Instrumental Methods of Analysis

Instance: 2012/2013 - 1S

Cycles of Study/Courses

Last updated on 2012-10-25.

Fields changed: Objectives, Métodos de ensino e atividades de aprendizagem, Fórmula de cálculo da classificação final, Provas e trabalhos especiais, Avaliação especial, Componentes de Avaliação e Ocupação, Obtenção de frequência, Programa, Observações, Lingua de trabalho, Melhoria de classificação final/distribuída

Teaching language

Objectives

The main objectives are:

·        To provide an adequate knowledge of the principles, instrumentation and applications of common analytical techniques, including atomic and molecular absorption spectroscopy, electrochemical and separation methods (chromatographic and electrophoretic);

·        To provide an adequate knowledge of the main processes of extraction and handling of solid liquid and gas samples and their implications for the analytical measurement uncertainty;

·        To provide the necessary skills to enable students to select a particular analytical technique to solve a problem, to determine restrictions, to select the most appropriate analytical methodologies, to identify alternatives, to compare the advantages and disadvantages of each one and to develop a critical reasoning about the analytical results;

·        To develop communication skills, particularly the technical results and the group cooperation skills;

·        To encourage the use of their scientific knowledge to solve real problems and to develop their critical reasoning.

Learning outcomes and competences

To achieve these objectives students should know how:

·        To explain the principles and the operation mode of the most used analytical equipments in electrochemistry, spectroscopy and chromatography;

·        To design an analytic experience to solve a real problem;

·        To carry out laboratory analysis in accordance with Good Laboratory Practices, in conditions of hygiene and safety, which involves sample handling, extraction, preconcentration, instrumental measurements and calculate the analytical result and its uncertainty;

·        To interpret and communicate an analytical result and write technical reports;

·        To work as a team.

Working method

Pre-requirements (prior knowledge) and co-requirements (common knowledge)

not applicable

Program

Theoretical-practical program: Introduction. Instrumental methods of analysis. Factors of selection of analytical methods. Basic concepts of validation. Sample preparation processes (LLE, SPE, SLE and SPME). Spectral methods. Molecular absorption spectroscopy in ultraviolet (UV) and visible (VIS). Atomic absorption spectroscopy. Flame atomization, electrothermal and ICP. Mercury analysis by cold vapour and hydrides generator for arsenic and selenium. Electrochemical methods. Potentiometric determination with ion selective electrodes. Chromatographic methods. Theory of chromatography. Gas chromatography with flame ionization, electron capture and mass spectrometry detectors. High performance liquid chromatography with ultra violet/visible detection and fluorescence.

Laboratory program:

The laboratory classes take place in the laboratory of Instrumental Methods of Analysis of DEQ (E105).

Given the large number of students per class, in this year eight groups will be formed. Students must do 6 laboratory works, 4 of which in a rotation scheme.

In the first week all students will perform the work T0, in the following weeks the students will perform 4 works in a rotation scheme and finally, they all do work T6.

The works are:

T0. Evaluation of the validation parameters of an analytical method to determine cadmium in solids by atomic flame absorption spectroscopy after acidic digestion

T1. Determination of copper content in a copper wire by flame atomic absorption spectroscopy

T2. Analysis of nitrates in vegetables by ion selective electrode with potentiometric detection

T3. Analysis of caffeine in energy drinks by HPLC-UV

T4. Determination of the purity of organic solvents by gas chromatography coupled with flame ionisation detection (GC- FID)  

T5.  Identification of contaminants of recovered organic solvents by GC-MS  

Mandatory literature

Teaching methods and learning activities

Theoretical-practical classes: presentation of the themes with the support of audiovisual tools. It will be given a special emphasis to the application of students’ knowledge to everyday life situations and phenomena related to Chemical Engineering. Problems resolution.

Evaluation Type

Assessment Components

Amount of time allocated to each course unit

Eligibility for exams

Laboratory classes are mandatory to all students, including those under Article 4 a) and b).

The students must have necessarily done all the practical works, as well as shown proper preparation and execution of the works and should develop in the laboratory notebook the discussion of the results. The teacher can request the laboratory notebook in the following week.

The opportunity to repeat the work in case of an excused absence is provided. However, the date of work replacement must be scheduled in advance and in accordance with the availability of the lab.

Calculation formula of final grade

FG = 0,05 AS +0,30 MT + 0,30 PRES + 0,35 REL

AS – Assiduity and punctuality grade in all classes (AS=20 for 0 non-attendances; AS=10 for 1 and 2 non-attendances; AS=0 for >3 non-attendances). It should be noted that for the purposes of this evaluation component, 10 minutes after the start of classes will be reported non-attendance, even if the student attends the class later. In the laboratory classes is not allowed to enter after 15 minutes of the beginning of the class.

MT – average grade of the two mini-tests of 15 min (T/F). These tests will not be scheduled and they will take place at theoretical-practical classes. Students have to reach a minimum grade of 7 out of 20. If students skip one of the tests or not reach the minimum grade, they can perform this evaluation component in the last week of classes in a global mini-test.

PRES – average grade of two oral group presentations on the results and discussion of one lab work (randomly assigned).

REL – Grade of the group report drawn on the last day of the practical works. Deadline: 17 hours of the 21st December 2012.

Students have to reach a minimum grade of 10 out of 20 to complete the course. 

IMPORTANT: Obvious cases of plagiarism will be penalized with a zero in its evaluation component.

Examinations or Special Assignments

not applicable

Special assessment (TE, DA, ...)

An exam at the special season.

Students should have lab frequency and should have done the report (REL).

The exam will focus on the mini-tests component (MT) and practice evaluation. This will consist of questions related to the practical work and the final classification (CF1) is given by:

CF1 = 0,65 EE + 0,35 REL

EE – practical exam in special season (minimum grade of 7/20) and REL- report

Students have to reach a minimum grade of 10 out of 20 to complete the course. 

Classification improvement

Students who have attended classes and have a grade to all components of assessment, but have not passed in the regular season, or wishing to undertake improvement of classification, may perform the exam at the recurso season that will focus on the mini-tests component (MT) and practice evaluation. The final classification (CF2) is given by:

CF2 = 0,65 EE + 0.35 REL

EE – practical exam in special season (minimum grade of 7/20) and REL- report

Students have to reach a minimum grade of 10 out of 20 to complete the course. 

Observations

Students, who are repeating the course, have to do one of the group laboratory assignments (must be scheduled). They have to write a complete individual report about it. They also have to attend to the global mini-tests in the last week of classes. The final classification (CF3) is given by:

CF3 =  0,65 MT + 0,35 REL

MT – grade of the global mini-test (minimum grade of 7/20) and REL- report

Students have to reach a minimum grade of 10 out of 20 to complete the course.