The aim of this module is to instruct students in the practice of taking physical measurements, the critical analysis and evaluation of experimental data, the application of measurements to the study of chemical phenomena and the dissemination of results.

(LO1) By the end of the module, students should be able to
1. Take physical measurements of varying complexity using a wide range of experimental techniques;
2. Assess the risks involved in chemical lab work and handling chemical materials in a safe manner;
3. Choose appropriate methods for the analysis of data;
4. Analyse experimental data using graphs, spreadsheets and linear regression;
5. Assess the accuracy and significance of experimental results;
6. Apply the results of physical measurement to the interpretation of chemical phenomena;
7. Combine units and perform a dimensional analysis;
8. Have experience of the application of spectroscopic techniques (UV, IR, NMR and mass spectrometry) in the characterisation of organometallic and inorganic compounds;
9. Organise and plan their time effectively.

Practical. This is a laboratory-based module in which students practise a range of measurement techniques appropriate for investigating a wide range of chemical phenomena spanning thermodynamics, kinetics, spectroscopy, electrochemistry, surface science and transition metal chemistry.
Students perform experiments with minimum supervision (although staff and postgraduate demonstrators are at hand to answer questions and provide guidance if necessary) and are responsible for planning and timetabling their experiments themselves.
Students are expected to complete a minimum number of six experiments (including the virtual NMR experiment), although two more experiments may be undertaken.
Each experiment must be analysed using appropriate techniques and written up in a laboratory report which is presented to a demonstrator for marking before the next experiment is allocated. Marks are allocated for the quality of the data, the quality of the write-up and the understanding disp layed.

Coursework - There are 2 x 3hr physical workshops and 3 x 2 hr NMR workshops. Students’ work is assessed and feedback is given during the physical chemistry workshops. For NMR, students hand in their work after the workshops.

Lectures - There are two one hour lectures: 1) introductory lecture to the module, and 2) introductory lecture to NMR.

*Practical: 72 hr
*Workshops: 11 hr
*Lectures: 2 hr

The experiments comprise a series of experiments from Physical Chemistry and Inorganic Chemistry:
• Kinetics of the acid-catalysed hydrolysis of ethyl ethanoate
• Critical micelle concentration
• Boiling point - composition diagram
• The dipole moment of dibenzoyl
• Iodine absorption spectrum
• Redox potential of the iron system
• The dissociation of ethanoic acid by conductance
• Potentiometirc titration
• Reaction isotherm
• Fluorescence of Rhodamine B and its quenching by iodide ions
• Gas-liquid chromatography
• The enthalpy of neutralisation
• Bomb calorimetry
• The association of uranyl and thiocynanate ions
• The reaction of crystal violet with hydroxide ions
• Thermodynamics of ethanoic acid dimerisation
• T he characterisation of reaction intermediates by NMR Spectroscopy
• Job's method
• Preparation & thermochromic transition of diethylammonium tetrachlorocuprate(II)
• Conductivity of transition metal complexes
• Magnetic susceptibility of nickel complexes
• UV-vis spectra of transition metal ions

The physical workshops are designed to teach generic skills needed for the analysing experimental results (Data and error analysis, Dimensional analysis).
There are also a series of spectroscopic workshops. Each workshop will begin with a short lecture to introduce the topics covered. Students will be introduced to spin 1/2 NMR active nuclei other than 1H and will then work through problem sheets under the guidance of the demonstrators.
The following material will be covered:
• Introduction to the physical basis of NMR. Quantum numbers, energy levels, magnetic equivalence, che mical shifts and scalar couplings.
• The use of mass spectra, infrared spectra, elemental analyses and multinuclear NMR spectra to determine the structure of inorganic and organometallic complexes.
• Scalar coupling (J values) in NMR and its use in the determination of stereochemistry and conformational analysis