The book is a humble attempt towards sharpening the knowledge of undergraduate, postgraduate and also the young researchers who are interested to persue 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. In the present book author described the Solvent Extraction technique used as a separation technique which is coupled with Visible-Spectrophotometer for the quantitative determination with a good example of a transition metal.In the present book the author has highlighted all the parameters need to be study for the development of any analytical method. This book can be used as a reference book for the scientists.The final part of the book covers the brief explanation of Extractive Determination of Ce(IV) by using a complexing ligand. The results and Discussions are fruitful for new researchers in their initial approach of the research. This book is also useful to those academicians who are interested to carry major & minor research.