Academic management

“Analytical Chemistry II” is taught in the third year of the Chemistry Degree. It belongs to the Fundamental module (Analytical Chemistry) and introduces students within the field of highly sensitive and selective analytical techniques and methods (based in optical spectrometry, electrochemistry and mass spectrometry) essential in Chemistry studies. “Analytical Chemistry II” provides the students with basic and applied knowledge related with modern analytical techniques. Also, it gives the criteria to select the most adequate techniques to solve particular analytical problems and to correctly interpret the results.

The techniques and fundamentals presented in this course are crucial for the basic academic formation, allowing the student a better understanding of other subjects within the third year (e.g. “Experimentation in Organic Chemistry I”, or “Physical Chemistry II” and “Physical Chemistry III”). Also, it is very important for subjects of the fourth year. In fact, it is mandatory to have passed this “Analytical Chemistry II” to get enrolled in “Experimentation in Analytical Chemistry II” (fourth year).

Teachers belong to the Analytical Chemistry area of the Department of Physical and Analytical Chemistry. Lectures will be given by M. Teresa Fernández Abedul and Rosario Pereiro. Seminars and Group tutorial sessions will be given by M. Teresa Fernández Abedul and Beatriz Fernández.

It is recommendable for the student to be familiarized with the units system, with mathematical calculations (logarithms, exponentials, use of calculators, etc) and with the basic principles of Analytical Chemistry; i.e. to have passed General Chemistry, Mathematics and Physics of the first year and “Analytical Chemistry I” and “Experimentation in Analytical Chemistry I” (second year). Actually, registration in “Analytical Chemistry II” requires “Analytical Chemistry I” passed.

The General Competencies to be pursued in this course are those collected in the VERIFICA Memory of this Degree as CG-1, CG-2, CG-7, CG-8, CG-9, CG-11, CG-12, CG-17, CG-18.

The Specific Competencies to be pursued are CE-6, CE-13, CE-14, CE-15, CE-18, CE-19, CE-20, CE-22, CE-24, CE-30, CE-34, CE-35.

The expected Learning Outcomes are the following:

1. To search for and use scientific information in an effective way.
2. To examine and analyse new problems in the scope of Chemistry and to plan strategies to solve them.
3. To demonstrate knowledge and understanding of the concepts, principles and theories related with Analytical Chemistry and their application to problem solving.
4. To link the fundamentals of analytical techniques, spectroscopic and of structural investigation with their applications.

• UNIT 1. INTRODUCTION TO DYNAMIC ELECTROCHEMICAL TECHNIQUES

Electrochemical cells and electrode processes. Electrochemical techniques: classification. Basic instrumentation. Kinetics of charge transfer. Mass transport in electrochemical cells. 

• UNIT 2. LINEAR  VOLTAMMETRY 

Introduction. Linear sweep voltammetry and cyclic voltammetry: theoretical considerations and analytical applications. Characterisation of electrode processes. Reactions coupled to electron transfer and adsorption processes. Hydrodynamic voltammetry.

• UNIT 3. PULSE VOLTAMMETRY

Introduction. Normal and differential pulse voltammetry (NPV and DPV): theoretical considerations and analytical applications. Square-wave voltammetry (SWV): theoretical considerations and analytical applications.

• UNIT 4. PROCESSES OF PRECONCENTRATION AT ELECTRODES

Introduction. Electrodic preconcentration: possible processes. Stripping voltammetry. Adsorptive sptripping voltammetry. Analytical applications.

• UNIT 5. COULOMETRY

Introduction. Direct coulommetry: a) at constant intensity, b) at constant potential. Applications. Coulometric titrations: fundamentals, types and analytical applications.

• UNIT 6. INFRARED SPECTROSCOPY

Vibrational state of a molecule. Rotational transitions. Rotational/vibrational transitions. Types of molecular vibrations. Mechanical model for vibration in diatomic molecules. Infrared spectrum. Infrared absorption. Basic instrumentation. Dispersive IR spectrophotometers. Interferometers. Fourier analysis. FTIR spectrophotometers. IR microscopy. Relevant applications.

• UNIT 7. FLAMELESS ATOMIC ABSORPTION SPECTROMETRY

Introduction to electrothermal atomic absorption spectrometry. Characteristics of the graphite furnace. Basic steps in analysis by electrothermal atomic absorption spectrometry: the temperature program. Instrumentation for ETAAS. Interferences. Chemical modifiers. Analytical performance characteristics of ETAAS. Applications of ETAAS. Introduction to hydride and cold vapour generation. Volatile hydrides generation by tetrahydroborate(III) in aqueous media. Cold vapor generation. Trapping/preconcentration of volatilized analytes. Applications of hydride and CV generation.

• UNIT 8. ATOMIC EMISSION SPECTROMETRY WITH PLASMA SOURCES

Plasmas as excitation sources. Analytical plasmas: definition and characterization. The inductively coupled plasma (ICP). Basic instrumentation. Analytical performance characteristics. Other plasma sources of analytical interest. Applications.

