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The purpose of this work has been the determination of structure in solids using the technique of solid-state nuclear magnetic resonance spectroscopy. High-resolution (^31) p NMR spectra have been obtained for a range of phosphate species. A number of techniques have been applied to these systems including cross-polarization, magic angle spinning, and high power proton decoupling. Characterisation using additional NMR techniques such as (^1) H cramps has been carried out wherever possible. The results obtained yield molecular and crystallographic information consistent with data from X-ray diffraction when known. Shielding tensor components were determined from static and/or spinning spectra wherever possible. The phosphate species studied include a series of precipitated calcium phosphates. A particular model for the structure of amorphous calcium phosphate is favoured in the light of (^31) p NMR measurements. One sample showed NMR evidence for changes in composition whilst in the solid state. The origins of (^31) p NMR line widths in high-resolution solid-state spectra have been considered in some detail. Variation of (^31) p NMR linewidth as function of spinning rate has been noted for a number phosphate compounds. Multiple pulse techniques have been applied on the phosphorus channel with pleasing improvements in spectral resolution. Five solid binary phosphorus sulphides have also been studied using phosphorus MAS NMR, and the results compared to solution state data wherever possible. A number of anomalies between solution and solid-state data have been noted and discussed.

The magnetic particle inspection (MPI) method is a widely used non destructive testing (NDT) technique for ferrous structures. Magnetic inks used in MPI are suspensions of fine ferro/ferrimagnetic particles which, when applied to a magnetized test specimen, delineate surface flaws. This work is an investigation of some of the properties of magnetic ink systems and some aspects of their interaction with defect leakage flux. Reviews of magnetism, the MPI method and leakage flux at defects are given. The construction, characterization and automation of a 1.2 T electromagnet vibrating sample magnetometer, used for magnetic measurements on the inks, is described. The instrument has a resolution of better than l0(^-9) JT(^-1) . A 2D model of indication formation in MPI, based upon the simulation of many particles in the neighbourhood of a defect, is presented. Results of the role of several of the model parameters are given. Results indicate that carrier coefficients of viscosity at the lower end of the range investigated (η = 0.3 mPas) are optimum. The size and contrast of an indication increases with defect size. The contrast and rate of formation of contrast increase with defect aspect ratio. The effect of the contrast paint layer thickness indicates that the recommendation of the British Standard, BS 5044 (1973), is qualitatively correct. Experimental observations of particles in field gradients reveals a discrepancy between theoretical and observed behaviour which is attributed, in particular, to unobservable voids in the particles. Detailed characterization of the particles shows them to be aggregates of 20 - 200 nm crystallites which are probably single domain particles. The morphology of larger aggregates is related to measurements of the low field susceptibility. Evidence from intensive magnetic measurements supports the relationship between magnetic properties and aggregate characteristics. A 'In t' magnetic viscosity effect is reported. At 77 K, the coefficient of magnetic viscosity has a maximum near the coercivity field.