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Excipients are used in pharmaceutical formulations as fillers and drug carriers. Their successful function is inextricably linked to their physicochemical properties and, in turn, these properties are directly related to their structure. This thesis is concerned with the structural and spectroscopic characterisation of a selection of excipients by powder and single crystal X-ray diffraction, Raman and IR spectroscopy and MASNMR and an investigation of their stability as a function of temperature, humidity and particle size. As well as being a well-known excipient used in the pharmaceutical industry, lactose is also a common food additive. The diverse usage of lactose has led to a wealth of contradictory information relating to both structure and properties of this material. The first part of experimental work in this thesis identifies the four real lactose polymorphs; the naturally occurring a-lactose monohydrate; the anhydrous stable form of a-lactose; the hygroscopic unstable form of a-lactose; and the anomeric equivalent, p-lactose using powder X-ray diffraction. The work shows that anhydrous lactose formed by solvent dehydration often termed aM is simply the anhydrous stable form of a-lactose formed via a different route. Simple methods for discerning between the polymorphs using standard laboratory equipment are suggested. IlC MASNMR data were collected on all four forms of lactose for the first time and illustrate key differences between the four structures. Single crystal data were successfully collected on the a-lactose monohydrate and refinement carried at low temperature to determine the hydrogen bonded arrangement for the first time. Rietveld refmement of the hygroscopic unstable form of a-lactose using in-situ temperature resolved X-ray diffraction has shown that the hygroscopic form can be produced as a single phase. Refinement of Plactose using the Rietveld method has shown that powder diffraction data were comparable with single crystal data, with respect to structure refinement but attempts at both crystallisation and refinement of the stable anhydrous a-lactose polymorph were unsuccessful due to the complexity of the structure. Powder X-ray diffraction analysis was shown to be an effective tool in the quantification of mixed phase lactose samples with respect to both mixed phase stable anhydrous a-lactose and a-lactose monohydrate; and mixed p-Iactose and a-lactose monohydrate samples. The accuracy of the technique was determined to be at least 5%. Quantification was carried out using relative intensities of a well resolved unique reflection for each phase within the system. Dehydration techniques applied to lactose were applied to other hydrated pharmaceutical sugars; trehalose dihydrate and raffmose pentabydrate. Solid state techniques; powder X-ray diffraction, Raman and IR spectroscopy; showed that discrimination of other sugar hydrates became more complex with increasing levels of hydration.

This thesis provides a background on the effects of applied and magnetic fields on crystallisation, and summarises the analytical techniques employed for characterisation and analysis. The study of applied fields was carried out on the crystallisation of one main system-solid nonadecane. This was then studied further to establish the effects of a solvent and a mixed solid system on the crystallisation of nonadecane. The systems studied were the crystallisations of: static and dynamic nonadecane, static and dynamic nonadecane in heptane, static and dynamic nonadecane and heneicosane, static and dynamic nonadecane and heneicosane in heptane and static and dynamic nonadecane and crude oil. The results of these studies showed that the magnetic and applied fields can affect electrostatic forces in molecular solids. It also showed that even the weakest of these forces, Van der Waals forces are affected by applied and magnetic fields.

Nanocrystalline praseodymium oxide films have been successfully generated on stainless steel substrates. The electrochemical deposition was performed in the cathode compartment of a divided electrochemical cell with a regular three-electrode configuration. The green films obtained by electrodeposition were then annealed at high temperatures for 1-3 hours. X-ray diffraction revealed the fluorite structure of Pr6O11 and the crystallite size was calculated. X-ray photoelectron spectroscopy was employed to study the composition of the oxide films and also the oxidation state of Pr. Scanning electron microscopy was utilized to study the surface texture and microstructure of deposits. Fourier transform infrared spectrometery was used to investigate the composition of the films. The effects of different conditions on the green films were also studied such as different pH values of the electrolyte solution, different deposition modes, different supporting electrolytes and different applied current densities. Sintering experiments were conducted to investigate the properties of the green films. Praseodymium oxide powders were also successfully prepared by combining electrochemical methods with sintering processes. The praseodymium oxide powders were characterized by X-ray diffraction and Fourier transform infrared spectroscopy. The crystallite sizes of the powders were evaluated.