The book is an attempt to spread the research work worldwide. The book is intended for students of chemistry. The book serves as a supplement for undergraduates, postgraduate and also useful for the young researchers who are interested to peruse their research in the field of separation technique as well as quantitative estimation of trace metal ions spectrophotometrically. The book explains all the basic principles of separation techniques as well as the brief idea about all the modern techniques used for quantitative estimations. The book describes the Solvent Extraction technique as a separation technique which is coupled with UV-Visible Spectrophotometer for the quantitative determination with a good example of a transition metal. The book optimizes various parameters essential for development of analytical method. The final part of the book covers the brief explanation of Determination of Mo (VI) by using APDHTS as a complexing ligand. The results and Discussions are fruitful for analysis of molybdenum in trace amount. This book is also useful to those academicians who are interested to carry major as well as minor research project.