Analytical Techniques

This course is key to the chemistry module and that provides students with basic knowledge about the nature of the reactions in solution, and the fundamental principles and procedures for analytical determination of compounds. Also, the knowledge is applied in the laboratory analysis of water, food, health and environmental interest. It is also related to other subjects in the form of elemental chemistry and to achieve the skills of some subjects of the modules of Medicine and Pharmacology, Pharmacy and Technology and Biology.

UNIT 1 .- INTRODUCTION TO THE TECHNICAL ANALÍTICAS. Objective, purpose, methodology and classification of Analytical Techniques. Importance of the stages of the analytical process. Basic calculations: concentration and stoichiometry of reactions in solution.

UNIT 2 .- SAMPLING AND SAMPLE MANAGEMENT. Terminology related to the sample. Sampling plan. Sampling errors. Conservation of the sample. Sample preparation: dissolution and extraction and preconcentration techniques for the analysis of water, food, health and environmental interest.

UNIT 3 .- ANALYTICAL TREATMENT OF SOLUTION EQUILIBRIA I. VOLUMETRIC ANALYSIS. Overview: Characteristics of reactions used in titrations. Assessment procedures. Acid-base titrations: Titration Curves, acid-base indicators. Complexation titrations: titration curves, indicators metallochromic Applications.

UNIT 4.- ANALYTICAL TREATMENT OF SOLUTION EQUILIBRIA II.Volumetrías Precipitation: titration curves, indicators endpoint systems. Volumetric redox titration curves, redox indicators. Oxidizing and reducing reagents. Applications of volumetric methods. Gravimetric.

UNIT 5 .- BASIC CHARACTERISTICS OF QUALITATIVE ANALYTICAL INFORMATION. Introduction. Binary response. Errors: false positives and negatives. Classical Qualitative Analysis: reagents and systematic processes. Introduction to instrumental qualitative analysis .

UNIT 6 .- EVALUATION OF ANALYTICAL RESULTS. Analytical errors: random and systematic. Accuracy and precision. Confidence interval. Test results comparison. Anomalous error detection: Dixon's Q test. Expression of analytical results.

UNIT 7 .- SELECTION AND VALIDATION OF THE METHOD OF ANÁLISIS.Introducción. Selecting the method of analysis. Calibration Standards and Analytical Techniques. Validation of methods: concept and types. Quality parameters: Analytic properties supreme, basic and complementary.

UNIT 8.- QUALITY SYSTEMS IN THE ANALYTICAL LABORATORY. Introduction to quality: concept of quality, types and structure. Quality systems in analytical laboratories. Rules. Good laboratory Practices. Evaluation of analytical quality.

Program of practical classes:

Practice 1. Qualitative analysis
-Study of reactions in aqueous solution. Various aspects of chemical equilibrium.
-Identification of NH4+ and NO2- and NO3- anions in water.

Practice 2. Acid-Base Titrations in Aqueous Solution.
A) Titration of hydrochloric acid with sodium carbonate
B) Determination of the Na2CO3 and NaHCO3 content of a mixture.

Practice 3. Redox Titrations.
A) Normalization of a solution of potassium permanganate with oxalic acid.
B) Titration of hydrogen peroxide with potassium permanganate.

Practice 4. Application of an Iodometric Titration
A) Titration of a sodium thiosulfate solution
B) Determination of the content of hypochlorite and active chlorine in a sample of bleach

Practice 5. Development of an analytical process.
-Determination of iron in a vitamin complex.

Basic bibliography

1.- D. C. HARRIS. Quantitative Chemical Analysis Editor W. H. Freeman, 2016
2. D.A. SKOOG, D.M. WEST, F.J. HOLLER, S.R. CROUCH "Fundamentos de Química Analítica". 9ª Ed. CENGAGE Learning, Mejico (2015).

