66925 - Instrumental Analytical Chemistry

Academic Year 2017/2018

  • Teaching Mode: Traditional lectures
  • Campus: Bologna
  • Corso: First cycle degree programme (L) in Chemistry and Materials Chemistry (cod. 8006)

    Also valid for First cycle degree programme (L) in Chemistry and Materials Chemistry (cod. 8006)

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:

  • Course presentation.
  • Fundamentals of 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).

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

The course is given with only frontal classes (6 CFU=48 hours).

It is fundamental the use of the material shared with students on the website Alma@DL. This material is projected during classes.

Assessment methods

The exam is carried on as a WRITTEN TEST with OPEN QUESTIONS based on  the Program contents that were discussed in the classes. At the end, the Jury ranks the candidate and it decides the final evaluation. 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.

As a general rule, the Candidates with a Learning Plan including “Chimica Analitica 3” must take and pass at the same time  also the exam of “CHIMICA BIOANALITICA E LABORATORIO DI CHIMICA ANALITICA 3”.

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

Teaching tools

Blackboard, PC with Windows PowerPoint slides (in Italian), projector and whiteboard.

Office hours

See the website of Pierluigi Reschiglian