Chemical Engineering Practice I

Code:

EQ0016

Acronym:

PEQ I

Keywords
Classification	Keyword
OFICIAL	Life Sciences, Engineering and Chemical Labs

Instance: 2006/2007 - 1S

Active?	Yes
Responsible unit:	Department of Chemical Engineering
Course/CS Responsible:	Master in Chemical Engineering

Cycles of Study/Courses

Acronym	No. of Students	Study Plan	Curricular Years	Credits UCN	Credits ECTS	Contact hours	Total Time
LEQ	0	Plano de estudos de transição para 2006/07	2	4	4	-
MIEQ	81	Syllabus since 2006/2007	2	-	4	-

Teaching language

Portuguese

Objectives

The specific objectives of the discipline are:
1. To allow the proper knowledge of the theoretical principles, practical issues and application of instrumental analysis techniques related to the most common Instrumental Methods of Analysis: Spectroscopic, Electrochemical and Chromatographic;
2. To give students the ability to select the proper analytical methodologies to face specific requisites – specificity, sensitivity of detection, matrix interference, reproducibility and costs;
3. To familiarize students with the rules and procedures of analysis under the Portuguese System of Quality and the Good laboratory Practices (GLP’s), as well as Analytical Methods Validation.

Program

1. INTRODUCTION
1.1. Classical Laboratorial analysis versus Instrumental Analysis.
1.2. Steps involved in a laboratorial analysis.
1.3. Introduction to Instrumental Methods of Analysis. Classification.
1.4. Brief introduction to Good Laboratory Practices (GLP's).
1.5. Brief introduction to analytical methods validation. Associated parameters.
1.6. Suitability of the method. Calibration curves. Limits of detection and quantification.
1.7. Precision. Accuracy. Global uncertainty associated to an analytical result.

2. ABSORPTION SPECTROSCOPY ON ULTRAVIOLET, VISIBLE AND NEAR INFRARED
2.1. Electromagnetic Spectrum.
2.2. Radiation absorption. Nature of the electronic transitions. Radiation-absorbing species. Chromophors.
2.3. Beer Law. Limitations to à Beer Law: chemical and instrumental shifts.
2.4. Instrumentation. Basic components: radiation sourced; wavelength selectors, sample containers; radiation detectors; signal processors. Effect of the instrumental noise on the precision of spectrophotometric analysis.
2.5. Typical instruments: simple and double-beam spectrophotometer; photodiode detector.
2.6. Qualitative analysis. Selection of the solvent. Detection of functional groups.
2.7. Quantitative analysis. Applications. Typical procedure on an analysis: wavelength selection; absorbance-influencing variables; cleaning and handling of the cells; calibration curves. Standard addition method. Calculation method for the simultaneous determination of components in mixtures. Applications.
3. ATOMIC SPECTROSCOPY
3.1. Classification of spectroscopic methods.
3.2. Types of atomic spectra, energy diagrams; atomic emission or absorption spectra.
3.3. Atomic absorption. Instruments and modus operandi: radiation sources, atomizers: flame and electrothermal atomization, combustible and comburent gases. Chemical and spectral interferences. Correction methods: continuous source, Zeeman effect and Smith-Hieftje effect. Quantitative analysis: sample preparation; characteristic sample, calibration standards; standard addition method.

4. ELECTROANALYTICAL METHODS
4.1. Classification.
4.2. Review of electroanalysis concepts: electrochemical cells; anodes and cathodes; cell and electrode potentials; standard potentials; Nernst equation.
4.3. Potentiometric Methods.
4.4. Reference and trace electrodes.
4.5. The glass electrod for pH measurement. Errors affecting pH determination.
4.6. Potentiometric Titrations.
4.7. Ion-selective electrodes and selectivity coefficients. Use of calibration curves. Lower limit of linear response, limit of detection and meaning of slope.

5. CHROMATOGRAPHIC METHODS
5.1. Introduction. Classification.
5.2. Theory of chromatography. Separation mechanism. Retention time, capacity factor, chromatographic resolution and efficiency.
5.3. Optimization of a chromatographic separation. Example.
5.4. High performance liquid chromatography (HPLC). Instruments. Solvents used. Columns. Detectors. Operation in gradient elution. Application examples.
5.5. Gas chromatography (GC). Instruments. Injection systems. Mobile and stationary phases. Detectors. Operation at a programmed temperature. Quantitative analysis. Examples.
5.6. Gas chromatography with mass spectrometry detection (GC-MS). General principles of operation and application examples.

Mandatory literature

Madigan, Michael T; Brock biology of microorganisms. ISBN: 0-13-049147-0
Skoog, Douglas A.; Fundamentals of Analytical Chemistry. ISBN: 0-03-074922-0

Complementary Bibliography

Rubinson, Judith F.; Contemporary chemical analysis. ISBN: 0-13-519331-1
Skoog, Douglas A.; Principles of instrumental analysis. ISBN: 0-03-075398-8
Michael J. Pelczar, Jr., E. C. S. Chan, N. R. Krieg; Microbiologia: conceitos e aplicações, Makron Books do Brasil, 2nd ed, 1997

Teaching methods and learning activities

Lectures and tutorials; 7 laboratorial experiments; exercises of application

keywords

Natural sciences
Technological sciences

Assessment Components

Description	Type	Time (hours)	Weight (%)	End date
Subject Classes	Participação presencial	56,00
	Total:	-	0,00

Eligibility for exams

In order to perform the laboratorial exam at the end of the semester, alumni should obtain a positive grade during laboratorial classes. This is accomplished through the evidence of previous preparation of the tasks, the making of all the tasks and the updating management of the laboratorial notebook.

Calculation formula of final grade

Final Grade = 0.6xPE+0.4xWE

Classification improvement

The classification improvement will be assesssed by the final examination