2023-2024 / CHIM0321-3

Practical exercises - Introduction to pharmaceutical analytical chemistry

Duration

100h Pr

Number of credits

 Bachelor in pharmacy5 crédits 

Lecturer

Philippe Hubert

Language(s) of instruction

French language

Organisation and examination

Teaching in the second semester

Schedule

Schedule online

Units courses prerequisite and corequisite

Prerequisite or corequisite units are presented within each program

Learning unit contents

The practical work in Pharmaceutical Analytical Chemistry will enable students to familiarise themselves with good analytical practices by learning to correctly handle the equipment available in the student laboratory (analytical balance, scales, volumetric glassware, etc.). This practical work also aims to raise students' awareness of the concepts of quality assurance and statistics (concept of error and number of significant digits) necessary for any analysis. During the first sessions, students will be asked to describe the glassware they will mostly use for the operations that will follow. Ungraded sessions in smaller groups will allow students to practice the correct handling of glassware, analytical balances and scales.  Students will also have the opportunity and supervision required to perfect or acquire theoretical notions of the basics necessary to carry out their practical work. During this first period, students will have to solve a series of mandatory prerequisite exercises on the eCampus platform. The resolution of these exercises may require the revision of theoretical concepts seen during General Chemistry in Block 1. In addition, a manual of prerequisites will be available on the platform which will enable students to revise certain theoretical concepts essential to the practical work of pharmaceutical analytical chemistry. Thereafter, students will be evaluated on taking a sample using a measured pipette and simple handling involving accurate weighing and a quantitative transfer. On the basis of a percentage of error determined during a physical-chemical test, students should be able to analyse the quality of each step using a list containing all the critical points from weighing to drawing up the sample solution.

The practical sessions that follow will aim to provide the student with rigour, autonomy, care and organisation through a series of quantitative analyses, mainly by titrimetry (direct, indirect and back titrations), involving acid-base, redox, complexometry and precipitation reactions. A quantitative analysis will also be performed in UV-visible spectrophotometry allowing students to build a calibration curve and measure, in this interval, unknown samples through an appropriate use of the least squares regression model. Finally, a potentiometric titration of vanadyl sulphate in the form of a virtual practical session will be available on the eCampus platform and will be the subject of a report. This work will be evaluated on the basis of the quantitative results achieved and the quality of the electronic reports provided.

As an integral part of the practical work, a seminar will cover the concepts of pH and the preparation of buffer solutions. Exercises around these theoretical concepts will be carried out in the presence of the students. An exercise session will also be offered to students on tolerance and dilutions. Finally, through this practical work, students should learn to express a result correctly and master the concentration units.

Four graded exercises related to the practical work and prerequisites will take place in a lecture hall (dates included in the schedule). Analysis of the results will also be organised in a lecture hall after each of the tests to answer questions solely related to the resolution of the exercises.

Finally, an out-of-session practical exam will be organised. This exam will be divided in to parts. During the first part, graded exercices related to the partical work will take place in a lecture hall. During the second part, the students should be able to reproduce a manipulation carried out during the various practical work sessions using a very simplified protocol.

Learning outcomes of the learning unit

- Mandatory and formative prerequisite test available on the Ecampus platform. This ungraded test includes about twenty  questions related to good laboratory practice, concentration units, simple titration calculations and redox exercises. This test must be carried out during the first week of the practical work.

- Supervised training in good analytical practices in small groups will take place during the first week of the practical work. Students have access to videos illustrating the most common analytical manipulations as well as additional explanations on the Ecampus platform.

- Seminars with resolution of exercises on pH and buffer solutions. An exercise session on tolerance and dilution will also be organised.

- Explanatory sessions on the dosages to be carried out will be followed by practical sessions in the laboratory. 

- A virtual practical session must be followed on the eCampus platform on how to perform an automated potentiometric titration.

Prerequisite knowledge and skills

Before starting the practical work in Pharmaceutical Analytical Chemistry, the student must have a thorough knowledge of General Chemistry. During the first week, they should perfect their knowledge by reading the manual of prerequisites and performing the mandatory prerequisite training test available on eCampus. They must also have completed the safety training also available on this platform and passed the related exam.

Planned learning activities and teaching methods

Seminars in Analytical Chemistry, supervised training in good analytical practice (filmed demonstrations and personal work at the lab bench), explanations of doses followed by practical titrimentric and physical-chemistry procedures.

