Instrumental Methods of Analysis

Code:

L.BIO031

Acronym:

MIA

Keywords
Classification	Keyword
OFICIAL	Basic Sciences (Mathematics, Physics, Chemistry, Biology)

Instance: 2022/2023 - 1S

Active?	Yes
Responsible unit:	Department of Chemical and Biological Engineering
Course/CS Responsible:	Bachelor in Bioengineering

Cycles of Study/Courses

Acronym	No. of Students	Study Plan	Curricular Years	Credits UCN	Credits ECTS	Contact hours	Total Time
L.BIO	19	Syllabus	3	-	6	52	162

Teaching language

Suitable for English-speaking students

Objectives

The main objectives are:

• Provide an adequate knowledge of the principles, instrumentationand applications of the most commonanalytical techniques,includingatomic and molecular absorption spectroscopy, atomic emission spectroscopy with plasma induction atomization,electrochemical and separative (chromatographic) methods;
• Provide an adequate knowledge of the main processes of extraction and handling of solid, liquid and gaseous samples and their implications in terms of analytical measurement uncertainty;
• Providethe necessary skillsto enablestudents toselect a particularanalytical techniqueto solveaproblem, determine any restrictions, select themost appropriateanalytical method, identify alternatives, compare the advantagesand disadvantages of eachand develop a critical reasoning to interpret analytical results;
• Develop communication skills, particularly of technical results, and group cooperation;
• Encourage the use of foundations of scientific theory to solve real-world problems and develop critical thinking.

Learning outcomes and competences

To achieve these objectives, students should know how to:

• Explain the principles and mode of operation of the most commonly used analytical equipment in the areas of electrochemistry, spectroscopy and chromatography;
• Design an analytic experiment to solve a real problem;
• Conduct a laboratory analysis, according to the Good Laboratory Practices, in hygienic and safe conditions, involving sample handling, extraction, pre-concentration and instrumental measurement and calculate the analytical result and its uncertainty;
• Interpret and communicate an analytical result and produce technical reports;
• Work efficiently in 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 in the selection of analytical methods. Basic concepts of validation. Sample preparation processes (LLE, SPE, SLE and SPME).

Spectral methods of analysis. Molecular absorption spectroscopy in the UV-Vis. Atomic absorption spectroscopy. Flame atomization, electrothermal and plasma induction. Cold vapor chamber for mercury analysis and hydride generator for arsenic and selenium determination.

Electrochemical methods of analysis. Potentiometric determination with ion-selective electrodes.

Chromatographic methods. Fundamentals. Chromatography theory. Gas chromatography with flame ionization, electron capture and mass spectrometry detection. High performance liquid chromatography with ultraviolet/visible and fluorescence detection.

Laboratory program:

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

T1. Determination of nickel content in an electronic board by flame AAS;

T2. Determination of heavy metals content in an electronic board by ICP-OES;

T3. Determination of peroxide content in an oral elixir by molecular absorption spectroscopy using the standard addition method;

T4. Determination of nitrates content in a soil by ion selective electrode with potentiometric detection;

T5. Determination of the concentration of UV-filters in water by HPLC-DAD;

T6. Determination of the ethanol content in an alcohol gel by GC-FID by internal standard method.

The laboratory classes are held in the laboratory of Instrumental Methods of Analysis of DEQ (E105), with 6 groups per class. Students must complete 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

Presential classes supported by audiovisual material, emphasizing the application of knowledge to everyday issues and phenomena related to Chemical Engineering and Bioengineering; Resolution of exercises, as well as on-site laboratory classes to carry out laboratory work with analysis and discussion of results.

 

keywords

Physical sciences > Chemistry > Instrumental analysis

Evaluation Type

Distributed evaluation without final exam

Assessment Components

Designation	Weight (%)
Teste	40,00
Trabalho escrito	50,00
Trabalho laboratorial	10,00
Total:	100,00

Amount of time allocated to each course unit

Designation	Time (hours)
Estudo autónomo	48,00
Frequência das aulas	48,00
Trabalho escrito	40,00
Elaboração de relatório/dissertação/tese	26,00
Total:	162,00

Eligibility for exams

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

To obtain frequency, the students must have carried out all practical works, delivered the excel data file the week after doing the work, must have shown the correct preparation and execution of the works and must prepare in the laboratory notebook the discussion of the results obtained, which can be checked by the teacher in the week following its completion.

 

Calculation formula of final grade

Final grade (FG) is given by:

FG = 0.40 MT + 0.20 REL1 + 0.30 REL2 + 0.10 A&P

where:

MT – average grade of 2 mini-tests of 20 min (multiple answer), scheduled and held during the theoretical-practical classes. Students must obtain a minimum average mark of 7/20. If a student misses any mini-test or does not obtain the minimum mark, he/she must complete this evaluation component in the special examination period.

REL 1 - grade of the interim group report, referring to one of the laboratorial works carried out in class and selected by the teacher;

REL2 – grade of the final group report, referring to one of the laboratorial works carried out in class and selected by the teacher. The final report should be delivered until 17:00 on January 4^th, 2023;

A&P – grade that includes attendance in TP and LAB classes, laboratory performance and discussion of REL 1.

NOTE: Plagiarism in any written component will be penalized with a zero grade.

 

Examinations or Special Assignments

Not applicable

Internship work/project

Not applicable

Special assessment (TE, DA, ...)

Exam in the special examination period, according to the general rules. Students must have practical attendance (implies completion of all lab works) and must have an evaluation of the REL1 and REL2 components. The final classification (FG1) is given by:

FG1 = 0.70 SE + 0.10 REL1 + 0.20 REL2

where:

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

Students must 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 evaluation components (MT, REL1, REL2, A&P), but those who have not been approved in the regular examination period, or who wish to improve their grade, may perform the exam at the special examination period. In this case, he Final Grade (FG2) will be given by:

FG2 = 0.70 SE + 0.10 REL1 + 0.20 REL2

where:

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

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

 

Observations

Repeating students with practical frequency who wish to be excused from laboratory classes, must submit a complete report of one of the laboratory works, on an individual basis, to be agreed upon with the professors by the end of October. The final classification (FG3) will be 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 must reach a minimum grade (FG3) of 10 out of 20 to complete the course