Module Details

The information contained in this module specification was correct at the time of publication but may be subject to change, either during the session because of unforeseen circumstances, or following review of the module at the end of the session. Queries about the module should be directed to the member of staff with responsibility for the module.
Title Preparative Chemistry: Synthesis and Characterisation
Code CHEM245
Coordinator Dr K Luzyanin
Chemistry
Konstantin.Luzyanin@liverpool.ac.uk
Year CATS Level Semester CATS Value
Session 2022-23 Level 5 FHEQ First Semester 15

Pre-requisites before taking this module (or general academic requirements):

 

Aims

The module aims to present a unified approach to the synthesis and characterisation of organic and inorganic compounds and will build on techniques introduced in the first year laboratory courses.


Learning Outcomes

(LO1) Students will complete a number of different experiments and synthetic techniques across synthetic, organic and inorganic chemistry.

(LO2) Students will appreciate how spectroscopic techniques can be used in the characterisation of organic and inorganic compounds and will be able to use analytical and spectroscopic methods to characterise their synthesised compounds.

(LO3) Students will make use of scientific databases during some assignments and an electronic report.

(LO4) Students will assess the risks involved in chemical lab work and handle chemical materials in a safe manner.

(LO5) Students should be able to organise and plan their time effectively

(LO6) Students will experience working collaboratively with others in multiple learning environments

(S1) Organisational skills

(S2) Problem solving skills

(S3) Teamwork


Teaching and Learning Strategies

In this module students will be expected to complete a series of synthetic experiments. Each experiment will have a preliminary exercise (which includes a consideration of safety issues) which must be completed to a satisfactory standard before the experiment is performed. On completion of the experiment, students must produce a write-up describing what was done and submit their results.

The laboratory sessions are complemented by workshops on spectroscopic techniques. Students are expected to work through a series of exercises with the support of teaching staff. The knowledge gained in the workshops is tested in class and by the means of a series of online tests.

Additional lecture/tutorial/workshop activities include:
1. Introductory and Safety lectures (three lectures, 3x1h)
2. Spectroscopy and analytical characterisation lectures (five lectures, 5x1h) and respective workshops (four workshops, 4x2h).
3. Lectures on an introduction to databases (two lectur es, 2x1h) and in person/computer-based workshop (3h)
4. In person and online tutorials/workshops on use of analytical software and instrumentation (Topspin workshop, 3h; OpenChrom tutorial, 1h)
5. Problem-based group activity/workshop (2h)
Self-Directed Learning Description: While there is plenty of opportunity for self-directed learning, this is encompassed in the learning strategies mentioned above.

*Laboratory work: 72 hr
*Workshops: 16 hr
*Lectures and lecture-related tutorials: 11 hr


Syllabus

 

Practical
Students are expected to complete a variety of synthetic, organic and inorganic experiments which may include, but not limited to:
• A Hantzsch pyridine synthesis.
• Synthesis of dimedone by carbonyl condensations.
• A Grignard reaction using a protecting group.
• Separation of fluorene/fluorenone using column chromatography
• Preparation and analysis of iron(II) oxalate.
• Preparation and analysis of acetylacetonato-complexes of metals.
• Preparation of a cobaltammine and the determination of its molecular formula.
• Preparation of dichlorobis(ethylenediamine)cobalt(III) complex
• Preparation of a metal-organic framework based around magnesium formate (MOF)
• Comparing copper complexes of ‘soft’ PPh3 and ‘hard’ O=PPh3

Supporting exercises include a mixture of online and face-to-fa ce strategies including lab book write ups, submission of results and calculations, pre- and post- lab assessments and engagement with safety and the course via checkpoints/assignments. The "MOF" experiment is completed in groups and students are assessed together initially, with group assessment subject to peer evaluation for to allow adjustments for individual grades. Other experiments may be completed in pairs but will be assessed individually.

Coursework:
Workshops on spectroscopy and analytical methods: Revision and expansion of various spectroscopic techniques including mass spectrometry, infrared spectra, ultraviolet spectroscopy, elemental analyses and NMR (1H and 13C). Spin-spin coupling (J values) in 1H NMR and their use in the determination of stereochemistry and conformational analysis will be introduced. Interpretation of these spectroscopic methods will be required to determine the structures of organic and inorganic molecules.

Databases, TopSpi n and electronic reports: This will include a refresher of year 1 database/TopSpin material and the introduction of structure and text combination searches using databases such as Reaxys. The focus will be on small molecules, inorganic salts and simple organometallics and searching using chemical properties, reactions, stereochemistry, generic groups and reagents. This will culminate in how to combine all material learnt into an electronic report.

Safety: Annual safety lecture, NMR safety lecture and workshop on why risk assessments are needed (COSHH, carcinogens and general) and how they are generated via SDS and legislation.


Recommended Texts

Reading lists are managed at readinglists.liverpool.ac.uk. Click here to access the reading lists for this module.

Teaching Schedule

  Lectures Seminars Tutorials Lab Practicals Fieldwork Placement Other TOTAL
Study Hours 11

    72

  16

99
Timetable (if known)              
Private Study 51
TOTAL HOURS 150

Assessment

EXAM Duration Timing
(Semester)
% of
final
mark
Resit/resubmission
opportunity
Penalty for late
submission
Notes
             
CONTINUOUS Duration Timing
(Semester)
% of
final
mark
Resit/resubmission
opportunity
Penalty for late
submission
Notes
Lab experience.    70       
Spectroscopy and Databases    30