Fundamentos de Análise Instrumental

Base Knowledge

undefined

Teaching Methodologies

The teaching methodology is developed through theoretical lessons, using slides, accompanied by the presentation and development of the subjects that compose the program content. In practical classes, groups of students carry out experimental works. The experimental works includes the realization of the experiments, preparing the written report, and analyzing and discussion the results.

Learning Results

At the end of this curricular unity, is intend that the student should be able to:
• Recognize the main methods of analytical spectrometry (molecular and atomic) and chromatography (gas and liquid), including the adoption of the method to identify and quantify the sample components, sample preparation and measurement with the appropriate equipment and familiarization with the equipment used.

 • Get practical knowledge of analytical spectrophotometry (molecular and atomic) and chromatography (gas and liquid) with practical experiences through the use of spectrophotometers, chromatographs and laboratory equipment involved in the preparation of samples for analysis.

Program

THEORETICAL
1. Analytical methods
2. Concepts and fundamentals:
2.1 Terms and quantitative relations in the practice of spectroanalysis and chromatography.
3. Spectrochemical methods of analysis:
3.1 Optical molecular spectroscopy
3.1.1 Electronic absorption (or ultraviolet-visible) (molecular) spectroscopy.
3.1.2 Vibrational (or infrared) (molecular) spectroscopy
3.2 Atomic spectroscopy (absorption and emission) in the optical region.
3.3 Luminescence techniques (fluorescence and chemiluminescence).
4. Chromatographic systems: instrumentation, main separation mechanisms and types of detectors.

PRACTICES
Execution of laboratory works:

1. Simultaneous spectrophotometric determination of acetylsalicylic acid and ascorbic acid in a pharmaceutical tablet.

3. Spectrofluorimetric determination of quinine in tonic water.

4. Detection of dioctyl phthalate (DOP) in cling film by Vibrational Absorption Spectroscopy (FT-MIR)

5. Determination of ethanol in red table wines by GLC with packed column and detection by FID.

6. Determination of organic acids (L(+)-tartaric, L(-)-malic, citric, L(+)-lactic, acetic and succinic acids) in red table wines by reversed phase HPLC-UV-anion exclusion.

Curricular Unit Teachers

José Manuel Matias Vieira de Sousa

Grading Methods

The assessment of the curricular unit is continuous and periodic along the semester and will take into account:

(C1) Practical lessons: Assessment of performance in laboratory lessons: students will be assessed in all lessons of the curricular unit based on their demonstrated interest, level of learning, dynamics of each student's work in groups and punctuality.

(C2) Elaboration and assessment of summary reports of the Experimental Works, carried out in groups. Each report must be submitted on the date established at the end of each experimental work.

(C3) Written test at the end of the semester.

The final grade is obtained by adding the contributions of the various components:

C F = 0.4 * C1 + 0.25 * C2 + 0.35 * C3

If the student don´t get approval in the continuous and periodic assessment, he/she can carry out the partial exam. In this case, the final classification is obtained by adding the contributions of the various components:

C F = 0.4 * C1 + 0.25 * C2 + 0.35 * C4

Maintaining the classification of the parameters C1 and C2 obtained in the continuous assessment.

(C4) Exam (carried out during exam seasons).


    Internship(s)

    NAO

    Bibliography

    Recommended bibliography:

    Skoog, Douglas A. ; Leary, James J. (1992). Principles of instrumental analysis. Fourth Edition. Fort Worth : Saunders College Publishing. 1 vol. (multiple pages). ISBN 0-03-075398-8. Available at the ISEC Library: 6-4-33 (ISEC) – 061517

    Rouessac, Francis ; Rouessac, Annick. (2000). Chemical analysis: modern instrumental methods and techniques. English ed. Chichester [etc.] : John Wiley & Sons, Ltd, cop. 445 p.. ISBN 0-471-97261-4. Available at the ISEC Library: 6-4-3 (ISEC) – 11339

    Laboratory handshout provided in advance by the teacher

    Supplementary bibliography:

    Levine, Ira N., (2003). Physical Chemistry. 5th ed.. Boston [etc.]: McGraw-Hill. 986 p.. ISBN 0-07-123213-3. Available at the ISEC Library: 6-5-74 (ISEC) – 14838 ; 6-5-73 (ISEC) – 14839. – Repeated example

    Davies, A. M. C.; Creaser, C. S. (1991). Analytical applications of spectroscopy II. Cambridge: The Royal Society of Chemistry, cop. 321 p.. ISBN 0-85186-403-1. Available at the ISEC Library: 6-5-63 (ISEC) – 06174

    Peters, Dennis ; Hayes, John M. ; Hieftje, Gary H. (1974). Chemical separations and measurements: theory and practice of analytical chemistry. Philadelphia: W. B. Saunders, cop. XXIII, 749 p.. ISBN 0-7216-7203-5. Available at the ISEC Library: 6-4-40 (ISEC) – 00704