• UNIT 9. X-RAY SPECTROMETRY FOR CHEMICAL ANALYSIS

Introduction. X-ray absorption. General method for x-ray fluorescence analysis. X-ray excitation sources. Sample holder. Separation of fluorescent lines: analyser, X-ray detectors. Wavelength dispersive spectrometers and energy dispersive spectrometers. Interferences and calibration. Sample preparation. Analytical applications of x-ray fluorescence. Microanalysis methods: electron microprobe.

• UNIT 10. ELEMENTAL AND MOLECULAR MASS SPECTROMETRY

Introduction to mass spectrometry and fundamentals. Classification of mass spectrometric techniques. Mass spectrometers. Detectors. Inorganic mass spectrometry. Basic instrumentation in ICP-MS. Analytical performance characteristics and relevant applications of ICP-MS. Molecular mass spectrometry. Ionization sources in molecular mass spectrometry. Coupled spectrometers. Relevant applications of molecular mass spectrometry.

The contents of this course will be presented using three different types of in-class activities:

1. Lectures: The course content will be presented by the teacher. At the beginning of each unit, the main objectives of the unit under study will be commented and at the end, some questions that allow correlating all the acquired knowledge will be posed. With the aim of following the lectures in an adequate way, students will have previously the material employed by the teacher (e.g. in the Campus Virtual platform). The explanation of each unit will be done by using the blackboard and/or audiovisual media.
2. Seminars: Calculations related to the contents of the the Lectures will be discussed. Active participation will be favoured. Numerical problems will be given previously  to the students.
3. Group tutorial sessions (mandatory). Questions and problems related to the different units will be discussed in these sessions. Students will have sufficiently in advance the questions and exercises that should be dealt with either individually, or collectively, before the tutorial session. In the tutorial session the student will present the solved exercises and the teacher will clarify doubts and problems that students have found in the resolution of the proposed tasks. The general objective of these activities is that students know the utility of instrumental analytical methodologies that were studied along the course as well as their real application in e.g. environmental, technological, industrial, clinical, forensic or food fields. Also, they will visit the “Scientific-Technical Services” of the University of Oviedo. With this activity the students will have the opportunity of evaluating the importance of the available analytical instrumentation and the problems it solves.

In the exceptional case that sanitary, safety, or any other condition require extraordinary measures, any teaching activity (lectures, seminars, and group tutorials) can be carried out in an online platform. In this case, the students will be timely informed about the changes made.

The Campus Virtual will be used and will allow fluent communication between students and teachers. It is the basic tool employed by teachers for giving material to students. The course has 6 credits that correspond to 150 hours of student work. The distribution of this work is shown in the following table:

Ordinary evaluation will consist of:

1. Written test. The maximum mark will be 10 points, being 5 points the minimum required to pass. The mark obtained will be 85% of the final grade. The test will take a maximum of 3 hours and will consist of a theoretical part (60% of the mark) and a practical part (numerical questions, 40% of the mark). The minimum mark that allows compensation of each part is 4.5.
2. Group tutorial sessions. They will be marked from 0 to 10 points, and they will account for the 15% of the final mark.

In extraordinary examinations, evaluation will consist only of a written test, that is 100% of the final mark. In this test, it will be required to obtain 5 points over 10 for passing the course. The test will take a maximum of 3 hours and will have a theoretical part (60% of the mark) and a practical one (numerical questions, 40% of the mark). The minimum mark that allows compensation of each part is 4.5.

In the exceptional case that sanitary, safety, or any other condition require extraordinary measures, any evaluation method can be carried out in an online platform. In this case, the students will be timely informed about the changes made.

Power-Point presentations will be used in lectures and seminars. Material will be available either in Campus Virtual or at the class, where the teacher will give it to the students. The same happens with auxiliary materials such as publications, practices, calculations…

Some bibliography related to the different units is listed below:

• Principles of Instrumental Analysis, 7th Edition. D. A. Skoog, F. J. Holler, S. R. Crouch, 2018.
• Quantitative Chemical Analysis, D. Harris, 8ª Edition, W. H. Freeman and Company, 2010.
• Chemical Instrumentation: a Systematic Approach 3rd Edition; H. A. Strobel, W. R. Heineman. John Wiley & Son, New York, 1989.

Complementary texts are:

• Chemical Analysis. Modern Instrumentation, Methods and Techniques, 2nd Edition, F. Rouessac, A. Rouessac. Wiley, 2007.
• Electrochemical Methods. Fundamentals and Applications; A. J. Bard, L. R. Faulkner, 2nd Edition, J. Wiley & Sons, New York, 2001.
• Analytical Electrochemistry, 2nd edition, J. Wang, Wiley-VCH, 2000.
• Laboratory Techniques in Electroanalytical Chemistry, 2nd Edition, P. T. Kissinger, W. R. Heineman, Marcel Dekker, 1996.
• Técnicas Espectroscópicas en Química Analítica. Tomos I y II. A. Ríos Castro, M.C. Moreno Bondi, B.M. Simonet Suau (coords.), Editorial Síntesis, 2012.