Instrumental Methods of Analysis

Code:

EQ0129

Acronym:

MIA

Keywords
Classification	Keyword
OFICIAL	Physical Sciences (Chemistry)

Instance: 2019/2020 - 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
MIB	22	Syllabus	3	-	6	56	162
MIEQ	69	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 scientific knowledge to solve real problems and to develop 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 in electrochemistry, spectroscopy and chromatography;
• To design an analytic experiment 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 and instrumental measurement and to 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

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 of analysis. 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 determination. Electrochemical methods of analysis. 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 ultraviolet/visible and fluorescence detectors.

Laboratory program: The laboratory classes take place in the laboratory of Instrumental Methods of Analysis of DEQ (E105) and 6 groups per class will be formed. Students must do 7 laboratory works, 6 of which in a rotation scheme. In the first week all students will perform the work T0. In the weeks before FEUP’s week, the students will perform the works T1 to T3 in a rotation scheme. The week after FEUP’s week will be reserved for the preparation of the short-term report about one of the laboratorial works already performed (which will be selected by the professor). The works T4 to T6 will be carried out in the remaining weeks in a rotation scheme.

T0. Validation of an analytical method for the analysis of cadmium in soils by flame atomic absorption spectroscopy (AAS) after acid digestion;

T1. Determination of the copper content in an electrical wire by flame AAS;

T2. Determination of the heavy metals content in a soil by ICP-OES;

T3. Determination of the peroxide content in mouthwash by molecular absorption spectroscopy using the standard additions method;

T4. Determination of the salt content (Na⁺) in a food product by ion selective electrode;

T5. Determination of the concentration of the antibiotic metronidazole in an aqueous solution by HPLC-UV;

T6. Determination of the linalool (essential oil) in plant extracts by GC-FID using the internal standard method.

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, emphasizing the application of students’ knowledge to everyday issues and phenomena related with Chemical Engineering; Resolution of key-problems.

keywords

Physical sciences > Chemistry > Instrumental analysis

Evaluation Type

Distributed evaluation without final exam

Assessment Components

Designation	Weight (%)
Exame	30,00
Teste	30,00
Trabalho escrito	25,00
Trabalho laboratorial	15,00
Total:	100,00

Amount of time allocated to each course unit

Designation	Time (hours)
Elaboração de relatório/dissertação/tese	25,00
Estudo autónomo	75,00
Frequência das aulas	56,00
Trabalho escrito	3,00
Trabalho laboratorial	3,00
Total:	162,00

Eligibility for exams

Laboratory classes are mandatory to all students, including those who have a special status (article 4, paragraph a) e b)).
To obtain frequency, 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 obtained. This can be requested by the teacher in the following week.
An opportunity is given to repeat one of the works in case of justified absence, provided that the date of replacement of the work is combined with a minimum advance of 2 weeks and to the extent of the laboratory availability.

Calculation formula of final grade

FG = 0.30 MT + 0.15 RELint +0.25 REL + 0.30 EX

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.

RELint – grade of the group short-report related to one of the laboratorial works, selected by the professor. The final report (paper version) should be delivered to the professor in the following laboratorial class.

REL – grade of the group report related to one of the laboratorial works, selected by the professor. The final report (PDF file) should be sent to the professor Vítor Vilar by email (vilar@fe.up.pt) until December 26^th at 5:00 p.m. and later delivered in paper version until 4:00 p.m. on January 3^rd.

EX – grade of exam in the regular examination, performed on 13^th December. Open-response questions about the analytical methods studied in the laboratory classes will be done, as well as calculating results and discussion of them. The minimum grade is 7/20.

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

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

Examinations or Special Assignments

Not applicable

Internship work/project

Not applicable

Special assessment (TE, DA, ...)

 

An exam at the special examination period, according to the general rules. Students have to attend to the laboratory classes and do all the assignments. Students should have practical frequency and should have done the report (REL). 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

Students who have attended classes and have a grade to all components of assessment (MT, RELint and REL), but have not passed in the regular examination period, or wishing to undertake improvement of classification, may perform the exam at the special examination period. The final classification CF2 is given by:

              CF2 = 0.60 EXR + 0.20 RELint + 0.20 REL

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

 

Students with practical frequency from a previous academic year, wishing to undertake improvement of classification, must carry out one of the laboratory work in a group (date to be agreed until the end of October). They have to write an individual full report about the obtained results (REL). The final classification CF3 is given by:

 

CF3 = 0.60 EXR + 0.40 REL

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

 

Students have to reach a minimum grade (CF2 or CF3) of 10 out of 20 to complete the course.

 

Observations

Repeating students with practical frequency, wishing to be exempted from laboratory classes, must carry out one of the laboratory work in a group (date to be agreed until the end of October). They have to write an individual full report about the obtained results (REL). The final classification is given by:

CF4 = 0.60 EXR + 0.40 REL

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

 

Students have to reach a minimum grade (CF4) of 10 out of 20 to complete the course.