytical spectroscopy: sources, wavelength selectors: filters, prism and grid monochromators. Pass band. Detectors: single phototubes, photomultipliers. Single-ray and double-ray spectrophotometers: in-time and in-space configurations. Noise suppression: lock-in and chopper. Spectrophotometric detectors for liquid chromatography.
• Fundamentals of atomic spectrometry. Instrumental details: sources (hollow-cathode lamp), atomizators (flame, furnace, inductively coupled plasma), chopper-based background correction.
• Separation techniques. Basics of chromatography. The chromatographic peak. Retention time. Theoretical plates. Separation efficiency and relevant dependence on the experimental conditions. Efficiency measurements. Capacity factor. Selectivity. Resolution and its dependence on selectivity and efficiency. Resolution equation. van Deemter's equation and its dependence on the experimental and instrumental conditions. Isothermal distribution and its deviations from linearity.
• Gas chromatography (GC). Packed and capillary columns. Stationary phases for GC. Gradient-temperature analysis. Injectors. Detectors for GC.
• Liquid chromatography (LC), HPLC. Different techniques in LC. Pumps, injectors. Stationary phases for LC. Direct and reversed phase, isocratic, and mobile phase gradient elution modes. Guidelines to choose the most appropriate LC technique to face an analytical case. Detectors for LC.
• Fundamentals on mass spectrometry (MS), instrumental basics: ion source and analyzers. “Hard” and “soft” ion sources: electron impact and chemical ionization, electron-spray ionization (ESI), fast-atom bombardment (FAB), and matrix-assisted, laser depletion/ionization (MALDI). Analyzers for MS: magnetic sector, quadrupole, time-of- flight (TOF).

Program Module 2:

• Spectroscopy: Uv-vis, atomic absorption, chemiluminescence.
• Separation techniques: HPLC (reverse-phase HPLC, size exclusion chromatography, ionic chromatography).
• Analysis of complex samples: digestion; matrix effect determination.
• Methods for the determination of protein concentration.

 

Readings/Bibliography

Suggested textbooks :

• D. C. Harris, Quantitative Chemical Analysis, 6th Edition, W.H. Freeman and Co., New York (USA), 2003
• Skoog, West, Holler, Crouch. Foundamentals of Analytical Chemistry, 8th Edition, Brooks/Cole, Thomson Learning, 2004

Teaching methods

Module 1: only frontal classes (6 CFU=48 hours). It is fundamental the use of the material shared with students on the web. This material is projected during classes.

Module 2: Room lessons assisted by projected material available to students on electronic media from the web.Training in laboratory. Data elaboration and report preparation.

Assessment methods

The exam is carried on as a WRITTEN TEST with OPEN QUESTIONS based on EVERY program chapter discussed in the classes and in the laboratory. The student draws lots a question for every chapter. Then the student  gives an answer to each question. The exam must be completed in a given slot of time and number of pages. 

The Jury ranks the candidate and it decides the final evaluation, which takes into account also a rank given to the lab reports.

If necessary, the Jury discusses with the Candidate the manuscript and the possible differences between Jury's evaluation and self-evaluation, as well as the possible reasons of the discrepancies.

The Candidates are strongly advised to have the exams of “Chimica Analitica 1” and “Chimica Analitica 2” passed before they take the present exam.

Non-Italian mothertongue Candidates may ask to take the exam in written English.

Teaching tools

Blackboard, PC with Windows PowerPoint slides (in Italian), projector and whiteboard. Word reports on-line available (Module 2) 

Office hours

See the website of Pierluigi Reschiglian

See the website of Barbara Roda