Spectroscopy integrated laboratory

Duration

100h Pr

Number of credits

Lecturer

Christian Damblon, Gauthier Eppe, Bernard Leyh, Jean-Christophe Monbaliu, Loïc Quinton

Coordinator

Gauthier Eppe

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 Integrated Spectroscopy Laboratory course (iTP) is a fully practical course organized into three distinct projects that require mobilizing the knowledge acquired over the three years of the Bachelor's in Chemical Sciences, as well as integrating different spectroscopic methods to extract physicochemical information on molecular systems. Each project implements a different molecular system that students are invited to study in parallel and with partial autonomy under the supervision of the teaching unit's instructors.

Project 1: Identification of a photochromic spiropyran (several possible molecules) by vibrational spectroscopy; study of the optical properties of its open merocyanine form in solution (various possible solvents) by computational chemistry and UV-Visible spectroscopy; kinetic study to determine the thermodynamic activation parameters of the thermal cyclization reaction; and assessment of the synergistic effect of a specific solvent mixture.

Project 2: Calculation of the dissociation constants of substituted aromatic carboxylic acids by computational chemistry to determine Hammett substituent parameters; study of the kinetics of the basic hydrolysis of a mixture of the corresponding substituted ethyl esters by NMR spectroscopy; and establishment of a Hammett plot by relating the experimental relative rate constants of hydrolysis to the electron-donating/withdrawing characters of the substituents.

Project 3: Stereoselective synthesis of a dipeptide by benzotriazole activation of protected amino acids, with characterization of the activated reaction intermediate by vibrational spectroscopy; then blind identification and characterization of the sequence of a dipeptide (several possible molecules) by 1D and 2D NMR spectroscopy and HPLC-UV-IM-MS/MS ion-mobility mass spectrometry; discussion of the dipeptide's chiral identity.

Learning outcomes of the learning unit

By the end of this course, students will be able to:

• Follow a stereoselective synthesis protocol to obtain a molecule of interest for spectroscopic characterization.
• Critically analyze, discuss, and implement an experimental protocol from the literature to obtain reliable spectroscopic data. If necessary, propose a relevant alternative protocol by leveraging the spectroscopic techniques available in the laboratory.
• Use a range of spectroscopic and spectrometric techniques (FTIR-ATR, Raman, UV-Visible, 1D/2D NMR, HPLC-UV-MS/MS, IM-MS, polarimetry) to identify and characterize complex molecular systems (molecule-solvent) and extract useful information (rate constants, energy barriers, energy diagrams).
• Apply computational chemistry methods to calculate and interpret the electronic and photochemical (optical) properties of molecules in different solvents, as well as the dissociation constants of substituted aromatic carboxylic acids.
• Properly process spectroscopic data within an integrated scientific approach and link these experimental data to the structural, stereochemical, and mechanistic concepts of the studied molecular systems.
• Communicate scientific results clearly and in a structured way, both orally and in writing, to fellow students and peers, articulating experimental data, calculations, and interpretation.
• Work with partial autonomy and collaboratively within a group, in order to develop transversal skills: scientific rigor, critical thinking, teamwork, and clear communication.

Prerequisite knowledge and skills

Students must master the basic notions of general, physical, organic, and analytical chemistry covered during the Bachelor's program in Chemical Sciences. Mastery of the fundamental principles underlying spectroscopic and spectrometric methods-their implementation, data processing, and interpretation-is essential.

Prerequisites: CHIM9283-1 - Organic Chemistry II; CHIM9283-2 - Organic Chemistry II; CHIM0750-1 - Data Visualization and Processing in Chemistry; CHIM9285-1 - Chemical Kinetics, Introduction to Spectroscopy, and Group Theory.

Corequisites: CHIM9288-1 - Spectroscopy and Elements of Statistical Thermodynamics; CHIM9289-1 - Analytical Chemistry III - Physical Methods; CHIM9291-1 - Structural Analysis; PHYS0968-1 - Signal Processing.

Planned learning activities and teaching methods

The Integrated Spectroscopy Laboratories (iTP) course is an exclusively hands-on laboratory course. Attendance is mandatory. Laboratory work is carried out in groups of 2 to 3 students. Each group is formed by a random draw during an introductory session and is assigned three original molecular systems to work on.

A work schedule specific to each group is provided to students at the start of the labs and will be adjusted according to the progress of the different groups. This schedule takes into account the possibility of repeating inconclusive experiments and includes periods for processing the collected spectroscopic and spectrometric data, as well as for writing reports. An office workspace is available to student groups so they can process their data together and promote cooperation and the exchange of viewpoints.

A series of discussion sessions with the different instructors is organized to support students in their work. Sessions dedicated to the use of data-processing software (such as Excel, TopSpin, MNova, Gaussian) are held during the lab sessions.

Each student records their observations and results in a laboratory notebook. The planning of experiments, progress status, and presentation of results are discussed during group meetings held 1 to 2 times per week during the integrated laboratory sessions. These group meetings simulate research-lab group meetings and foster the exchange of ideas between supervisors and students. Students present their results and experimental planning in the form of a PowerPoint presentation, the content of which may serve as a basis for drafting the final reports (see the assessment methods below).

