Analytical Methods
Objectives
1 – The student should understand the fundamentals and working principles of the analytical instrumentation in the areas of spectroscopy, electrochemistry and separation science (knowledge to be acquired);
2 – to decide the suitability of a specific analytical method to answer to a specific problem (knowledge to be acquired and decision competences to be developed);
3 - at a laboratorial level the student should be able to operate in an autonomous manner the different instrumentation; so the course will provide practical and technical skills in scientific instrumentation;
4 – be able to work as a team and to present a scientific result (competences to be developed);
5 –as ultimate objective, the student should know identify the analytical problem, to design the experimental procedure, to conduct the experiment, to analyze with criteria the experimental data, to interpret and build report (competences to be developed in planning, organizing, decision making, reporting, systematization, and knowledge to be acquired in data treatment with worksheets).
General characterization
Code
12589
Credits
6.0
Responsible teacher
Maria Madalena Alves de C.S.D. Andrade
Hours
Weekly - 4
Total - 73
Teaching language
Português
Prerequisites
Available soon
Bibliography
Main reference
D. Harris, Quantitative Chemical Analysis, 7nd ed. W. H. Freeman and Company, New York, ISBN: 0-7167-7041-5, Available in:http://www2.fc.unesp.br/lvq/LVQ_experimentos/analitica_qualitativa/material%203.pdf
Alternative references: D.A. Skoog, D. West, F.J. Holler, S.R. Crounch (2000). Analytical Chemistry. An Introduction, 7th edition, Thomson Learning.
Slides of the course
Teaching method
Theoretical classes, problem solving classes with group strategy solving, laboratory classes with students taking an active role in the assembly of equipment (in electrochemistry), decision on the strategy for the execution of the work, autonomous research on case studies and on experimental techniques suitable for characterization
Evaluation method
The curricular unit has two assessment components: theoretical (T), with a weight of 60%, and practical (P), with a weight of 40%.
The average of the two tests must be equal to or greater than 9.5.
The grade of the practical component is calculated based on the classification obtained in the lab performance/realization/discussion of the electrochemistry questionnaires (50%) and performance/presentation of the case study (50%). The minimum grade of the P component is 9.5.
For approval, the weighted average T(tests)x0.6 + Px0.4 must be ³ 9.5.
If the student obtains a minimum grade P of 9.5, but lower in the T component, will be evaluated in final exam and the T classification thus obtained, if equal or higher than 9.5, will be weighted with the practical component according: T(exam)x0.6 + Px0.4 = final grade.
If T(exam) grade is less than 9.5, the P grade will be kept for the following year.
Subject matter
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Introduction to the instrumental methods of analysis – Classification of Methods of Analysis. Performance characteristics of Instrumental Methods of Analysis (precision, accuracy, sensitivity, selectivity, dynamic range, limit of detection, limit of quantification). Calibration methods. Statistical treatment of data. Significant figures. Precision and accuracy. Types of errors. Statistical treatment of underdetermined errors. Rejection of results. Rules for Uncertainty Propagation. Normal and t-student distribution. Minimum Mean Square Error. Linear and non-linear regression. Chemical equilibrium in complex systems: application in quantitative analyzes of complexometry and precipitation; resolution of (multi) equilibrium problems in complex systems, determination of algebraic expressions for calculation of solution composition Introduction to spectroscopic techniques. Atomic and Molecular Absorption. Visible ultraviolet spectroscopy. The equipment in spectroscopy. Quantitative aspects of the molecular absorption spectra UV-Vis. Lambert''s Law; Beer''s Law; Limitations and deviations from the quantitative analysis. Emission spectroscopy: Fluorescence and Phosphorescence. Vibrational Spectroscopy: Infrared and Raman. Introduction to nuclear magnetic resonance spectroscopy. Introduction to electroanalytical methods: the electrochemical cell and its schematic representation; Nernst equation and electrode potential. The ionic strength and concept of activity. Potentiometry: reference electrodes and selective electrodes. Voltammetry. Reversible reactions and degree of reversibility. Chemical reactions coupled to electrochemical processes. Corrosion and corrosion control. Introduction to Chromatographic techniques. Gas Chromatography (GC). Liquid chromatography (LC). High Performance Liquid Chromatography (HPLC). Hyphenated techniques and mass spectroscopy (MS): GC-MS, LC-MS . Case study. |