Advanced techniques for sample preparation

To present the advanced analytical techniques in sample preparation. To show the analytical possibilities of the new developments showing the different working modalities in each case and describing the use of different types of equipment. To describe the analytical problems existing in the determination of substances at trace level showing the most frequently used approaches in the determination of organic and inorganic species.

Unit 1.- Introduction to sample preparation techniques. Importance of sample preparation. Classical extraction techniques. Enzymatic treatment of the sample. New trends in sample preparation. Passive sampling devices. Active air sampling.

Unit 2.- Supercritical Fluid Extraction. Properties of supercritical fluids. Instrumentation for SFE. SFE Operating Parameters. Extractions modes: off-line and on-line methods. Applications.

Unit 3.- Microwave-Assisted Extraction. Theoretical Principles. Microwave heating. Solvent selection. Instrumentation. Applications.

Unit 4.- Pressurized Fluid Extraction. Theoretical Considerations. Instrumentation for PFE.
Method Development. Applications.

Unit 5.- Solid Phase Extraction. Theoretical Considerations. Types of SPE Media (Sorbent). SPE Formats and Apparatus. Method development. Automation and On-Line SPE. Microextraction in a Packed Syringe (MEPS). Dispersive Solid Phase Extraction (DSPE,QuECHers). Matrix Solid Phase Dispersion (MSPD)

Unit 6.- Solid Phase Microextraction. Introduction. Theoretical Considerations. Extraction modes. Types of SPME media (fibers, coatings). Factors Affecting SPME. Quantification. Automation. Aplications

Unit 7.- Liquid-phase microextraction. Principles. Different approaches. Single-drop microextraction (SDME). Membrane Assisted Solvent Extraction (MASE). Hollow fiber-LPME. Dispersive liquid-liquid microextraction (DLLME). Ultrasound-Assisted Emulsification-Microextraction (USAEME). Applications

Seminars:
Session 1: Enabling the student in the search and selection of information in the area of the chemical analysis.
Session 2 and 3: Two seminar sessions will be devoted to selection of recent applications with the objective of preparing and presenting the applications of the topics and to be able to discuss them in group.
Session 4: Analysis of allergen fragrances in cosmetics by accelerated solvent extraction (ASE) and matrix solid phase dispersion (MSPD).
Session 5: Determination of PAHs in water by solid phase extraction (SPE)
Session 6: Analysis of PCBs by SPME and GC-MS
Session 7. Application of DLLME and/or MEPS to the extraction of different analytes.

Basic Bibliography:
Pawliszyn J. Ed.: Comprehensive Sampling and Sample Preparation. Elsevier. Amsterdam, (2012)., Sheffield
Complementary bibliography:
E. Ibañez, A. Cifuentes. Green Extraction Techniques. Elsevier 2017.
Cela, R.; Lorenzo, R.A.; Casais, C.: Técnicas de Separación en Química Analítica, Ed Síntesis, Madrid (2002).
Dean J.R. (Ed.): Extraction Techniques in Analytical Sciences. Wiley (2009).
Janusz Pawliszyn and Heather L. Lord. Handbook of Sample Preparation. Wiley (2010)
J.M. Kokosa, A.Przyjazny, M.A. Jeannot. Solvent Microextraction. Wiley (2009).
Self R.: Extraction of Organic Analytes from Foods, The Royal Sociaty of Chemistry (RSC) (2005).
Mitra S. (Ed) (2003): Sample Preparation Techniques in Analytical Chemistry, Wiley, New Jersey.
Fritz J.S.: Analytical Solid-Phase Extraction, Wiley-VCH. New York (1999).
Pawliszyn J.: Solid Phase Microextraction. Teory and Practice. Wiley-VCH. New York (1997).
Pawliszyn J. Ed: Applications of solid phase microextraction. RSC Chromatography Monographs. Cambridge (1999).
Scheppeers Wercinski S.A. Ed.: Solid Phase microextraction. A practical guide. Marcel Dekker, Inc. New York (1999).

General skills

*CG2 - Identify information of the scientific literature using the appropriate channels and integrate the information to pose and contextualise a subject of investigation
*CG5 - Use scientific terminology in English to argue the experimental results in the context of the chemical profession
*CG6 - Apply properly the new technologies of catchment and organisation of information to solve problems in the professional activity
*CB7 - The students should know to apply the knowledges purchased and his capacity of resolution of problems in new surroundings or little known inside contexts wider (or multidisciplinary) related with his area of study
*CB9 - The students should know to communicate their conclusions and the knowledges and the last reasons that souport to skilled publics and no specialised of a clear way and without ambiguities
*CB10 - That the students possess the skills of learning that allow them continue studying of a way that will have to be to a large extent self-directedor autonomous.

