Dysprosium-titanate (Dy 2 TiO 5 ), being highly refractory in nature, its dissolution using conventional (hot-plate and fusion) methods is very difficult. Hence, for quantitative dissolution, a microwave method has been developed. The instrumental parameters and amount of acids has been optimized. Studies have been carried out for precise and accurate estimation of major elements such as Dy, Ti, and Mo. An anion exchange column has been used to separate Mo, Dy and Ti. Analysis of these elements has been carried out using ICP-MS, UV-visible spectroscopy, and gravimetric methods. In the developed method, precipitation of molybdenum and dysprosium has been done using α-benzoine oxime, and oxalic acid respectively. These precipitates have been converted into their respective oxide form. The purities of these oxides (Dy 2 O 3 and MoO 3 ) have been determined using ICP-MS. The method has been validated using synthetic samples where it is found that accuracy of Dy and Mo is >99% and precision is <1 (%RSD). The titanium has been determined using UV-visible spectroscopy with accuracy >98% and precision <2 (%RSD).