Instrumental Methods of Analysis

Code:

EQ0129

Acronym:

MIA

Keywords
Classification	Keyword
OFICIAL	Physical Sciences (Chemistry)

Instance: 2020/2021 - 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	11	Syllabus	3	-	6	56	162
MIEQ	78	Syllabus	2	-	6	56	162

Teaching language

Portuguese

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, atomic emission spectroscopy, electrochemical and separation methods (chromatographic);
• 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 provide the necessary skills to enable students to select a particular analytical technique to solve a problem, to determine possible 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 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

B-learning

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 inductively coupled plasma (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:

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.
The laboratory classes take place in the laboratory of Instrumental Methods of Analysis of DEQ (E105) and 6 groups will be formed per class. Students must do 7 laboratory works (T0-T6).

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:

Remote classes and synchronous information sessions. 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.

Laboratory Classes (alternating face-to-face classes):

Experimental works, analysis and discussion of the results.

keywords

Physical sciences > Chemistry > Instrumental analysis

Evaluation Type

Distributed evaluation without final exam

Assessment Components

Designation	Weight (%)
Teste	40,00
Trabalho escrito	30,00
Apresentação/discussão de um trabalho científico	15,00
Participação presencial	15,00
Total:	100,00

Amount of time allocated to each course unit

Designation	Time (hours)
Estudo autónomo	75,00
Frequência das aulas	56,00
Trabalho escrito	25,00
Apresentação/discussão de um trabalho científico	6,00
Total:	162,00

Eligibility for exams

Laboratory classes are mandatory to all students, including those who have a special status (article 4, paragraph a) and 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.

Calculation formula of final grade

Final grade (FG) is given by:

FG = 0.40 MT + 0.15 LQ +0.15 OP + 0.30 REP

where:

MT – average grade of the two mini-tests of 20 min (True/False), scheduled to 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 must perform this evaluation component at the special examination period.

LQ – average grade obtained in questions that will be asked to students at the beginning of each laboratory class, answered individually and in writing.

OP – grade obtained in the oral presentation and discussion of one of the laboratorial works, selected by the professor;

REP – grade of the group report related to one of the laboratorial works, selected by the professor. The final report should be delivered in paper to the technicians/professors until 5:00 p.m. on January 4^th, 2021.

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 (REP). The final classification (FG1) is given by:

FG1 = 0.70 SE + 0.30 REP

where:

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

Students have to reach a minimum grade (FG1) 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, LQ, OA e REP), 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 Grade (FG2) in this case will be given by:

FG2 = 0.70 SE + 0.30 REP

where:

SE – grade of the exam at the special examination period.

Students have to reach a minimum grade (FG2) of 10 out of 20 to complete the course.

Observations

Repeating students with practical frequency, wishing to be exempted from laboratory classes, must present a complete report (prepared individually) of one of the laboratory works, to be agreed with professors until the end of October. The final classification (FG3) is given by:

FG3 = 0.70 SE + 0.30 REL

where:

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

Students have to reach a minimum grade (FG3) of 10 out of 20 to complete the course.