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

Face-to-face course


Further information:

The practical sessions (that is, the entirety of this course) are mandatory and held exclusively in person. Any absence must be reported without delay to the instructors and justified in accordance with the faculty procedure in effect.

The practical sessions are organized only once per academic year.

Assessment is based on the acquisition, analysis, and discussion of experimental results obtained during the sessions. Any absence, justified or not, except in cases of force majeure let to the discretion of the CHIM9293 course co-holders, exceeding 25% of the total schedule results in the course being invalidated (see Assessment Methods). Consequently, any student who has not attended at least 75% of the sessions will have to retake the course the following academic year.

Course materials and recommended or required readings

Platform(s) used for course materials:
- eCampus


Further information:

A manual is available online (via the e-campus platform). Reference scientific articles to consult are provided to students in the online manual.

Exam(s) in session

Any session

- In-person

written exam ( multiple-choice questionnaire, open-ended questions ) AND oral exam

Written work / report

Continuous assessment


Further information:

Additional explanations:

Course assessment is based on the acquisition, analysis, presentation, and discussion of experimental results obtained during the laboratory sessions. It is established from four distinct parts (A, B, C, and D; see below). The grade for each part is calculated as the arithmetic mean (without rounding) of the grades awarded by the different members of the course jury for the various teaching activities in which the jury participated. The jury is composed of the course holders, teaching assistants, and laboratory technicians involved in this teaching unit.

The four components of the assessment are:

• Part (A): continuous assessment of laboratory work. This part is graded out of 20, based on work, engagement, and attitude in the lab; keeping a lab notebook; oral presentations; and interim written reports on progress in the lab. The grade for this part may differ within the same student group. Except in cases of force majeure left to the discretion of the CHIM9293 course co-holders, any absence, justified or not, exceeding 25% of the total schedule results in the course being invalidated.
• Part (B): oral assessment. This part, graded out of 20, consists of a 15-minute oral presentation during which students present their experimental results and scientific interpretations. The oral presentation covers only one of the three projects carried out in the lab. The project to be presented by each student group is assigned by random draw. The visual support may be prepared in French or English, though English is recommended. Regardless of the language of the visual support, the presentation itself may be delivered in French or English. The presentation is followed by a 15-minute Q&A session with the jury. If students choose to present in English, they may answer the jury's questions in English or French. The jury's questions are specific to the project presented, but also of a general nature to verify that students master and can apply the basic notions of general, physical, organic, and analytical chemistry covered in the Bachelor's curriculum in Chemical Sciences. The grade for this part may differ within each group.
• Part (C): written assessment-1. This part, graded out of 20, consists of a written report on one of the two projects not covered by Part (B) above. The report follows a double-column scientific-publication template provided to students on the e-campus platform. It presents the experimental aspects (materials and methods), the results and their scientific interpretations, as well as a conclusion. The report may be written in French or English, though English is recommended. Students who submit their report before the deadline (specified on e-campus) will receive feedback in the form of a reviewing, covering both content and form, to improve the quality of their written report prior to its evaluation.
• Part (D): written assessment-2. This part, graded out of 20, consists of a written report on the project not covered by Parts (B) and (C) above. The modalities are identical to those of Part (C).

• Student 1: High and consistent performance: A 18.1; B 15.4; C 17.3; D 17.8. Average 17.2 (rounded to 17). The absorbing threshold does not activate. Overall grade G = 17; pass, no second session.
• Student 2: Major difficulties in B, C, and D: A 15.1; B 4.0; C 1.9; D 1.4. Average 5.6 (rounded to 6). Threshold activates; overall grade remains G = 6; fail, second session on Parts B, C, and D.
• Student 3: Good grades except in B: A 18.1; B 9.6; C 12.2; D 14.9. Average 13.7 (rounded to 14). Threshold activates and brings overall grade to G = 7; fail, second session on Part B.
• Student 4: Part A insufficient (practical sessions, no second session) but B-D satisfactory: A 7.2; B 14.1; C 14.4; D 12.6. Average 12.1 (rounded to 12). Threshold activated: G = 7; fail, no second session (A is practical and cannot be retaken).
• Student 5: Weaknesses in A, B, and C: A 9.0; B 4.3; C 4.9; D 12.2. Average 7.6 (rounded to 8). Threshold activated: G = 7; fail, no second session (A is practical and cannot be retaken).

Work placement(s)

Organisational remarks and main changes to the course

Contacts

C. Damblon, C.Damblon@uliege.be 

G. Eppe, G.Eppe@uliege.be 

B. Leyh, Bernard.Leyh@uliege.be 

C. Malherbe, C.malherbe@uliege.be

J.-C. Monbaliu, jc.monbaliu@uliege.be 

L. Quinton, Loic.Quinton@uliege.be 

Association of one or more MOOCs