Complentary bibliography

1.- M. VALCARCEL. "Principios de Química Analítica". Springer, Barcelona (1999).
2.- D. HARVEY. “Química Analítica Moderna”. Mc Graw Hill. Madrid (2002). "Modern Analytical Chemistry”. Mc Graw-Hill. New York (2000).
3.- M. SILVA y J. BARBOSA. “Equilibrios iónicos y sus aplicaciones analíticas “. Ed Síntesis. Madrid (2002).
4.- C. CÁMARA, P. FERNÁNDEZ, A. MARATÍN-ESTEBAN, C. PÉREZ-CONDE y M. VIDAL. Toma y tratamiento de muestras . Ed Síntesis. Madrid (2002).
5.- MILLER, J.C. MILLER, J.N. “Estadística y Quimiometría para Química Analítica”. 2ª Prentice Hall. Madrid (2002)
6.- ÁVILA ROSÓN, J.C., FERNÁNDEZ GUTIERREZ, A., ALONSO HERNÁNDEZ, E.J., FERNÁNDEZ SÁNCHEZ, J.F. "Equilibrios químicos en disolución: Aplicaciones". Ed. Universidad de Granada. Granada (2005).
7.- R. COMPAÑÓ BELTRÁN Y A. RIOS CASTRO. “Garantía de calidad en los laboratorios analíticos”. Ed Síntesis. Madrid (2002)

Calculations bubliography

1.- P. YÁÑEZ-SEDEÑO ORIVE; J.M. PINGARRÓN CARRAZÓN; F.J. DE VILLENA RUEDA.- “Problemas resueltos de química Analítica”. Ed Síntesis. Madrid (2003).
2.-T. P. HADJIIOANNOU, G. D. CHRISTIAN, M.A.KOUPPARIS y P.E. MACHERAS. “Quantitative Calculations in Pharmaceutical Practice and Research” Ed. VCH, New York (1993)
3.- J. Guiteras, R. Rubio, G. Fonrodona “Curso experimental en Química Analítica” Ed. Síntesis. Madrid (2003).

KNOWLEDGE:
Know 11. Know the physical-chemical characteristics of the substances used to manufacture medicines.
Know 12. Know and understand the characteristics of reactions in solution, the different states of matter and the principles of thermodynamics and their application to pharmaceutical sciences.
Know 13. Know and understand the characteristic properties of elements and their compounds, as well as their application in the pharmaceutical field.
Know 14. Know and understand the nature and behavior of functional groups in organic molecules.
Know 15. Know the principles and procedures for the analytical determination of compounds: analytical techniques applied to the Know 16. Know and apply the main structural research techniques including spectroscopy.

COMPETENCES
Comp 01. Capacity for analysis and synthesis.
Comp 02. Ability to organize and plan
Comp 03. Oral and written communication in one's own language.
Comp 05. Basic computer handling skills.
Comp 06. Information management skills (ability to search and analyze information from diverse sources).
Comp 07. Problem solving.
Comp 10. Critical capacity and self-criticism.
Comp 11. Teamwork.
Comp 18. Ability to apply knowledge in practice.
Comp 20. Ability to learn.
Comp 28. Concern for quality.

A) Large group expository classes (“CE” in the time tables): Explanation of the theoretical foundations of each topic, complemented by general examples and resolution of exercises related to analytical techniques applied to the analysis of water, food and the environment. These classes will be carried out in person and students will have additional material on the virtual platform of the USC (Virtual Classroom).
B) Interactive classes in small groups (Seminars, “S” in the time tables): The Teacher will provide the student, periodically and well in advance, exercise bulletins and practical cases. The teacher will solve doubts about exercises and will debate with the students in person. The participation of the students is required, since the deliveries of some proposed exercises are part of the continuous evaluation. During the semester they will consider carrying out a small group work and will be exposed in the classroom.
C) Interactive practical laboratory classes: The classes that take place in a practical laboratory are included here. In them the student acquires the skills of working in a laboratory and consolidates the knowledge acquired in the exhibition classes. The student will carry out different experiments in which they will become familiar with the experimental application of the analytical concepts and methodologies explained. The student's personal work, outside the laboratory, of the students in this activity is much smaller. In support of practical teaching, the student will have a laboratory practice manual, which will include general considerations on the work in the laboratory, as well as a script for each of the practices to be carried out, which will consist of a brief presentation of the fundamentals, the methodology to be followed and the indication of the calculations to be made and results to be presented. The student must go to each practice session having carefully read the content of this manual. After an explanation from the teacher, the student will carry out individually or in small groups, the experiences and calculations necessary to achieve the objectives of the practice, collecting in the laboratory diary the development of the practice and the calculations and obtained results. The student will cover a report with this information and the resolution of some questions, for each practice. The portfolio or report will be made individually and will be evaluated by the corresponding practice teacher.
The student will not be evaluated if he does not carry out and pass the laboratory practices.
It is not mandatory to repeat the practices if they were carried out in any of the 2 academic courses prior to the current course and if the laboratory part has been approved.
D) Tutorials in a very small group (“T” in the time tables): Scheduled tutorials, which will mean for each student 2 hours per semester in person. The teacher will guide the student both in global proposals and in specific questions related to the contents of the subject. Activities such as supervising supervised works, clarifying doubts about theory or practices, problems, exercises, readings or other proposed tasks are proposed.