Specific competitions:


*CE2 - Propose alternatives for the resolution of chemical problems complexes of the different chemical specialitys.
*CE6 - Design processes that involve the treatment or elimination of dangerous chemical products.
*CE9 - Value, promote and practise the innovation in the industry and in the chemical investigation.
*CE7 - Operate with instrumentation advanced for the chemical analysis and the structural determination.

Transversal competitions .

*CT1 - Elaborate, write and defend publicly reports of scientific character and technician.
*CT3 - Work with autonomy and efficiency in the daily practice of the investigation or of the professional activity.
*CT4 - Appreciate the value of the quality and the continuous improvement, acting with rigour, responsibility and ethical professional

MD1. Theoretical face-to-face classes. Lectures (utilisation of blackboard, computer, cannon), complemented with the own tools of the virtual teaching.
MD3. Seminars with Master's teachers, or with professionals invited of the company, the administration or of other universities. Interactive sessions related with the distinct matters with debates and exchange of opinions with the students.
MD4. Resolution of practical exercises (problems, question type test, interpretation and processing of the information, evaluation of scientific publications, etc.)
MD5. Tutoríals Individual or in group reduced.
MD6. Realisation of works, so much individually, as in group, on scientific subjects related with the distinct matters of the Master.
MD7. Oral exhibition of works, reports, etc., including debate with professors and students.
MD8. Utilisation of skilled computer programs and internet. On-line educational support (Virtual Campus).
MD9. Experimental work on basic technicians of work in laboratory
MD10. Personal study based in the different sources of information
MD11. Realisation of the different proofs for the verification of the obtaining so much of theoretical knowledges like practical and the acquisition of skills and attitudes

Due to the health uncertainty caused by the COVID 19 crisis, three possible scenarios are contemplated.

Scenario 1: adapted normality (without restrictions to physical attendance).
The expository and interactive teaching will be fundamentally face-to-face, although in an exceptional and justified way telematic teaching may be combined with face-to-face teaching up to a maximum of 10% of the hours of the subject, and in the case of practical teaching carried out with means telematics may be up to 25%.

The tutorials may be partially carried out electronically.

Final tests will be in person.

The evaluation will be continuous and will be based on:

- The assistance and participation in the theoretical sessions, seminars and tutorials that constitute this course (10% global evaluation)

- Elaboration of a work and exposition. Adequacy of the contents to the suggested subject
Clarity in the written and oral presentation, capacity of synthesis. Level of understanding of the presented work. (10% global evaluation)

- Discussion in the tutorials and Presentation and discussion of the work (written and oral) (10% global evaluation)

- Work in the seminars: Planning, organization and skills in the work. Motivation and profit (10 % global evaluation)

- The obligatory accomplishment of an examination type test covering the contents of the course. Evaluating: Domination of the knowledge, resolution of questions and capacity of expression and of synthesis (60% global evaluation).

The qualification will be obtained as result of applying the following formula:
Final qualification= 0.4 x N1 +0.6 x N2
Being N1 the numerical note corresponding to the continuous evaluation (scale 0-10) and N2 the numerical note of the final examination (scale 0-10).
- The repeating students will have the same regime of assistance to the classes as those that pass on the matter for the first time will.


"For cases of fraudulent performance of exercises or tests, the one set forth in the Regulations for the evaluation of the academic performance of students and the review of grades will apply."

It is estimated that in addition to daily attendance, students must dedicate approximately 1-2 hours of personal work per each lecture or seminar hour.

Study time and personal work that a student must dedicate to overcome it
Study time and individual work

PRESENTIAL WORK IN THE CLASSROOM HOURS PERSONAL WORK OF THE STUDENT HOURS
Large group expository classes 12 Individual autonomous study in group 12
Small group interactive classes (Seminars) 7 Resolution of practical cases and assignments 21
Small group tutoring 2 Preparation of oral, written presentations, preparation of proposed exercises. Similar activities in library 21
Total hours of face-to-face work in the classroom or laboratory 21 Total hours of personal work of the student 54

- Class attendance.
- Study of the questions and problems formulated in the seminar classes before doing them.
- Class active participation, especially in the seminar classes.
- Consultation of the recommended bibliography.
- To attend the tutorial hours along the term when necessary.