Mode of delivery (face to face, distance learning, hybrid learning)

Face-to-face course


Additional information:

Since the purpose of the practical work is to provide both manual and theoretical training, attendance at the practical work sessions and tests is required.

Attendance at the practical work sessions is therefore compulsory.

Students must, therefore, provide a medical certificate justifying any absence or risk being awarded a zero for the session(s) which they were unable to attend.

Recommended or required readings

The Pharmaceutical Analytical Chemistry manual of prerequisites, notes from the Pharmaceutical Analytical Chemistry field work and the Introduction to Pharmaceutical Analytical Chemistry course (CHIM0320-3). Reference works: D.A. Skoog, D.M. West, Chimie Analytique, 3ème Edition, De Boeck, 2015 et A. Bourderioux, M. Bourjot, S. Lordel-Madeleine, L. Valois, Mémo Visuel de Chimie Analytique, 1ère Edition, Dunod, 2020.

Written work / report

Out-of-session test(s)

Other : Practical test, out of session, including the writing of a report


Additional information:

During the year:

- Students will first be evaluated on performance of simple analytical manipulations such as pipetting with a volumetric pipette and quantitative transfer. Secondly, students will be evaluated on the dosages carried out on the basis of the quality of the manipulation (percentage of error in relation to the reference value determined by an evaluation grid adapted according to the expected precision of the manipulation) and the quality of the report. The report is a document to be completed and submitted on the Ecampus platform. Each report is worth 10 points from which penalties will be deducted if the student does not comply with the instructions or provides incomplete or incorrect reports. If the student returns a report with a calculation error in the final answer, the assistant will recalculate the value and the student will be sanctioned by losing half the points for the manipulation. All points obtained during the practical sessions represent 40% of the points of the year.

- Evaluation of theoretical knowledge during four tests directly related to the manipulations carried out during the practical work and to the prerequisites. The average of the four questions represents 30% of the points of the year.

Examination:

- In the first session, the student begin with a question similar to those covered during the year. They then select a manipulation at random and are evaluated according to the same criteria as during the year. Students have access to their laboratory notebook (checked by the assistant before the examination) and receive a simplified protocol without equations or explanations. At the end of the examination, the student must write a handwritten report comparable to those written during the year, focusing on the preparation of the solutions necessary for handling (calculation of weights based on the equation, concentrations, etc. of the standard substance and to be calibrated). If the student returns a report with a calculation error, the assistant will recalculate the value and the student will be sanctioned by losing half the points of the manipulation. The result of the examination is 30% of the points of the year.

Second session:

To begin with, the student receives a question similar to those covered during the year. They then randomly select a manipulation and are evaluated on the basis of the same criteria as during the year. Students have access to their laboratory notebook (checked by the assistant before the examination) and receive a simplified protocol without equation or explanation. At the end of the examination, the student must write a handwritten report focusing on the preparation of the solutions necessary for handling (calculation of weights based on the equation, concentrations, etc. of the standard substance and to be calibrated). If the student returns a report with a calculation error, the assistant will recalculate the value and the student will be sanctioned by losing half the points of the manipulation. In the final grade, the test represents 30% of the points while the manipulation represents the remaining 70%.

Reminder: Attendance at the practical work is compulsory. Therefore, in accordance with Article 40 of the General Examination Regulations, an excessively high absenteeism rate may result in a student being prohibited from taking the examination.

 

Work placement(s)

n/a

Organisational remarks and main changes to the course

There is an eCampus platform on which course and prerequisite booklets are available. Additional explanations and illustrative videos are also available on this site. All slides relating to the explanation sessions, seminars and exercises can also be downloaded via the platform. Students can also download the report templates to be completed from this site, before reposting them. Students will then receive the corrections to their reports via this platform and will also be able to monitor their notebooks.

Contacts

Philippe Hubert, Laboratory of Analytical Chemistry Department of Pharmacy, CHU, Bât. B36, Quartier Hôpital,avenue Hippocrate 15, 4000 Liège 1  Tel : 04/366.43.16 (15) e-mail: ph.hubert@ulg.ac.be
Eric Ziemons Tel.: 04/366.43.26 Fax: 04/366.43.17 e-mail: eziemons@ulg.ac.be
Hugues Jambo Tél : +32 4 366.43.19 e-mail : hjambo@ulg.ac.be
Charlotte De Bleye Tel: +32 4 366.39.79 e-mail: cdebleye@ulg.ac.be
Sébastien Lhoest Tel.: 04/366.43.23 Fax: 04/366.43.17 e-mail: slhoest@ulg.ac.be

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