Specimens prepared from melt grown high purity single crystals of cadmium have been examined by optical and X-ray microscopy. The X-ray microscopy examination was carried out using the Lang technique. A correlation, although not a direct one, between etch pits on the (1010) plane produced using a dilute Nital solution and dislocations has been obtained. The substructure of cadmium in specimens prepared in both basal and (1010) orientation has been studied. Large edge type dislocation loops have been observed in basal oriented slices after annealing and slow cooling and provisional Burgers vectors of and attributed to them. A tentative explanation as to their origin has been arrived at. The annealing kinetics of loops at room temperature has been studied. A marked dependence upon the cooling rate and annealing regime on the room temperature dislocation density and subgrain size for basal oriented specimens has been found. The alcohol based nitric acid etching and polishing solutions for cadmium have been chemically examined. A novel temperature programmer developed in conjunction with another person in this department and used for producing high quality single crystals of cadmium for X-ray microscopy examination has been patented by N.R.D.C.