Instrumental Methods of Analysis

Code:

EQ0129

Acronym:

MIA

Keywords
Classification	Keyword
OFICIAL	Physical Sciences (Chemistry)

Instance: 2014/2015 - 1S

Active?	Yes
Responsible unit:	Department of Chemical and Biological 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
MIB	17	Syllabus	3	-	6	56	162
MIEQ	87	Syllabus	2	-	6	56	162

Teaching language

Suitable for English-speaking students

Objectives

The main objectives are:

·         To provide an adequate knowledge of the principles, instrumentationand applications of commonanalytical techniques,includingatomic and molecular absorption spectroscopy, electrochemical andseparationmethods(chromatographic andelectrophoretic);

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

·         To providethe necessary skillsto enablestudents toselect a particularanalytical techniqueto solveaproblem, to determine possible restrictions, to select themost appropriateanalytical methodologies, to identify alternatives, to compare the advantagesand disadvantages of eachoneand 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 equipment’s 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, pre-concentration, 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

Presencial

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 vapor and hydrides generator for arsenic and selenium.Electrochemical methods. Potentiometric determination with ion selective electrodes. Theory of chromatography. Gas chromatography with flame ionization, electron capture and mass spectrometry detectors. High performance liquid chromatography with ultraviolet/visible detection and fluorescence.

Laboratory program: The laboratory classes take place in the laboratory of Instrumental Methods of Analysis of DEQ (E105) and 8 groups per class 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 - To obtain validation parameters of the cadmium analysis method in solids by atomic flame absorption spectroscopy after acidic digestion. In the following weeks the students will perform 4 works, using the principles of an analytical technique selected previously, intercalated with weeks of problems solving and an intermediate report. The works to be performed are:

T1.Determinationof copper content in a copper wire by flame atomic absorption spectrophotometry (AAS)

T2. Determination of the salt content in a soup by ion selective electrode with potentiometric detection

T3. Analysis of caffeine in different types of coffees by HPLC-UV

T4. Determination of the purity of recuperated acetone by gas chromatography coupled with flame ionization detection (GC- FID) using the internal standard method

In the last week, all students will do the work T5 – Identificationof contaminants of recoveredorganic solventsby GC-MS.

Mandatory literature

Douglas A. Skoog, Donald M. West, F. James Holler; Fundamentals of analytical chemistry. ISBN: 0-03-074922-0
Douglas A. Skoog, James J. Leary; Principles of instrumental analysis. ISBN: 0-03-075398-8
James N. Miller and Jane C. Miller; Statistics and chemometrics for analytical chemistry. ISBN: 0-13-022888-5

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; Resolution of key-problems.

keywords

Physical sciences > Chemistry > Instrumental analysis

Evaluation Type

Distributed evaluation without final exam

Assessment Components

Designation	Weight (%)
Exame	35,00
Teste	35,00
Trabalho escrito	30,00
Total:	100,00

Amount of time allocated to each course unit

Designation	Time (hours)
Elaboração de relatório/dissertação/tese	56,00
Estudo autónomo	26,00
Frequência das aulas	56,00
Trabalho laboratorial	24,00
Total:	162,00

Eligibility for exams

Laboratory classes are mandatory to all students, including those who have a special status (artigo 4ª, alíneas a) e 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. This can be requested by the teacher in the following week. If students skip one assignment, they have to justify their absence and then they can do the assignment, since the substitution is combined with at least two weeks in accordance with the laboratory availability.

Calculation formula of final grade

FG = 0.35 MT + 0.10 RINT +0.35 EP + 0.20 REL

where:

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 at the special examination period.

RINT – average grade of one intermediate report about a laboratorial work (sorted) .

EP – Grade of practical written exam, performed on 28th november. Open-response questions about the analytical methods studied in the laboratory classes will be done, as well as calculating results and discussion of them. If practical exam grade is less than 7/20, the students can do this component at the special examination period.

REL – Grade of the group report related to one of the laboratorial works, sorted in the day of the practical written exam. The deadline is up to 17 hours of the 31st December 2014.

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

 

Examinations or Special Assignments

Not applicable

Special assessment (TE, DA, ...)

An exam at the special examination period. Students have to attend to the laboratory classes and do all the assignments. Students should havepractical frequencyand should have done the report (REL). The exam will focus on the mini-tests (MT) and practical written exam (EP). The final classification is given by:

             CF1 = 0.80 EE + 0.20 REL

             where: EE – exam grade at the special examination period (minimum grade of 7/20).

Students have to reach a minimum grade (CF1) of 10 out of 20 to complete the course.

Classification improvement

Studentswho have attendedclasses and havea grade toallcomponents of assessment,but have not passedin theregular examination period, orwishing to undertakeimprovement of classification, may perform the exam at the special examination period:

              CF2 = 0.50 ER + 0.20 RINT + 0.30 REL

              where: ER – grade of the exam at the special examination period.

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 laboratory assignments in group and date to be arranged by the end of September. They have to write an individual report about it (REL).They also have to attend to the mini-tests and the practical written exam. The final classification is given by:

CF2 = 0.35 MT + 0.35 EP + 0.30 REL

Students have to reach a minimum grade (CF2) of 10 out of 20 to complete the course.