Pressurised pipelines are the primary mode of choice for transporting large quantities of hazardous fluids across the globe. The failure of such pipelines can lead to the release of significant amounts of flammable or toxic inventories, which may in turn present significant risks to life, environment and property. In order to mitigate such risks, various types of emergency shutdown valves (ESDVs), including Check Valves (CVs), Automatic Shut-off Valves (ASVs) and Remote Control Valves (RCVs), are installed along such pipelines as the front-line emergency mitigation tool.Accounting for the critically important ensuing in-pipe transient fluid flow, this thesis presents the development and application of a multi-objective optimisation study for selecting the ESDV type, number and spacing as well as its combinations and operational settings for striking a balance between the minimum valve capital cost against the efficacy in minimising and ultimately isolating outflow following pipeline failures.To my parents and brother: Thank you for your never-ending support and motivation.