SYLLABUS
Programme: Environmental Engineering
Title of course unit: Methods of Instrumental Analysis
Year: 2
Semester: 2
ECTS credits: 4,0
CNAEF area: 524
Student workload in hours
Contact
Total
100
Autono-
Theoretical
Lectures
Theoreticalpractical
Lectures
Laboratory
Classes
Supervised
Field Work
Seminars
Placements
Tutorials
mous
15
-
45
-
-
-
-
40
Summary
Fundamentals and applications of optical methods in analytical chemistry: molecular absorption
spectroscopy (ultraviolet and visible), atomic absorption spectrometry (flame or electrothermal
atomization and hydride generation system), atomic emission spectrometry and flame emission
spectrometry. Fundamentals and applications of electrochemical methods in analytical chemistry:
potenciometric methods. General processes of separation and purification. Extraction. Chromatography:
Theoretical aspects. Thin Layer Chromatography. Column chromatography. Gas Chromatography. High
Pressure Liquid Chromatography. Ion Chromatography.
Course Contents
Development of a Chemical Analysis: Choosing a suitable analytical method. Sampling. Transportation
and Conservation of the sample. Preparation of the sample. Analysis.
Basic Concepts in Chemical Analysis: Errors in Analytical Chemistry. Systematic Errors and Accidental
Errors. Precision, accuracy and detection limit. Elements of statistics useful in chemical analysis. Standard
solutions. Calibration Curves. Using the methods of Least Squares. Concentration of solutions. Diluting.
Significant figures.
Introduction to Optical Methods: Characteristics of electromagnetic radiation. Wave behavior of
electromagnetic radiation. Corpuscular behavior of electromagnetic radiation. Classification of various
optical methods. Energy of electromagnetic radiation in various spectral regions. Atomic absorption.
Molecular absorption. Emission of radiation.
Molecular absorption spectrophotometry: General aspects of radiation absorption. Quantitative aspects
Página 1 de 4
of radiation absorption: Beer-Lambert law. Deviations from Beer's law. Nomenclature and graphical
presentation of data in spectrophotometry. Sensors. Qualitative Analysis. Quantitative Analysis.
Atomic Absorption Spectroscopy: Theoretical principles of atomic absorption spectroscopy. Apparatus
for measuring atomic absorption spectroscopy. Radiation sources. Flame and electrothermal atomization.
Limitations in atomic absorption. Interferences. Comparison of absorption spectrometry techniques
flame and graphite furnace. Quantitative Analysis.
Atomic Emission Spectroscopy: Introduction to different methods of atomic emission. Theoretical
principles of flame emission photometry. Sensors. Limitations on flame emission photometry.
Interference. Qualitative Analysis. Quantitative Analysis. Comparison of two methods of flame: emission
and absorption. Atomic emission spectroscopy. Excitation sources in atomic emission spectroscopy. The
technique of atomic emission spectroscopy with inductively coupled plasma (ICP).
Potentiometry: Introduction to potentiometric methods. Reference electrodes. Indicator electrodes.
Sensors in potentiometric measurements. Calibration curve method or direct potentiometry.
Sample Preparation for chromatography: General procedures for separation and purification.
Extraction: Theory of extraction. Liquid-liquid extraction and solid-liquid extraction. Simultaneous
extraction and distillation. Solid phase extraction. Solid phase microextraction. Supercritical extraction.
Extraction adsorbent magnetic bar.
Chromatography: Introduction to Chromatography. Theoretical Aspects. Separation processes.
Analytical or preparative thin layer chromatography: Stationary phase. Eluotropic series and choice of
eluent. Preparation of chromatographic plates. Elution and revelation. Applications.
Column chromatography: Preparation of a chromatography column. Stationary phases. Eluotropic series
and choice of eluent. Applications.
High pressure liquid chromatography: basic instrumentation. Reservoir of mobile phase. Pumps. Nozzles.
Basic parameters. Stationary phases. Columns. Detectors - Basic characteristics. Data acquisition system.
Bases of the separation process.
Gas chromatography: basic instrumentation. Gas carrier. Sample introduction systems. Temperature
Control Column. Basic parameters. Stationary phases. Capillary columns (open tubular columns).
Detectors: - Basic characteristics, operation and applications, thermal-conductivity detector; - flame
ionization detector; - Nitrogen-Phosphorus Detector; - Electron Capture Detector, - Other detection
systems. Qualitative and quantitative analysis.
Ion Chromatography: Fundamentals. Stationary phase. Eluents. Cations. Anions. Suppression. Sensitivity.
Recommended or required reading
Required: Available on-line on the elearning platform or at the ESAB Copy Center:
Página 2 de 4




Alvarenga, P. (2010). Manual de Apoio para as Aulas Teóricas de Métodos Instrumentais de
Análise – 1º Módulo. Escola Superior Agrária de Beja. Beja.
Alvarenga, P. (2010). Guia Laboratorial para a Disciplina de Métodos Instrumentais de Análise –
1º Módulo. Escola Superior Agrária de Beja. Beja.
Chaves, H. (2010). Manual de Apoio para as Aulas Teóricas de Métodos Instrumentais de Análise
– 2º Módulo. Escola Superior Agrária de Beja. Beja.
Chaves, H. (2010). Guia Laboratorial para a Disciplina de Métodos Instrumentais de Análise – 2º
Módulo. Escola Superior Agrária de Beja. Beja.
Recommended:








Gonçalves, M.L.S. (1990). Métodos Instrumentais para a Análise de Soluções - Análise
Quantitativa. 2ª Edição. Fundação Calouste Gulbenkian. Lisboa.
Skoog, D.A. & Leary, J.J. (1992). Principles of Instrumental Analysis. 4th Edition. Saunders College
Publishing.
Skoog, D.A., West, D.M. & Holler, F.J. (1997). Fundamentals of Analytical Chemistry. 7th Edition,
Saunders College Publishing.
Ewing, G.W. (1985). Instrumental Methods of Chemical Analysis. 5th Edition. McGraw- Hill
International Edition.
Pecsok, R.L., Shields, L.D., Cairns, T., McWilliam, I.G. (1976). Modern Methods of Chemical
Analysis. 2nd Edition. John Wiley & Sons.
Braun, R.D. (1987). Introduction to Instrumental Analysis. McGraw-Hill International Editions.
Chemistry Series.
Strobel, H.A, Heineman, W.R. (1989). Chemical Instrumentation: A Sistematic Approach. 3rd
Edition. Wiley Interscience.
Welz, B., Sperling, M. (1999). Atomic Absorption Spectrometry. 3rd Edition. Wiley-VCH.
Learning outcomes
On successful completion of this course unit, the student should be able to:



Identify different types of instrumental methods of analysis, its theoretical and its practical
applications.
Plan and run a chemical analysis on its various components: establishment and implementation
of sampling, choice of instrumental method of analysis most appropriate treatment of the
sample, analysis, processing of results and critical analysis of the results.
Have professional capacity to use an instrumental method of analysis in the analysis of different
types of environmental samples (water, soil, air and tissues of living organisms).
Planned learning activities and teaching methods
Expository lectures, practice classes, laboratorial classes, guided study.
Contribution to the acquisition and development of specific skills
Fundamental:
Complementary:
Partial:
Página 3 de 4
Assessment methods and criteria
Laboratorial/Practical evaluation (written reports with discussion of the results obtained in the
laboratorial classes): 30%.
Theoretical examination (two tests or a final exam): 70%.
Página 4 de 4