This course encompasses a set of laboratory practices with which it is intended that the student gains knowledge on the Basic safety standards in a chemical laboratory, acquire skill in the following basic operations:

preparation and titration of solutions, solid/liquid and liquid/liquid separation techniques, purification techniques and gas and solid handling techniques.



In fact, thanks to this subject the student will acquire the following skills:

M01CM03- Safe use of the usual means and techniques of a laboratory

M01CM05- Ability to observe, analyze and present results in the field of chemistry and other experimental sciences.

M01CM09- Use of the various experimental sciences for the understanding of chemical phenomena

M01CM11- Knowledge and use of the most common sources of information and documentation in experimental sciences.

THEORY PROGRAM

1. Work and safety standards in the laboratory. Basic safety rules in the laboratory. Personal protection. Description and handling of laboratory equipment. Cleaning and drying of glassware. Chemical reagents handling. Commonly used toxic and dangerous substances. Appropriate use of fume hoods. Waste management.

Organization and management. Quality management in a chemical laboratory. Preparation and presentation of the laboratory notebook. Data treatment. Bibliography management. Report writing.

2. Fundamental operations. Weighing methods. Most used concentration units. Preparation and tritation of solutions. Preparation of liquid-liquid and solid-liquid aqueous solutions. Acid-base or redox volumetry.

3. Chemical reactivity. Acid-base reactions. PH measurement methods. Redox reactions. Reactions with gas evolution. Reversible and irreversible reactions. Precipitation reactions. Separation of precipitates. Complex formation. Performance of a reaction. Solid state reactions: thermal decomposition.

4. Separation and purification techniques.

Inorganic compounds crystallization. Fundamentals. Types of crystallization. Crystallization by evaporation of the solvent, by addition of solvent, by temperature variation and by sublimation. Crystal separation.

Recrystallization of organic compounds: choice of solvent. filtration and drying. Melting points. Material and process.

Extraction. Fundamentals. Partition coefficient. Liquid-liquid and solid-liquid extraction. Material and procedure. Desiccant agents. Acid-base extraction.

Distillation. Fundamentals. Types and utility. Boiling point. Simple, fractional, vacuum and steam distillation. Azeotropic mixtures. Material and procedure.

Chromatography. Fundamentals. Types of chromatography. Utility. Stationary phase: types of adsorbents. Mobile phase. Thin layer chromatography technique (TLC). Retention factor (Rf).



LABORATORY PRACTICE PROGRAM

Practice 1. INORGANIC SYNTHESIS. CRYSTALLIZATION

Management and identification of basic laboratory material. Weighing methods: types of scales in the laboratory. Synthesis and crystallization of (NH4) 2Ni (SO4) 2.6H2O. Crystal separation, washing and drying. Reaction yield. Crystallization by temperature variation, by evaporation of the solvent, by addition of solvent, and by diffusion between solvents.

Practice 2. PREPARATION OF SOLUTIONS. ACID-BASE TRITATION

Management and identification of basic laboratory material. Liquid volume measurements: Volumetric material. Preparation of solutions: Elementary techniques and concepts, most used concentration units. Acid-base Volumetry.

Practice 3. OBTAINING AND IDENTIFICATION OF GASES.

Gas generation and identification. Glassware preparation for the reation implementation.

Practice 4. REACTIONS IN TEST TUBE

Chemical reactivity: pH changes, color changes, gas evolution, reversible and irreversible reactions, complex formation, ion exchange, redox reactions.

Practice 5. PRECIPITATION REACTIONS.

Preparation of solids by precipitation. Solids separation by filtration/centrifuging/spin cycling. Cation identification. Analytical march.

Practice 6. EXTRACTION I. Extraction of caffeine from tea.

Reflux heating, extraction, drying, filtration, solvent evaporation.

Practice 7. EXTRACTION II. Acid base extraction. Separation of a mixture of ethyl 4-aminobenzoate, benzoic acid and fluorene.

Extraction, drying, filtration, solvent evaporation.

Practice 8. CRYSTALLIZATION. Solids purification. Crystallization of benzoic acid and fluorene.

Reflux heating, filtration, crystallization.

Practice 9. DISTILLATION. Simple and fractional distillation. Purification of a liquid and separation of liquids. Distillation, boiling point, separation of two liquids.

Practice 10. CHROMATOGRAPHY. Thin layer chromatography. Identification of painkillers: ibuprofen, paracetamol, aspirin, caffeine.

Thin layer chromatography, Rf calculation, compound identification.

Seminars (2 hours) where the characteristics and details of the subject are specified, classroom practices (14 hours) which consist of explaining each practice to be carried out and solving problems related to the way the basic operations are conducted in the laboratory. (44 hours).

ORDINARY ASSESSMENT:



A. CONTINUOUS EVALUATION.



1. CONDUCT OF THE PRACTICES

- Mandatory character.

- The appropriate handling of reagents and laboratory material will be evaluated.

- Weight of this section: 30%. Minimum grade: 4.



2. INDIVIDUAL WORKS

- Mandatory character.

- The comprehension and explanatory capacity of phenomena and processes will be evaluated.

- The delivery of all the questions answered corresponding to each practice is essential.

- Weight of this section: 25%. Minimum grade: 4.



3. THEORETICAL EXAMINATION

- Mandatory character.

- The appropriate approach and the accuracy and coherence of the response will be evaluated.

- Weight of this section: 20%. Minimum grade: 4.



4. PRACTICAL EXAMINATION

- Mandatory character.

- Skill in basic laboratory operations and respect and compliance with the standards of security.

- As support material, only the laboratory notebook (DIN A4) written by the student or

student during practical sessions and signed by the teacher.

- Weight of this section: 25%. Minimum grade: 4.



RESIGNATION

- To give up the continuous evaluation, it is necessary to indicate it in writing to the teachers before week 9.

- It will be enough to not take the exams to renounce the ordinary call.



B. FINAL EVALUATION.



1. PRACTICAL EXAM

- Mandatory character.

- The appropriate handling of reagents and laboratory material, understanding and explanatory capacity of phenomena and processes and skill in basic laboratory operations, as well as respect and compliance with safety rules.

- Weight of this section: 80%. Minimum grade: 4.



2. THEORETICAL EXAMINATION

- Mandatory character.

- The appropriate approach and the accuracy and coherence of the response will be evaluated.

- Weight of this section: 20%. Minimum grade: 4.





GIVE UP THE CALL

- It will be enough to not take the final exam to waive the ordinary call.

Lab coat. Safety glasses. Laboratory gloves. Spatula. Laboratory notebook, DIN A4 size

Basic bibliography

Basic bibliography

1. M. Fernández González, Operaciones de laboratorio en Química, Anaya, Madrid, 2004.

2. M. J. Insausti, E. Charro, P. Redondo, Manual de experimentación básica en Química, Universidad de Valladolid, Valladolid, 1999

3. J. Martínez Urreaga, Experimentación en química general, Thomson, Madrid, 2006.

In-depth bibliography

In-depth bibliography
M. A Martínez, A. G. Csákÿ, Técnicas experimentales en síntesis orgánica, Síntesis, Madrid, 1998.
J. Tanaka y S.L. Suib, Experimental Methods in Inorganic Chemistry. Prentice Hall (1999).
J.D. Woollins, Inorganic experiments. 2ª ed., VCH Publishers: Nueva York (2003).

Journals

Journal of Chemical Education