The research described in this dissertation is a comprehensive account of an attempt to correlate structural and physicochemical properties of various metal-containing aluminophosphate molecular sieves (MeAPO-5) and metal-silicon-containing aluminophosphate molecular sieves (MeAPSO-5) with their catalytic properties. Mg, Co, Mn and Zn were incorporated into the AlPO₄-5 framework by isomorphous substitution to form MAPO-5, CoAPO-5, MnAPO-5 and ZAPO-5, respectively. The incorporation of these metals was also carried out into the silicon-containing aluminophosphate molecular sieves (SAPO-5) framework to form MAPSO-5, CoAPSO-5, MnAPSO-5 and ZAPSO-5, respectively. The MeAPO-5 and MeAPSO-5 were characterised by X-ray diffraction (XRD), infrared (IR) spectroscopy, temperature-programmed desorption (TPD), scanning electron microscopy (SEM), nitrogen adsorption, thermal analysis and chemical analysis followed by ³¹P and ²⁹Si of magic-angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. The catalytic properties of MeAPO-5 and MeAPSO-5 were studied in the conversion of cyclohexanol. The results from the study proved that the metals were successfully incorporated into the AlPO₄-5 and SAPO-5 frameworks. Incorporation of metal was detected by the conversion of cyclohexanol over these catalysts. The results show that MeAPO-5 and MeAPSO-5 possess Bronsted acidity as indicated by the dehydration of cyclohexanol to cyclohexene, and basicity from dehydrogenation of cyclohexanol to cyclohexanone. HZSM-5, as a comparison, was more active for dehydration of cyclohexanol than MeAPO-5 and MeAPSO-5, in agreement with the higher strength of the acid sites, as measured by the temperature-programmed desorption of ammonia. Incorporation of metal resulted in a structural distortion of MeAPO-5 and MeAPSO-5; indicated by the increase in the a-axis and the decrease in the c-axis of the lattice parameters. This is explained by the influence of the size (ionic radii) of metal atom; a larger metal atom distorts the structure of MeAPO-5 and MeAPSO-5. The distortion of the structure was associated with the T-O-P angle and the acid/basic strength. The degree of the distortion was correlated with the strength of the Bronsted acid sites in decreasing order of acidity as the following: Mn > Zn > Co > Mg in MeAPO-5 and MeAPSO-5. This was also correlated with the basic strength of these catalysts as measured by the conversion of cyclohexanol; the incorporation of metal increased the Bronsted acidity and decrease the basicity at the localised structure. The topology of Si also affected the acidity of these catalysts as proven by ²⁹Si MAS NMR. The incorporation of Si was controlled by the incorporation of metal. MnAPSO-5 showed the highest catalytic activity, and is considered a potential catalyst for the conversion of alcohols.