1. The student will not be able to pass the subject if he does not complete and pass the laboratory practices.
2. The evaluation will consist of:
- The written exam that will be taken at the end of the semester and in person. It will consist of a set of theoretical-practical questions and several numerical exercises that cover the different contents of the subject assimilated with the competencies (general and specific) and skills, representing 70% of the overall evaluation.
- Completing and passing the evaluation of the interactive laboratory classes (15 hours) will be essential to pass the subject. The practical grade is 15% of the overall grade for the subject. The practices will be evaluated on the basis of the following three items, each of which represents 5% of the overall evaluation: attendance and completion of the practices, presentation of results (via practice report or similar means) and practice exam. . This exam will consist of questions related to the practices carried out.
- Interest and participation in the expository and interactive seminar and tutorial classes and the completion of some exercises proposed by the Professor during the semester will be evaluated. In addition, the completion and presentation of a work, the ability to speak and write, and the teacher/student debate will be evaluated. The evaluation of these activities represents 15% of the overall evaluation.
3. In the second opportunity, the same evaluation criteria, described in sections 1 and 2, are maintained as in the first opportunity.
4. The evaluation of the knowledge, skills and competencies acquired in the subject will be carried out through the following means:
In the theoretical exam: Know 11, Know 12, Know 13, Know 14. Comp 01, Comp 02, Comp 28
In laboratory practices: Know 16, Comp 05, Comp 06, Comp 10, Comp 11, Comp 18, Comp 20
In interactive classes: Know 15, Comp 03, Comp 06, Comp 07, Comp 11
In cases of fraudulent completion of exercises or tests, the provisions of the Regulations for evaluating the academic performance of students and reviewing qualifications 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.
PRESENTIAL WORK IN THE CLASSROOM HOURS TUDENT'S PERSONAL WORK HOURS
Large group expository classes 30 Individual or group self-study 45
Small group interactive classes 9 Resolution of exercises. Presentation and discussion of practical cases 13,5
Works (individual or in group) 1 Preparation, presentation and exhibition 13
Laboratory practices + Report 15 Experimental work in the laboratory and preparation of the practice report 7,5
Very small group tutorials 2 Orientation and resolution of doubts 2
Examinations and review 3 Taking and Reviewing the Exam 9
Total face-to-face hours 60 Total non-contact hours 90

- Attendance at the exhibition classes.
- Previous study and completion of the exercises and questions included in the bulletins that will be delivered prior to the completion of the seminar classes.
- Active participation of the student in the seminar classes and delivery of the exercises proposed by the Professor.
- It is essential to prepare the practices or alternative activity before entering the laboratory. First, the theoretical concepts necessary to carry out each experiment must be reviewed, and then the practice script must be read carefully, trying to understand the objectives and development of the proposed experiment. Any questions that may arise should be consulted with the teacher.
- Consultation of the recommended bibliography.
- Taking advantage of the hours of tutoring during the development of the subject. Those students who encounter significant difficulties when working on the proposed activities should attend the teacher's tutoring hours, in order for the teacher to analyze the problem and help solve those difficulties.